Trends in non-alcoholic beverages 9780128169384, 0128169389

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Trends in Non-alcoholic Beverages

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Trends in Non-alcoholic Beverages

Edited by Charis M. Galanakis Research & Innovation Department, Galanakis Laboratories, Chania, Greece Food Waste Recovery Group, ISEKI Food Association, Vienna, Austria

Academic Press is an imprint of Elsevier 125 London Wall, London EC2Y 5AS, United Kingdom 525 B Street, Suite 1650, San Diego, CA 92101, United States 50 Hampshire Street, 5th Floor, Cambridge, MA 02139, United States The Boulevard, Langford Lane, Kidlington, Oxford OX5 1GB, United Kingdom Copyright © 2020 Elsevier Inc. All rights reserved. No part of this publication may be reproduced or transmitted in any form or by any means, electronic or mechanical, including photocopying, recording, or any information storage and retrieval system, without permission in writing from the publisher. Details on how to seek permission, further information about the Publisher’s permissions policies and our arrangements with organizations such as the Copyright Clearance Center and the Copyright Licensing Agency, can be found at our website: www.elsevier.com/permissions. This book and the individual contributions contained in it are protected under copyright by the Publisher (other than as may be noted herein). Notices Knowledge and best practice in this field are constantly changing. As new research and experience broaden our understanding, changes in research methods, professional practices, or medical treatment may become necessary. Practitioners and researchers must always rely on their own experience and knowledge in evaluating and using any information, methods, compounds, or experiments described herein. In using such information or methods they should be mindful of their own safety and the safety of others, including parties for whom they have a professional responsibility. To the fullest extent of the law, neither the Publisher nor the authors, contributors, or editors, assume any liability for any injury and/or damage to persons or property as a matter of products liability, negligence or otherwise, or from any use or operation of any methods, products, instructions, or ideas contained in the material herein. British Library Cataloguing-in-Publication Data A catalogue record for this book is available from the British Library Library of Congress Cataloging-in-Publication Data A catalog record for this book is available from the Library of Congress ISBN: 978-0-12-816938-4 For Information on all Academic Press publications visit our website at https://www.elsevier.com/books-and-journals

Publisher: Charlotte Cockle Acquisition Editor: Patricia Osborn Editorial Project Manager: Charlotte Rowley Production Project Manager: Omer Mukthar Cover Designer: Matthew Limbert Typeset by MPS Limited, Chennai, India

Contents List of Contributors.......................................................................................... xiii Preface ............................................................................................................ xv Chapter 1: Carbonated Beverages........................................................................... 1 Ibrahim M. Abu-Reidah 1.1 Introduction.......................................................................................................... 2 1.2 Ingredients ........................................................................................................... 4 1.2.1 Water ...................................................................................................... 4 1.2.2 Sweeteners .............................................................................................. 5 1.2.3 Acidulants............................................................................................... 7 1.2.4 Preservatives ......................................................................................... 10 1.2.5 Carbon Dioxide .................................................................................... 10 1.2.6 Flavors .................................................................................................. 11 1.2.7 Colorants .............................................................................................. 13 1.2.8 Carbon Dioxide Production .................................................................. 15 1.2.9 Carbonation (CO2 Impregnation) Process ............................................. 16 1.2.10 Syrup Preparation ................................................................................. 17 1.2.11 Deaeration ............................................................................................ 18 1.2.12 Carbonators .......................................................................................... 18 1.2.13 Mixing Procedures ................................................................................ 18 1.2.14 Filling Processes ................................................................................... 19 1.2.15 Continuous Blend Production ............................................................... 19 1.2.16 Packaging ............................................................................................. 21 1.3 Types of Carbonated Beverages ......................................................................... 23 1.3.1 Cola ........................................................................................................ 23 1.3.2 Energy and Sports Drinks ....................................................................... 23 1.3.3 Functional Beverages.............................................................................. 24 1.3.4 Low and Mid-Calorie beverages ............................................................. 25

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vi Contents Balancing of Acidity and Sweetness .................................................................. 25 Quality Standards ............................................................................................... 26 Regulatory Issues of Beverages.......................................................................... 27 Economic Aspects .............................................................................................. 27 Quality Control .................................................................................................. 28 1.8.1 Ingredients .............................................................................................. 28 1.8.2 Syrup ...................................................................................................... 29 1.8.3 Beverages ............................................................................................... 29 1.8.4 Packaging ............................................................................................... 30 1.9 Basic Considerations in the Soda Industry ......................................................... 30 1.10 Sensory Evaluation of Carbonated Soft Drinks .................................................. 31 1.11 Recent and Future Advances and Trends ........................................................... 31 1.11.1 Insights and Perspectives ...................................................................... 33 1.12 Conclusion ......................................................................................................... 35 References.................................................................................................................... 35 Further Reading ........................................................................................................... 36 1.4 1.5 1.6 1.7 1.8

Chapter 2: CO2 and Bubbles in Sparkling Waters ................................................. 37 Ge´rard Liger-Belair 2.1 Introduction ......................................................................................................... 37 2.2 Materials and Methods ......................................................................................... 39 2.2.1 Three Batches of Naturally Carbonated Waters ........................................ 39 2.2.2 Measuring the Kinetics of Dissolved CO2 Progressively Discharging from Water ............................................................................ 40 2.2.3 Measuring the Kinetics of Bubbles Growing Stuck on the Bottom of a Plastic Cup ............................................................................ 41 2.3 Results and Discussion......................................................................................... 42 2.3.1 Deciphering the Thermodynamic Equilibrium in the Sealed Bottles ......... 42 2.3.2 The Kinetics of Dissolved CO2 Escaping from the Water Bulk after Pouring ..................................................................................................... 45 2.3.3 The Kinetics of Bubbles Growing Stuck on the Bottom of a Plastic Cup ................................................................................................ 48 2.3.4 Is There a Critical Dissolved CO2 Concentration Required for Bubbling? ............................................................................................ 55 2.3.5 How Many Bubbles in Your Glass of Sparkling Water? ........................... 57 2.4 Conclusion ........................................................................................................... 59 Acknowledgments ........................................................................................................ 60 References.................................................................................................................... 60 Further Reading ........................................................................................................... 62

Contents vii

Chapter 3: Cereal-Based Nonalcoholic Beverages ................................................... 63 Loreta Basinskiene and Dalia Cizeikiene 3.1 Introduction ......................................................................................................... 63 3.2 Nonfermented Cereal-Based Beverages ............................................................... 66 3.2.1 Cereal-Based Milk Substitutes .................................................................. 66 3.2.2 Roasted Grain Beverages .......................................................................... 71 3.3 Fermented Nonalcoholic Beverages ..................................................................... 73 3.3.1 Traditional Cereal-Based Fermented Beverages ........................................ 73 3.3.2 Nutritional Properties ................................................................................ 76 3.3.3 Nontraditional Cereal-Based Probiotic Beverages ..................................... 81 3.4 Future Trends ....................................................................................................... 86 3.4.1 New Probiotic Cultures Selection and Application for Beverages Production ................................................................................................. 86 3.4.2 Micro- and Nanoencapsulation Techniques for Improved Probiotics Surveillance .............................................................................................. 88 3.4.3 Nanotechnology Application for Functional Cereal-Based Beverages ....... 90 3.4.4 Colloidal Delivery Systems for Food-Grade Nanoparticles ....................... 90 References.................................................................................................................... 91 Further Reading ........................................................................................................... 99

Chapter 4: Ready-to-Drink Tea............................................................................101 Kriti Kumari Dubey, Madhura Janve, Aratrika Ray and Rekha S. Singhal 4.1 Introduction...................................................................................................... 102 4.2 Types of Ready-to-Drink Tea........................................................................... 103 4.2.1 Instant Tea Powder ............................................................................... 103 4.2.2 Batch Brewed Tea ................................................................................ 104 4.2.3 Brewed Tea Extract .............................................................................. 104 4.3 Raw Materials for the Manufacture of RTD Tea .............................................. 105 4.4 Green Tea Leaves ............................................................................................ 108 4.5 Black Tea Leaves............................................................................................. 111 4.6 Additives.......................................................................................................... 112 4.7 Prebiotic and Probiotic Components of Different Types of RTD Tea .............. 112 4.8 Manufacturing and Processing of RTD Tea Beverages .................................... 117 4.9 Extraction of Black and Green Tea Extract ...................................................... 117 4.10 Taste Enhancement of RTD Tea ...................................................................... 117 4.11 Color Improvement of RTD Tea ...................................................................... 118 4.12 Aroma Enhancement of RTD Tea .................................................................... 118 4.13 Clarity of RTD Tea .......................................................................................... 119 4.14 Mouthfeel of RTD Tea..................................................................................... 119

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Contents Prevention of Creaming of RTD Tea ............................................................... 120 Shelf Stability of RTD Tea .............................................................................. 121 Packaging of RTD Tea..................................................................................... 122 Sensory Evaluation of RTD Tea Beverages ..................................................... 123 Health Benefits of RTD Tea ............................................................................ 124 Safety of RTD Tea During Processing and Consumption................................. 125 Bioavailability of RTD Tea Constituents ......................................................... 129 Ready-to-Drink Tea Market ............................................................................. 130 Factors Affecting RTD Tea Manufacturing ...................................................... 131 4.23.1 Product Innovation ............................................................................. 131 4.23.2 Raw Material Sourcing ....................................................................... 131 4.23.3 Process Development .......................................................................... 132 4.23.4 Testing of Quality Parameters ............................................................ 132 4.23.5 Packaging ........................................................................................... 132 4.23.6 Marketing ........................................................................................... 132 4.24 Conclusion ....................................................................................................... 133 References.................................................................................................................. 133 Further Reading ......................................................................................................... 139 Websites..................................................................................................................... 139 4.15 4.16 4.17 4.18 4.19 4.20 4.21 4.22 4.23

Chapter 5: Membrane Technologies for the Production of Nonalcoholic Drinks .......141 Roberto Castro-Mun˜oz 5.1 Introduction ....................................................................................................... 141 5.2 Nutritional Value of Alcoholic Beverages.......................................................... 143 5.3 Nonalcoholic Beer Production Through Membrane Processes ........................... 145 5.4 Nonalcoholic Wine Production Through Membrane Processes .......................... 151 5.5 Production of Other Nonalcoholic Beverages by Membrane Processes .............. 157 5.6 Conclusion ......................................................................................................... 158 Abbreviations ............................................................................................................. 159 References.................................................................................................................. 159

Chapter 6: Nonalcoholic Beer ..............................................................................167 Nihal Gu¨zel, Mustafa Gu¨zel and K. Sava¸s Bahc¸eci 6.1 Introduction ....................................................................................................... 167 6.2 Chemical and Sensorial Properties ..................................................................... 171 6.3 Production of Nonalcoholic Beer ....................................................................... 174

Contents ix 6.3.1 Biological Methods............................................................................... 175 6.3.2 Physical Methods.................................................................................. 181 6.3.3 Other Methods ...................................................................................... 191 6.4 Conclusion ......................................................................................................... 192 References.................................................................................................................. 193 Further Reading ......................................................................................................... 200

Chapter 7: Nonthermal Technologies for Nonalcoholic Beverages ...........................201 G.J. Swamy, K. Muthukumarappan, A. Sangamithra, V. Chandrasekar and S. Sasikala 7.1 Introduction...................................................................................................... 202 7.2 Ultrasound ....................................................................................................... 202 7.2.1 Generation of Power Ultrasound........................................................... 202 7.2.2 Microbial Inactivation in Nonalcoholic Beverages ............................... 204 7.3 Ozonation......................................................................................................... 207 7.4 Ozone Generation ............................................................................................ 208 7.5 High-Pressure Processing ................................................................................. 210 7.6 High-Pressure
Processing Equipment ............................................................. 211 7.7 Ultraviolet and Pulsed-Light Technology ......................................................... 212 7.8 Irradiation ........................................................................................................ 213 7.8.1 Mode of Inactivation of Microbes ........................................................ 216 7.9 Cold Plasma ..................................................................................................... 217 7.9.1 Mode of Action of Cold Plasma ........................................................... 218 7.9.2 Treatment of Nonalcoholic Drinks with Plasma ................................... 218 7.10 Pulsed Electric Field Processing ...................................................................... 220 7.10.1 PEF Equipment Design....................................................................... 220 7.11 Dense-Phase Carbon Dioxide Technology ....................................................... 221 7.12 Conclusion ....................................................................................................... 226 References.................................................................................................................. 227 Chapter 8: Emerging Technologies for Noncarbonated Beverages Processing ..........233 Meliza Lindsay Rojas, Alberto Claudio Miano, Karla Aguilar and Pedro Esteves Duarte Augusto 8.1 Introduction ....................................................................................................... 233 8.2 Principles and Fundamentals of Emerging Technologies ................................... 234 8.2.1 High Power Ultrasound ........................................................................... 234 8.2.2 Ultraviolet ............................................................................................... 235

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Contents 8.2.3 High Hydrostatic Pressure ....................................................................... 237 8.2.4 High Pressure Homogenization ............................................................... 238 8.2.5 Pulsed Electric Fields .............................................................................. 239 8.3 Applications of Emerging Technologies on Noncarbonated Beverages .............. 240 8.3.1 Microbiological and Biochemical Stability ............................................. 240 8.3.2 Properties Modification ........................................................................... 245 8.4 Conclusion ......................................................................................................... 254 References.................................................................................................................. 255

Chapter 9: Labeling of Nonalcoholic Beverages .....................................................263 Igor Pravst and Anita Kuˇsar 9.1 Introduction ....................................................................................................... 263 9.2 The European Union Regulations on the Provision of Food Information to Consumers ..................................................................................................... 266 9.2.1 General Food Labeling............................................................................ 266 9.2.2 Front-of-Package Nutrition Labeling ....................................................... 272 9.3 Use of Nutrition and Health Claims ................................................................... 279 9.3.1 Nutrition Claims ..................................................................................... 280 9.3.2 Health Claims ......................................................................................... 283 9.4 The Use of Food Labeling to Support Monitoring of the Food Supply .............. 287 9.5 Conclusion ......................................................................................................... 300 Acknowledgments ...................................................................................................... 302 References.................................................................................................................. 302 Further Reading ......................................................................................................... 307

Chapter 10: Sparkling, Nonfermented, Nonalcoholic Beverages ............................309 Marı´a de Lourdes Samaniego-Vaesken, Teresa Partearroyo, Emma Ruiz and Gregorio Varela-Moreiras 10.1 Background ...................................................................................................... 309 10.2 Definitions, Regulations, and Classification ..................................................... 310 10.3 Ingredients and Nutritional Composition .......................................................... 312 10.4 Trends in Nonalcoholic Beverage Consumption............................................... 317 10.5 Contribution to Diet and Controversies ............................................................ 320 10.6 Conclusion ....................................................................................................... 321 References.................................................................................................................. 322

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Chapter 11: Soft Drinks: Public Health Perspective .............................................325 ˇ Nataˇsa Fidler Mis and Igor Pravst Nina Zupanic, 11.1 Introduction...................................................................................................... 325 11.2 Consumption Trends ........................................................................................ 328 11.3 Sugar-Sweetened Beverage Consumption and Regulation of Energy Intake ................................................................................................... 330 11.4 Sugar-Sweetened Beverage Consumption and Nutrient Intake ......................... 332 11.5 Sugar-Sweetened Beverage Consumption and Health Outcomes ...................... 334 11.5.1 Effect on Weight Gain and Fatness .................................................... 335 11.5.2 Effect on Oral Health ......................................................................... 339 11.5.3 Effect of Sugar-Sweetened Beverages on Cardiometabolic Diseases .............................................................................................. 342 11.6 Sugar-Sweetened Beverages, Insulin Resistance, and Type 2 Diabetes Mellitus ............................................................................................................ 343 11.7 Sugar-Sweetened Beverages and Cardiovascular Disease................................. 345 11.8 Possible Interventions to Reduce Sugar-Sweetened Beverage Consumption .... 347 11.8.1 Taxation and Sales Restrictions .......................................................... 347 11.8.2 Food-Labeling Systems ...................................................................... 350 11.8.3 Restrictions in Advertising of Sugar-Sweetened Beverages ................ 352 11.8.4 Individual Knowledge, Health Literacy, and Public Awareness Campaigns .......................................................................................... 354 11.8.5 School-Based and Other Educational Programs .................................. 355 11.9 Conclusion ....................................................................................................... 357 Acknowledgments ...................................................................................................... 357 References.................................................................................................................. 357

Index ............................................................................................................ 371

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List of Contributors Ibrahim M. Abu-Reidah Arab American University, West Bank, Palestine Karla Aguilar Universidad Auto´noma Metropolitana (UAM)
Unidad Iztapalapa, Ciudad de Me´xico, Mexico Pedro Esteves Duarte Augusto Department of Agri-Food Industry, Food and Nutrition (LAN), Luiz de Queiroz College of Agriculture (ESALQ), University of Sa˜o Paulo (USP), Piracicaba, Brazil Loreta Basinskiene Department of Food Science and Technology, Kaunas University of Technology, Kaunas, Lithuania Roberto Castro-Mun˜oz University of Chemistry and Technology Prague, Prague 6, Czech Republic; Institute on Membrane Technology, ITM-CNR, Rende, Italy; Nanoscience Institute of Aragon (INA), Universidad de Zaragoza, Zaragoza, Spain; Tecnolo´gico de Monterrey, Campus Toluca. Avenida Eduardo Monroy Ca´rdenas 2000 San Antonio Buenavista, 50110 Toluca de Lerdo, Mexico V. Chandrasekar ICAR-CIPHET, Ludhiana, India Dalia Cizeikiene Department of Food Science and Technology, Kaunas University of Technology, Kaunas, Lithuania Kriti Kumari Dubey Food Engineering and Technology Department, Institute of Chemical Technology, Mumbai, India Mustafa Gu¨zel Department of Food Engineering, Hitit University, C¸orum, Turkey Nihal Gu¨zel Department of Food Engineering, Hitit University, C ¸ orum, Turkey Madhura Janve Food Engineering and Technology Department, Institute of Chemical Technology, Mumbai, India Anita Kuˇsar Nutrition Institute, Ljubljana, Slovenia Ge´rard Liger-Belair Equipe Effervescence, Champagne et Applications (GSMA), UMR CNRS 7331, Universite´ de Reims Champagne-Ardenne, Reims, France Alberto Claudio Miano School of Agroindustrial Engineering, Universidad Privada del Norte (UPN), Trujillo, Peru Nataˇsa Fidler Mis Department of Gastroenterology, Hepatology and Nutrition, University Children’s Hospital, University Medical Centre Ljubljana, Ljubljana, Slovenia K. Muthukumarappan Department of Agricultural and Biosystems Engineering, South Dakota State University, Brookings, SD, United States Teresa Partearroyo Departamento de Ciencias Farmace´uticas y de la Salud, Facultad de Farmacia, Universidad San Pablo-CEU, CEU Universities, Urbanizacio´n Monteprı´ncipe, Alcorco´n, Madrid, Spain

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Igor Pravst Nutrition Institute, Ljubljana, Slovenia Aratrika Ray Food Engineering and Technology Department, Institute of Chemical Technology, Mumbai, India Meliza Lindsay Rojas Department of Agri-Food Industry, Food and Nutrition (LAN), Luiz de Queiroz College of Agriculture (ESALQ), University of Sa˜o Paulo (USP), Piracicaba, Brazil Emma Ruiz Spanish Nutrition Foundation (FEN), Madrid, Spain Marı´a de Lourdes Samaniego-Vaesken Departamento de Ciencias Farmace´uticas y de la Salud, Facultad de Farmacia, Universidad San Pablo-CEU, CEU Universities, Urbanizacio´n Monteprı´ncipe, Alcorco´n, Madrid, Spain A. Sangamithra Department of Food Technology, Kongu Engineering College, Perundurai, India S. Sasikala Department of Food Process Engineering, School of Bioengineering, SRM University, Kattankulathur, India K. Sava¸s Bahc¸eci Department of Food Engineering, Hitit University, C¸orum, Turkey Rekha S. Singhal Food Engineering and Technology Department, Institute of Chemical Technology, Mumbai, India G.J. Swamy Department of Agricultural and Biosystems Engineering, South Dakota State University, Brookings, SD, United States Gregorio Varela-Moreiras Departamento de Ciencias Farmace´uticas y de la Salud, Facultad de Farmacia, Universidad San Pablo-CEU, CEU Universities, Urbanizacio´n Monteprı´ncipe, Alcorco´n, Madrid, Spain Nina Zupaniˇc Nutrition Institute, Ljubljana, Slovenia

Preface Nonalcoholic drinks are nowadays the new trend in the market of beverages, facing a growing evolution. This is driven by the continuous introduction of innovations in many different aspects (e.g., reduced calorie content, flavor) of these products. Indeed, a renaissance of new nonalcoholic products has reached the market and subsequently research on this field has attracted great interest. Commercial nonalcoholic beverages (e.g., tea, coffee, cocoa, fruit smoothies, etc.) include an extensive and ever-increasing variety of products that are part of modern diet patterns, appreciated for their stimulant flavors and convenience of consumption while also being associated with leisure time and social activities. In addition, they contain numerous functional and nutritious ingredients like vitamins, antimicrobials, minerals, flavors, and antioxidants. The degradation of these compounds during processing and storage leads to degradation of the beverage itself and subsequently establishes its shelf life. However, with the recent advances in personalized nutrition and food processing fields (e.g., nonthermal technologies, modern encapsulation techniques, etc.), new developments, data, and state of the art come up in the field. Modern new product developers, food scientists, and technologists often deal with new product development and functional foods and, thus, more integral references are needed. The Food Waste Recovery Group (www.foodwasterecovery.group of ISEKI Food Association) has organized different training and development actions in the field of food science and technology, for example, teaching material (e-course, reference module, training workshops, webinars), an experts’ database, and news channels (social media pages, videos, blogs) aiming at disseminating knowledge and bridging the gap between academia and food industry. The group has also published books dealing with food waste recovery technologies, different food processing by-products’ valorization (e.g., from olive, grape, cereals, coffee, meat, etc.), sustainable food systems, innovations in the food industry and traditional foods, nutraceuticals and nonthermal processing, shelf life and food quality, and personalized nutrition as well as targeting applications of functional compounds like polyphenols, proteins, carotenoids, and dietary fiber. Following these efforts, Trends in Non-alcoholic Beverages aims at covering nonalcoholic beverages in view of the new advances in production technologies, stability, nutritional characteristics, and applications in the market. The ultimate goal is to support the scientific

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community, professionals, and enterprises that aspire to develop industrial and commercialized products. The book consists of 11 chapters. Chapter 1 introduces carbonated beverages (e.g. soft drinks, energy drinks and others) with an historical overview of nonalcoholic drinks starting from carbonated water up to today’s various carbonated drink categories. It also describes water treatment, carbonation, sugar dissolving, syrup production, packaging, marketing, and legislative issues. Olfactory sensations of carbonated beverages, marketing, and branding are all factors that contribute to a product’s success. Not long ago, the industry experienced major changes regarding product innovations and offerings. To face the growing market challenges, companies are bringing in new flavors taking into account the well-being and health concerns of consumers. The bottled sparkling water segment is a very competitive market, still looking for new insights and further development regarding carbon dioxide and bubble dynamics. Chapter 2 discusses theoretical and experimental observations relevant to common situations involving the conditioning and tasting of carbonated bottled waters, under standard tasting conditions. More generally, the very large area of nonalcoholic sparkling beverages could also certainly benefit from such developments regarding bubble dynamics and gas-solution thermodynamics. Beverages with properties to improve gastrointestinal health such as probiotics, prebiotics, and synbiotics are one of the most important segments within functional foods. In this line, Chapter 3 covers nonalcoholic and functional beverages based on cereals. Those products have recently gained a lot of attention, especially for medical reasons (lactose intolerance, cow’s milk allergy) or as a lifestyle choice. Depending on the processing steps involved, cereal-based beverages could be classified as nonfermented and fermented. Nonfermented beverages may be used in the form of stimulants such as tea and coffee, as refreshers like soft drinks and water, or as nutritional drinks such as dairy-milk substitutes. Cereal-based beverages are deficient in some basic components (e.g., amino acid lysine), but fermentation may improve their nutritional value and sensory properties. Tea and its consumption has also been claimed to be associated with beneficial health effects. Indeed, systematic scientific studies have proposed the beneficial effects of regular use of tea on modulating the initiation and propagation of cardiovascular diseases and carcinogenesis. Chapter 4 provides insights into the ready-to-drink teas available in the market, and discusses processing and manufacturing aspects, health benefits, bioavailability, and strategies to enhance and improve production. Chapter 5 provides a compelling overview of the most relevant applications for the production of nonalcoholic drinks (e.g., beer, wine, cider) by means of membrane-based technologies (e.g., nanofiltration, pervaporation, osmotic distillation, diafiltration, dialysis, reverse osmosis, membrane distillation, and membrane contactor). Particular attention is paid to experimental results which provide successful ethanol removal and minimal changes

Preface xvii on physicochemical properties of the beverages. In Chapter 6 trends and processing methods (advantages and drawbacks) in nonalcoholic beer production (biologically and physically via membranes) are discussed. Biological methods rely on altering process conditions and yeasts, whereas nonconventional yeasts have recently been emerging thanks to rapid advances in molecular biology. These yeasts include genetically modified strains and yeasts from non-Saccharomyces genus. Chapter 7 discusses processing of nonalcoholic beverages using nonthermal technologies. Considering product quality, consumers demand food with high levels of organoleptic and nutritional quality, but free of any health risks. The development of such kinds of products is usually connected with a reduction in the processing temperature, since thermal treatment often leads to loss of the desired organoleptic properties of fresh products and damage to temperature-labile nutrients and vitamins. Chapter 8 also deals with nonthermal technologies, targeting applications of high-power ultrasound, ultraviolet irradiation, highhydrostatic pressure, high-pressure homogenization, and pulsed-electric fields for the processing of noncarbonated beverages. After providing the fundaments and main mechanisms of these technologies, it describes microorganisms’ and enzymes’ inactivation, as well as physical and sensorial properties’ modification and nutritional composition changes. Chapter 9 presents the general rules for labeling of foods and drinks in the European Union, explaining mandatory information on food packages, including nutrition declaration, and provisions related with labeling of food allergens, additives, and other ingredients, as well as specifics related to added vitamins and minerals. Various front-of-package shames for labeling of nutritional composition or overall nutritional food quality are also presented, although the majority of those are not used in the European Union. In addition, examples of nutrition and health claims that can be used in Europe are denoted prior to focusing on possible uses of food labeling in research, for example, for monitoring the food supply. Chapter 10 draws an updated map of the nutrition facts in the different categories of nonalcoholic beverages in the European and Spanish market based on the information available on their labels, and also provides also an overview of the impact on diet quality. In fact, the increased consumption has been translated into important changes in diet quality (e.g., caloric and lipid profile). Finally, Chapter 11 provides a public health perspective on the consumption of soft drinks and sugar-sweetened beverages. Given the growing amount of scientific evidence emphasizing negative health impacts of sugar-sweetened beverages, dietary guidelines consistently recommend limiting added or free-sugar consumption, particularly in the form of sugar-sweetened beverages. In response, public health policies across the globe are taking actions to reduce their consumption. Conclusively, the book addresses food scientists and technologists, consultants, nutrition researchers, and food chemists working with food applications and food processing as well

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as those who are interested in the development of innovative products and functional foods. It could be used by University libraries and institutes worldwide as a textbook and ancillary reading for undergraduate and postgraduate level multidiscipline courses dealing with food science, food technology, and nutrition. It is important to highlight and thank all the authors for their dedication in this effort. Their accepting my invitation, editorial guidelines, and timelines are highly appreciated. I consider myself fortunate to have had the opportunity to collaborate with so many experts of nonalcoholic beverages worldwide including colleagues from the Czech Republic, Brazil, France, India, Italy, Me´xico, Lithuania, Palestine, Peru´, Slovenia, Spain, Turkey, and the United States. I would also like to acknowledge the acquisition editor Patricia Osborn, the book manager Katerina Zaliva, and all members of Elsevier’s publication team for their help during the editing and production process. Last, but not least, a message for all the readers of this book. This reference is a collaborative scientific effort of hundreds of thousands of words and, of course, it may contain some errors or gaps. Instructive comments, questions, or even criticism are always welcome, so please do not hesitate to contact me in order to discuss any issues concerning nonalcoholic beverages.

Charis M. Galanakis1,2 1

Food Waste Recovery Group, ISEKI Food Association, Vienna, Austria 2Research & Innovation Department, Galanakis Laboratories, Chania, Greece

CHAPTER 1

Carbonated Beverages Ibrahim M. Abu-Reidah Arab American University, West Bank, Palestine

Chapter Outline 1.1 Introduction 2 1.2 Ingredients 4 1.2.1 1.2.2 1.2.3 1.2.4 1.2.5 1.2.6 1.2.7 1.2.8 1.2.9 1.2.10 1.2.11 1.2.12 1.2.13 1.2.14 1.2.15 1.2.16

Water 4 Sweeteners 5 Acidulants 7 Preservatives 10 Carbon Dioxide 10 Flavors 11 Colorants 13 Carbon Dioxide Production 15 Carbonation (CO2 Impregnation) Process Syrup Preparation 17 Deaeration 18 Carbonators 18 Mixing Procedures 18 Filling Processes 19 Continuous Blend Production 19 Packaging 21

1.3 Types of Carbonated Beverages 1.3.1 1.3.2 1.3.3 1.3.4

1.4 1.5 1.6 1.7 1.8

Cola 23 Energy and Sports Drinks 23 Functional Beverages 24 Low and Mid-Calorie beverages

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Balancing of Acidity and Sweetness 25 Quality Standards 26 Regulatory Issues of Beverages 27 Economic Aspects 27 Quality Control 28 1.8.1 1.8.2 1.8.3 1.8.4

Ingredients 28 Syrup 29 Beverages 29 Packaging 30

Trends in Non-alcoholic Beverages. DOI: https://doi.org/10.1016/B978-0-12-816938-4.00001-X © 2020 Elsevier Inc. All rights reserved.

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1.9 Basic Considerations in the Soda Industry 30 1.10 Sensory Evaluation of Carbonated Soft Drinks 31 1.11 Recent and Future Advances and Trends 31 1.11.1 Insights and Perspectives

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1.12 Conclusion 35 References 35 Further Reading 36

1.1 Introduction The consumption of beverages in their various forms has taken place over many centuries to meet humanity’s fundamental requirement of hydration. The most obvious source of hydration is water; however, over time much of our drinking water has become very unsafe since it is often polluted by microorganisms (MOs). Outbreaks of dysentery, cholera, and other water-borne diseases were common in many European towns before the 20th century. Today’s beverage market is diverse and enormous. While carbonated beverages (CBs) might have been enjoyed as an occasional treat only one or two generations ago, now they are omnipresent and consumed by almost everyone. This can be seen from the global consumption of CBs, which reached more than 200 million liters in 2013. In spite of the decline of the volume of CBs consumed in recent years, it is clear that carbonated drinks continue to be very common refreshments. The first palatable carbonated water was produced by J. Priestley in England in 1767. A few years later, T. Bergman invented a system that produced carbonated mineral water on a commercial level. Then in 1783, Jacob Schweppes accomplished an efficient method for manufacturing carbonated mineral water and created the Schweppes Company-Geneva. From then on, the addition of flavoring substances to “sparkling” water developed to produce various and major soft drink brands all over the world. S. Fahnestock, in 1819, developed the soda fountain. The problem of loss of carbonation was avoided by the use of Crown corks and the automated production lines of glass bottles in the late-18th century. Since then, advances in the closing technology, bottles and "cans" design and manufacturing, syrup recipes, carbonation and filling machines have led to the giant worldwide beverage industry we currently know (D. Steen). The first flavored drink contained lemon juice (lemonade) and was sugared with honey or table sugar and is believed to have originated in Italy. The CB has its beginning in the study of mineral waters in Europe in the 16th century. In the late-18th century, artificial mineral waters were investigated for their medicinal properties in Europe and the United States. The first marketable artificial mineral water was manufactured in Europe during the

Carbonated Beverages 3 1780s and in the United States in the early 1800s. Flavored CBs, or soft drinks, were developed by chemists and apothecaries in the 19th century by the addition of flavored syrups to fountain-dispensed carbonated water. The introduction of proprietary flavors began in the late-1880s. Lazenby created the formula for Dr Pepper in 1885, while J. Pemberton settled the formula for Coca-Cola the next year. Brad’s Drink (Pepsi-Cola) was introduced in 1896. Poor flavoring, spoilage, and color constancy were the main obstacles that limited the past bottling progression. Improvements and innovations in bottling equipment, glass manufacturing, stable flavors, crown closures, ingredients, and transportation lead to the rapid growth of bottled soft drinks manufacturing. Soft drinks consist of carbonated water, nonnutritive and/or nutritive sweeteners, acidulants, preservatives, juices, flavorings, and colorants. Recently, the diversity of beverage products has burst. After an intensive decade or more of consolidation, innovation, and meeting consumer demand, the well-known marketers of liquid drinks have become, quite simply, beverage companies. Companies such as The PepsiCo, The Coca-Cola Company, and Schweppes’ Americas Beverages are identical with carbonated drinks. Their brands, Coke, Pepsi, and Dr Pepper, were first tasted in the late-19th century and became Americans’ most loved refreshments in the 20th century. A beverage is typically defined as a drink particularly prepared for human consumption. The word “beverage” originated from the French word boivre meaning “to drink.” Soft drinks provide hydration and quench thirst. A wide choice of these beverages are available in various tastes, including soda water, tonic water, diet/lite versions, herbal or botanical, energy, and carbonated drinks (Appleton et al., 2018; Ullmann’s Food and Feed, 2016). CBs are drinks that comprise dissolved carbon dioxide. The dissolution of CO2 in a liquid, gives rise to effervescence. This is a result of carbon dioxide pressure release from the solution. The carbonation idea started with naturally gassy mineral water. The presence of carbon dioxide in aerated water and soft drinks make them more palatable and visually attractive. Today, beverage manufacturers varying their palates based on the consumers’ desires and appetites. While 50 years ago the soft drink business produced cola and a few other flavors, currently there are low-calorie, mid-calorie, and no-calorie sodas. There are caffeine-free and caffeinated formulas. The tropical tastes have combined lemon-lime. In summary, there is a carbonated form for every appetite and taste. At some point, advanced technology can lead to greater efficiency of soft drink production during all the manufacturing stages. New methods of water pasteurization, sterilization, and clarification may advance production and diminish the need for preserving additives in soft drinks.

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Chapter 1

1.2 Ingredients 1.2.1 Water Water is the main single ingredient used in CBs, and must be of high purity. Many local municipalities supply drinking water that does not meet the requirements in terms of purity levels for use in CBs. Water must be treated to remove different types of impurities such as chemical (inorganic and organic substances), biological (microbiological contaminants), and physical (particulate matter) that may affect the organoleptic properties, namely the odor, taste, or appearance of the final drink. Water treatment in the beverage industry includes essential steps such as chlorination, coagulation, clarification, lime-softening, (ultra)filtration through sediment filter, or activated carbon filtration. Water for soft drinks must be pure and free from organic/ inorganic matters, heavy metals, and have low alkalinity. Water can be treated in the soft drink industry with chemical treatment, reverse osmosis (RO), monochromatic UV radiation, ultrafiltration (UF)/microfiltration, chlorination, and/or ion exchange to make it safe for soft drinks. 1.2.1.1 Chemical Treatment of Municipal Water Chemical treatment is used by most CB facilities. Treatment includes chlorination for disinfection purposes and oxidation of some impurities in the water. The water is then softened through the addition of lime to reduce alkalinity by removing magnesium and calcium bicarbonates. The reaction products formed as a result of the softening process are removed by coagulation. The coagulants, ferrous sulfate or potassium aluminum sulfate, react with the calcium or magnesium hydroxides to form precipitates. The precipitates settle out and are removed from the bottom of the reaction tank. Any residual precipitates are removed by passing the water through a sand filter. Activated carbon adsorption is used to remove chlorine and any other organic compounds, thus reducing the chance of undesirable odors or tastes. The water may then go through a final polishing stage of filtration to remove any carbon fines. 1.2.1.2 Reverse Osmosis In this process, the removal of most water contaminants is achieved. Water is passed at high pressure through a semipermeable membrane. Owing to the very small pore size, particulates and microbiological contaminants are retained on the membrane. Organic material and dissolved ions are affected by the charge on the membrane and are also retained. The membrane-filtered water can then be used for product water. RO is generally used as a polishing step for other water treatment methods.

Carbonated Beverages 5 1.2.1.3 Ultrafiltration This process removes particulate matter, macromolecules, pyrogens, and MOs by using thin and selectively permeable membranes. UF is generally employed as a polishing process, but cannot remove ions from water. 1.2.1.4 Ion Exchange Ion exchange, also known as demineralization, is used to eliminate inorganic matter from water. In this process, either a mixed bed of ion exchange resins or separate beds of cationand anion-exchange resins are employed. A cation-exchange resin replaces cations present in water, such as Ca12, Na11, Mg12, or K11 with hydrogen ions (H11). On the other hand, 2 21 22 an anion-exchange resin replaces anions such as CO21 with 3 , HCO3 , SO4 , and Cl 21 hydroxide ions (OH ). Fortunately, these resins can be regenerated and reused.

1.2.2 Sweeteners The sweeteners used in CBs can be either nutritive or nonnutritive. The quality of the sweetener is one of the utmost important parameters affecting the overall quality of the beverage. Important quality parameters should be taken into consideration when selecting the sweetener such as organoleptic profile (taste and odor), solubility, and microbial and temperature stability. 1.2.2.1 Nutritive Sweeteners These include sucrose in solution (syrup), granulated sucrose, dextrose, invert sugar, and high fructose corn syrup (HFCS). Sucrose [57-50-1], C12H22O11, obtained from cane or sugar beets was used in ancient times as the principal sweetener for CBs. In the presence of acids, sucrose is hydrolyzed to dextrose (D-glucose) [50-99-7], C6H12O6, and fructose [57-48-7], C6H12O6, to form a mixture which is called “invert sugar.” A change in the sugar profile changes the perception of sweetness in the beverage. Industrial invert sugar is used in stead of using the traditional method by allowing the sweetened beverage itself to invert over time. HFCS was first used in the beverage industry in the early-1970s. HFCS replaced sucrose as the primary nutritive sweetener for the beverage industry by 1984. HFCS is produced from corn starch through breaking down the starch into glucose, enzymatic conversion of glucose to fructose, separation of the sugars, and blending of the sugars to produce various percentages of fructose and glucose. Different HFCS types are available with varying concentrations of fructose and percentage of solids. The choice of sweetener is dependent on the final sweetness desired and the beverage formula. Manufacturers may choose to use blends of sweeteners and the most common blends consist of various concentrations of liquid invert sugar and HFCS. Normally, the percentage of sweetener used in a soft drink may range from 7% to 14% (White et al., 2015).

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1.2.2.2 Nonnutritive Sweeteners Diet or low-calorie beverages represent a significant share (B30%) of the total soft drink market. Currently, aspartame, saccharin, stevia, sucralose, neotame, alitame, and acesulfame K are the most commonly known nonnutritive sweeteners approved for use in beverages by the United States Food and Drug Administration (FDA) and European Union. 1.2.2.3 Saccharin (Sugar Twin), [81-07-2], C7H5NO3S Discovered in 1878, saccharin has the longest history of use of all the nonnutritive sweeteners, and was first available for commercial use in 1900. It was used in soft drinks as a blend with sucrose during World War I because of the shortage of nutritive sweeteners. Saccharin is 300
400 times sweeter than sucrose. The FDA formally approved its use in foods and beverages in 1938. However, in 1977 the FDA proposed a ban on saccharin as a bulk additive in foods. The US Congress has enforced and frequently renewed a moratorium on the proposed ban of saccharin in beverages. Saccharin is considered caloriefree. 1.2.2.4 Aspartame [22839-47-0], C14H18N2O5 Aspartame is the primary nonnutritive sweetener used in carbonated soft drinks. It is a lowcalorie and intense sweetener that is B200 times sweeter than sucrose (table sugar). It is used in a variety of foods and beverages including drinks, energy-reduced diets, and as a tabletop sweetener. Aspartame has been broadly used for over 30 years. Aspartame was first discovered in 1965 and received initial FDA and EU approval in 1981. Aspartamesweetened soft drinks can play an advantageous role to help people manage or reduce their intake of calories (https://www.unesda.eu/lexikon, 2019). Some sources consider aspartame as a nutritive sweetener due to its composition of the methyl ester of a dipeptide of L-phenylalanine and L-aspartic acid. It is sensitive to low pH and elevated temperatures and decomposes over time. Aspartame can be used alone or in blends with other sweeteners. 1.2.2.5 Sucralose, [56038-13-2], C12H19Cl3O8 Sucralose has a taste-quality and time-intensity profile closer to sucrose than any other sweetener. Sucralose is made up of one sucrose molecule attached with three chlorine atoms. The human body does not identify sucralose as a carbohydrate, and so it is poorly absorbed and generally excreted unchanged in urine or feces. Therefore it provides no calories. 1.2.2.6 Stevia Stevia is used around the world to sweeten beverages and foods. Bulking agents are normally used in some stevia sweetener formulas to add a palatable flavor and to reduce the

Carbonated Beverages 7 aftertaste. Four major steviol glycosides are found in the stevia plant, including rebaudioside A (reb A, stevioside , reb C, dulcoside A). In the scientific literature, Steviol glycosides are referred to as stevia, stevia glycoside, and stevioside. 1.2.2.7 Acesulfame-Potassium (Ace-K), [55589-62-3], C4H4KNO4S Ace-K was approved by the FDA in 1998 for use in beverages, and in 2003 as a general sweetener. Ace-K is often combined with other sweeteners in low-calorie foods and beverages. It possesses no glycemic impacts. Ace-K resembles saccharin in structure and taste profile and has a long shelf life. 1.2.2.8 Neotame, [165450-17-9], C20H30N2O5 At the present time, neotame is available to food manufacturers for sweetening processed foods but not directly to consumers for home use. Neotame is similar to aspartame, and is a derivative of the amino species, phenylalanine and aspartic acid. In 2002, neotame was approved by the FDA as an all-purpose sweetener. This sweetener has essentially the same qualities as aspartame, having no bitter or metallic aftertaste. Neotame is strongly sweet, with a sweetening power between 7000 and 13,000 times of sucrose. It is approximately 30
60 times sweeter than aspartame. 1.2.2.9 Alitame, [80863-62-3], C14H25N3O4S Alitame is an aspartic acid-containing dipeptide sweetener. Alitame is a second-generation dipeptide sweetener. Alitame has no aftertaste, and is around 2000-times sweeter than sucrose and B10-times sweeter than aspartame. Its half-life under hot or acidic conditions is about twice as long as aspartame, although some other artificial sweeteners, including saccharin and acesulfame K, are even more stable. 1.2.2.10 Sodium Cyclamate, [139-05-9], C6H12NNaO3S Sodium cyclamate is an artificial sweetener B30
60 times sweeter than sucrose and is the least strong of commercially used sweeteners. It can be mixed with other artificial sweeteners, particularly saccharin; the mixture of 10:1 ratio of cyclamate and saccharin parts, respectively, is commonly used to mask the off-tastes of the two types of sweeteners. It is cheaper than most sweeteners and is stable upon heating. The EU recognizes cyclamates as safe.

1.2.3 Acidulants Acidulants give beverages a sour or tart flavor, preservatives in microbial control, chelating agents, buffers, and facilitates the sucrose inversion process in sweetened beverages. The principal acidulants used in the CB industry are citric acid and phosphoric acid. Other

8

Chapter 1 Table 1.1: List of organic acids that are used in the carbonated beverage industry.

Name Adipic acid Malic acid Gluconic acid Fumaric acid Citric acid, monohydrate Citric acid, anhydrous Phosphoric acid Tartaric acid

Chemical Formula

pH

Tartness

C6H10O4 C4H6O5 C6H12O7 C4H4O4 C6H8O7.H2O C6H8O7 H3PO4 C4H6O6

2.86 2.35 2.80 2.15 1.85 3.20 2.68 3.40

Smooth tart Smooth tart Mild tart Tart Sharp tart Sharp tart Sharp tart Tart

Figure 1.1 Structures of main acidulant additives used in the carbonated drinks.

acidulants include tartaric, malic, and adipic acid (Table 1.1). Fig. 1.1 illustrates the structures of most commonly used acidulants in carbonated drinks. 1.2.3.1 Phosphoric Acid After citric acid, the second-most commonly used acidulant in the beverage industry is phosphoric acid as it is used in producing cola drinks which are sold extensively all over the world. This acid is recognized for its pungent, sharp taste that amazingly completes the flavor of cola. This acid is the primary acidulant in cola beverages. Phosphoric acid is stronger than most organic acids and weaker than other mineral acids. The dibasic properties of phosphoric acid provide a minor buffering capacity in the beverage. Food-grade phosphoric acid is commercially available in concentrations of 75%, 80%, and 85% and is one of the most economical acidulants. This acid comprises phosphorus, which is considered an essential nutrient and is one of the basic elements of nature. Phosphorus is also a major component of bones. All cola beverages contain 40
70 mg phosphorus per 350 mL serving (Massey and Strang, 1982).

Carbonated Beverages 9 1.2.3.2 Citric Acid This acid is used in a variety of flavored CBs, including lemon-lime, orange, other fruit flavors, and colas. Citric acid acts as an antioxidant by sequestering heavy metals. Citric acid is naturally found in most fruits, especially citrus. 1.2.3.3 Tartaric Acid Tartaric acid has a naturally sour taste and gives soft drinks a sharp tart flavor. It is the utmost water-soluble of all solid acidulants. It gives a strong tart-taste which enhances soft drinks’ flavors. Tartaric acid is often used to give a sour taste in lime- and grape-flavored beverages. It is one of the chief acids exist in soft drinks. Tartaric acid can preserve foods and it is often added to the CBs. 1.2.3.4 Ascorbic Acid Ascorbic acid, a form of vitamin C (L-ascorbic acid or ascorbate), acts primarily as an antioxidant and reducing agent as it is an added nutrient in beverages. It reacts readily with oxygen (oxidized), by which preventing the oxidation of certain flavoring components. It is used in foods as an antioxidant, preservative, or color stabilizer, and can be used for to boost food’s vitamin C content. Ascorbic acid is considered as a safe additive, with a lower incidence of adverse effects or other allergic reactions. It can be commonly used as antioxidant food additives in a variety of forms, including salts and esters such as, calcium, sodium, and potassium ascorbates, ascorbyl stearate palmitate, or ascorbyl palmitate. Ascorbic acid is industrially produced through a multistep process involving bacteria that reduce glucose and produce ascorbic acid as a by-product. The reduced pH of ascorbic acid may help to prevent microbial growth, thereby preserving freshness and preventing spoilage. 1.2.3.5 Malic Acid Malic acid is generally used for the production of low-calorie beverages. It is a bit cheaper in comparison to citric acid and can replace citric acid in some flavored CBs. Malic acid enhances fruit flavors in soft drinks by prolonging their release and so the recipient cells are stimulated for a longer period of time, which is translated by the brain as a stronger fruit flavor. Malic acid provides more acidity per unit of weight than other acidulants used in carbonated soft drinks. The result is that the weight of the acidulant packages weighed previously is reduced. It can also provide cost savings and is recommended for use in beverage syrup (0.03%
0.90%) by dissolving after the addition benzoates, if used, have completely dissolved.

10

Chapter 1 Table 1.2: Synthetic preservatives (antimicrobials) used in the soft drink industry.

Name

CAS Registry No. Chemical Formula

Potassium benzoate Sodium benzoate Potassium sorbate Sodium sorbate Ascorbic acid (vitamin C) Sulfur dioxide

[582-25-2] [532-32-1] [590-00-1] [7757-81-5] [50
81] [7446-09-5]

C7H5O2K C7H5O2Na C6H7O2K C6H7O2Na C6H8O6 SO2

Sorbic acid and its salts

[110-44-1]

C6H8O2

Use Preservative (antimicrobial) Preservative (antifungal) Preservative (antimicrobial) Preservative (antimicrobial) Preservative (antioxidant) and nutrient Preservative (antioxidant and antimicrobial) Preservative (antioxidant and antimicrobial)

1.2.4 Preservatives The carbonation and acid content in lemon-lime and cola beverages usually act as adequate preservation against microbial growth. Sorbate and benzoate or salts are frequently added to other beverages for such protection (Table 1.2). Sodium or potassium benzoates are universally used preservatives that act as active agents against yeast and mold at a concentration of B0.05%. Benzoate, if used in higher concentrations, can also act effectively against bacteria. It is highly effective when the pH is between 2.0 and 4.0. Potassium or sodium sorbates hinder the growth of yeast and mold most effectively at pH values below 6.5.

1.2.5 Carbon Dioxide Carbon dioxide [124-38-9] provides soft drinks with an acidic bite, pungent taste, and sparkling fizz. Carbon dioxide also acts as a preservative against mold, yeast, and bacteria. The carbon dioxide used in soft drinks must be of food-grade quality and impurity-free in order to avoid affecting the odor or taste of the final product. The carbonation measure mostly used is based on carbon dioxide volumes dissolved in 1 L of beverage at standard temperature and pressure conditions (0 C, 1 atm). Carbonation volume 5 1 signifies that 1 L of CO2 gas is dissolved in 1 L of beverage. Carbon dioxide gas is added to either the water used to prepare beverages or to the syrup plus water blend, depending on the production apparatus type. In both processes of carbonation, the pressurized CO2 gas is introduced into the system. The beverage carbonation is dependent on the temperature of the mixture and the pressure of the CO2. The beverage formulations can have varied concentrations of CO2. For instance, lemon-lime and cola beverages typically contain more carbonation than berryflavored or citrus beverages in order to achieve the required taste and flavor.

Carbonated Beverages 11

1.2.6 Flavors Flavor is the most significant quality factor of a carbonated drink. Flavors do not always make the same taste intensity and exact intended palate, since they can taste very different from one formula to another. Another aspect to consider is that the enjoyment of a certain drink might affect how much of it you drink. For example, research found that the flavor of sports drinks causes athletes to drink more than when consuming only water (Dennis et al., 2004). Consequently, drinks that are more palatable may be of benefit in increasing fluid consumption to avoid dehydration. Shelf life is another important issue since, over time, the flavor may intensify or decrease in intensity, or it may alter its character. Beverage flavoring appears to be a mysterious process at times; nevertheless, understanding the chemistry of a few ingredients goes a long way in the direction of success. The major part of flavors used in the CB industry are derived from natural sources. Most CBs encompass complex mixtures of diverse flavors formed in several commercial formulas, namely emulsions, alcoholic solutions, and concentrates. 1.2.6.1 Caffeine, [58-08-2], C8H10N4O2 Caffeine is usually added to cola beverages for its pleasantly bitter taste and used as a flavor additive in the soda industry. Cola beverages not containing caffeine are designated as caffeine-free. About 60% of soft drinks commercially available in the United States contain caffeine. Soda producers claim caffeine is added to CBs as a flavor enhancer. This caffeine flavor is dependent on the concentration used in the beverage. For instance, the concentration of caffeine in soft drinks may be below the detection threshold of flavor (Keast and Riddell, 2007). 1.2.6.2 Juice-Based Flavors Fruit juices are concentrated for use in CB flavors. The final juice is concentrated between four and six times its initial strength by removing water under vacuum, after which it is pasteurized. Carbonation of natural health drinks could be a great approach to develop new products. Carbonation of natural juices may enrich the taste, aroma, and nutritional value of the beverages. Juicy fruits such as lemon-lime and amla can be readily fabricated into carbonated drinks to produce new fruit drinks with thirst-quenching and refreshing properties. Orange, lemon, grapefruit, grape, and apple are the most common fruit juices used in CBs. 1.2.6.3 Essential Oils or Volatile Components Volatiles from plants are referred to as essential oils (EOs). An EO is “essential” because it contains the “essence of” the characteristic fragrance of that plant-derived oil.

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There are EOs can be obtained by means of different systems, including the direct extraction of the oils from pressed fruits, distillation, or solvent extraction. EOs mainly comprise terpenes, oxygenated compounds, and sesquiterpenes. The main flavor components of EOs are the oxygenated compounds. EOs are extracted from herbs, fruits, flowers, spices, and roots. Terpenes are typically readily oxidized, so they are often removed from the EO because they are insoluble, besides this, they may cause undesirable off-odors or flavors. One or more of the EOs for a given CB are often formulated. The particular aroma and taste of the carbonated drink is a result of the interactions of EOs with other sweeteners, flavorings, acids, and CO2. EOs choice and blend in the formulation of the beverages bases lies behind the so-called “secret of a soda drink” (Ameh et al., 2016). 1.2.6.4 Oleoresins In contrast to EOs, oleoresins are enriched with less volatile lipophilic compounds, namely fats, waxes, resins, and fatty oils. These oily deposits, derived from the solvent used in herb extraction, may contain more distinguishing flavors than EOs. The extraction solvent eliminates almost all of the flavor constituents of the herb. By distilling the extractive solvent, the solution can then be reduced into an oily residue. Oleoresins of interest and mostly used in the CB industry are celery, ginger, and black pepper. 1.2.6.5 Alcoholic Solutions or Extracts Alcoholic extracts are prepared by dissolving the flavor-bearing body in a solution of alcohol and water. They may require filtration using filter aids to remove any insoluble precipitates or oils that may form. Alcoholic extracts are clear solutions and are used in beverages that do not require a haze or cloudiness. 1.2.6.6 Fragrant Emulsions An emulsion is the mixture of EOs with an emulsifying agent such as gum acacia or tragacanthin that is then homogenized. The homogenization process increases the emulsion stability by reducing the size of its particles. For attaining a long-term stabile emulsion, it is crucial that the oil phase particles be of a certain size, generally not exceeding 5 μm. The specific gravity (SG) of the emulsion is altered using glyceryl abietate (ester gum) or brominated vegetable oil as weighting agents. Adjustment is necessary to keep the emulsion in proper suspension in the beverage. If the emulsion’s SG is less than the final product (beverage) due to the density ratio, emulsion will drift to the top, making a neck ring—a common problem in the beverage industry. Emulsions naturally produce a relatively cloudy beverage. One main feature of beverage emulsion is that it is very diluted, comprising at least 20 mg/L of a dispersed phase (oil) in the finished product, keeping in mind that it must

Carbonated Beverages 13 remain physically stable for a relative long period of time (up to 12 months). For instance, a citrus flavor (EOs extracted from lemon or orange peels) is one of the most common flavors used in the formulation of soft drinks. Since they are oily constituents (immiscible in water), to solve such matter the drinks made up with these oils are blended to form what is called oil/water (O/W) emulsions. 1.2.6.7 Concentrates These are blends of alcoholic solutions or emulsions with other fruit juice mixtures in order to yield a water-miscible solution. The concentrate may be straightforwardly used in syrup manufacturing, providing the needed consistent quality of the CB. The term concentrate actually applies to only one or more designated liquid parts that contain the EOs, colors, and other ingredients. The other part/parts are granular substances like buffers and preservatives which, during blending of the various parts, are combined as prescribed by the beverages’ labels. Concentrates of cola comprises EOs from cinnamon, coca, neroli, vanilla, nutmeg, lemon, orange, lime, and coriander. On the other hand, citrus carbonated drinks’ concentrates encompass citrus oils, where orange oil is dominant in orange concentrates while lime, lemon, and neroli oils are dominantly used in lemon-lime concentrates (Ameh et al., 2016). 1.2.6.8 Concentrated Flavor or Beverage Bases Parent soft drink companies may provide franchise bottlers with concentrated flavor or beverage bases that contain all of the necessary ingredients, with some exceptions. In some cases, preservatives, nutritive sweeteners, and some nonnutritive sweeteners may be acquired by the franchise bottler or can be packaged separately.

1.2.7 Colorants Colorants are either synthetically manufactured (artificial) or harvested from natural sources (natural). Synthetic colorants are certified additives by the FDA and are usually called primary colors which include shades of red, yellow, blue, and green. The certified primary colors are blended to form the secondary colors with/without the use of diluents. Acceptable food colorants can be designated as “certified” or as “approved” and consist of natural organic and synthetic inorganic colors used in particular applications in the food industry. Colorants can be in the form of powder, paste, granules, liquid, and others. Colorant determination includes stability, desired hue, and water solubility. Colorants also are used in beverages to deliver an added sensory appeal. CBs may contain some natural colors resulting from the use of natural juices or flavors, but commonly require additional coloring agents such as a caramel color or other artificial colors.

14

Chapter 1 Table 1.3: Commonly used artificial colors used in beverages.

FD&C Colors Yellow #5 Yellow #6 Red #40 Red #3 Green #3 Blue #1 Blue #2

Common Name

Type of Chemical

CAS Registry No.

Tartrazine Sunset Yellow FCF Allura Red AC Erythrosine Fast Green FCF Brilliant Blue FCF Indigotine

Azo Azo Azo Xanthene Triphenylmethane Triphenylmethane Sulfonated indigo

[1934-21-0] [2783-94-0] [25956-17-6] [16423-68-0] [2353-45-9] [3844-45-9] [860-22-0]

Caramel color is used in most cola flavored CBs. It is manufactured through carefully controlled heat treatment of a good-grade carbohydrate source, usually dextrose, and a chemical catalyst such as food-grade bases, acids, or salts. Caramel is generally found in single or double-strength preparations according to the color intensity required. The doublestrength formulation is used in most diet or low-calorie colas due to its lower caloric contribution than single-strength formulas. 1.2.7.1 Artificial and Natural Colorants Water-soluble colorants are designated as federal food, drug, and cosmetic act (FD&C), followed by the color name and number, for example, FD&C Blue #2. They have a corresponding common name, for instance, indigotine. The colors differ in hue, solubility, and other properties, according to the intended application. Water-soluble colors include FD&C Blue #1, Blue #2, Green #3, Red #40, Yellow #5, and Yellow #6; see Table 1.3 for more details. Water-insoluble colors are termed FD&C aluminum lakes. Lakes preparation involves the absorption of a certified dye on an insoluble substrate, that is, aluminum hydroxide, and per se embrace the colors standard. Lakes are usually used for dry ingredient coloring, increasing stability increasing, and also for color migration reduction. Lakes may also be used in coloring of foods with a high fat or oil content, as well as in coated candies and dry mixes, and for other targets. With regard to natural coloring agents, these are usually extracted from botanical sources and often contain several pigments, although they are not utilized as direct substitutions for FD&C colors. The colors have a reduced tinctorial strength which is attributed to the low amount of existing pigment and, thus, are used at higher amounts than FD&C colors. The stability of these colors is generally poor as their color and degradation rate are fairly easily affected by temperature, pH, and other conditions. Some natural colorings are listed in Table 1.4. Various-sized vessels are required for color mixing. Additional tanks may be also required for storage as in the case when large batches are made and left to stand for some

Carbonated Beverages 15 Table 1.4: Some natural colorants used in the beverages industry. Colorant

Source

Color Hue

Annatto Turmeric

Coating seeds of Bixa orellana tree Curcumin produced from turmeric root

Yellow to reddish-orange Greenish-yellow to yelloworange Red to red-orange Deep reddish-purple Yellow to orange Orange to red Orange to red Red Purple

Paprika Oleoresin Capsorubin and capsaicin, belonging to carotenoids Beet color Red beets β-Carotene Carrots, pumpkin, and sweet potatoes Canthaxanthin Sea weeds, mushrooms, algae, and some fish Lycopene Fruits (tomatoes, watermelon, papayas), carrots, and algae Anthocyanin Radish, red cabbage, and strawberry Purple sweet potato, purple potato, purple corn, and red cabbage Black bean, black rice, black carrot, and black currant Blueberry and concord grape

Black Blue

period of time. Tanks must be made of a corrosion-resistant stainless steel, for example, 304 or 316, in such a manner as to prevent acidic syrups causing a metallic off-taste. The entry of airborne and other contaminants can be prevented by using specially secured covers. It is crucial for the mixing vessels to have agitators of adequate size with appropriate capacity and speed to mix the viscous syrup within a particular time without damaging or destroying the delicate savor blends. Likewise, all other complementary parts and fittings such as valves, pumps, and lines must be of stainless steel or, at least, of an inert plastic material to avoid imparting any off-taste. After mixing, the syrup should be processed into the beverage as rapidly as possible. Several soft drink products may contain sensitive and delicate flavors that may lose some of their olfactory properties due to oxidation or acid hydrolysis if stored for too long. Syrups containing aspartame must be processed speedily because this nonnutritive sweetener loses some of its sweetness over time in a low pH environment. Shelf lives of finished syrups depend greatly on: (1) their particular ingredients; (2) their general flavor category; and (3) whether the storage tanks are refrigerated, which may greatly affect the syrup by retaining its flavor for longer.

1.2.8 Carbon Dioxide Production Numerous approaches for the manufacture of CO2 are in commercial use and include the reaction between sodium bicarbonate and sulfuric acid, fuel oil combustion, taking out of carbon dioxide from the flue gas of heating facilities, distillation of alcohol, and fermentation of beer. CO2 is also a by-product of the manufacture of fertilizer. After

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manufacturing CO2, the gas must be depurated to guarantee, and it has no impurities and is fitting for the desired purpose. Two characteristic processes are described next. 1.2.8.1 Fermentation When a sucrose- or other simple carbohydrate-based solution is mixed with yeast and oxygen in a fermenter, then alcohol and CO2 vapor are formed. The CO2 can, at this point, be passed through a separator to eliminate any trace of leftover foam. 1.2.8.2 Direct Combustion A hydrocarbon-based fuel such as natural gas or light oil can be specifically burnt in order to produce CO2. The flue gas from this process contains below 0.5% oxygen by volume and is chilled and scrubbed to get rid of any impurities that might exist. The resulting gas is then passed over an absorbing tower where it gets into contact with the absorbing solution of CO2.

1.2.9 Carbonation (CO2 Impregnation) Process Carbonation is the saturation of a liquid with CO2 gas. In other words, it is a term used to describe the dissolution of CO2 gas in water utilizing pressure and temperature. It typically includes cold CO2 under high pressure. CO2 is a nontoxic, inert gas that is virtually tasteless and is readily available at affordable cost. It is soluble in liquids and can exist in the three matter phases, namely as a solid, liquid, or gas. This process can occur naturally or by artificial processes, as is the case in most soft carbonated drinks and soda water. The maximum amount of CO2 that can be dissolved in water is 8 g/L. The excess of CO2 will normally only remain in water when the drink is under pressure. Or in other words, the CBs are prepared by mixing chilled flavored syrups with carbonated water in which carbonation levels range up to 3.5
5 g CO2 per liquid volume in colas and related drinks, while fruity ones, are less carbonated. The dissolved gas not only imparts a distinctive taste and sparkle to the beverage, but also acts against bacteria. CO2 is effective as an antiyeast because it tends to suppress the production of extra CO2 as a by-product resulting from the fermentation of sucrose to ethanol. In addition, it deprives molds of the oxygen needed for their growth. Soft drink beverages contain carbonation ranging from 1 to 5 volumes of gas per volume of liquid. Soft drink classification based on the degree of carbonation has been defined as: (1) 3.5 or more CO2 volumes (colas, tonics, or soda); (2) 2.5
3.5 CO2 volumes (lemon, lime, soda, or grapefruit); and (3) 1.0
2.5 CO2 volumes (strawberry, cherry, grape, orange, pineapple, or fruit punch). There are perhaps hundreds of carbonated drinks on the market with scores of natural and synthetic flavors. The ingredients of a typical carbonated soft drink include purified water that has been impregnated with CO2 gas, sweetening agents (dry or liquid

Carbonated Beverages 17

Pressure (atm)

300

200

Solid

Liquid

Critical point

100

0 –100

Gas –80

–60

–40

–20 0 20 Temperature (ºC)

40

60

80

Figure 1.2 Phase diagram carbon dioxide.

sugars, or/and nonnutritive sweeteners), acids (citric, gluconic, tartaric, and/or phosphoric), flavors (derived from fruit, vegetables, or artificial flavors), color (natural or artificial), preservatives, and other optional ingredients (e.g., vitamin C) (Ullmann’s Food and Feed, 2016). Carbonated drinks are very popular throughout the world. This acidic drink creates a mild tingling sensation on the tongue, which gives the CB its distinct taste (https://www. unesda.eu/lexikon, 2019). The gas can be straightforwardly liquefied by cooling and compression. CO2 gas is a tiny component of the surrounding atmosphere and forms about 1% by volume of dry air. In Fig. 1.2, the phase diagram of CO2 gas shows the effect of temperature and pressure on the three state phases of CO2 gas. At the triple point (5.11 bar and 256.6 C), by small disturbing of gas then the gas can arise in the three states as a gas, a liquid or a solid (state of equilibrium). At the critical point, at a temperature exceeding 31 C, it is impossible to liquefy the gas by increasing the pressure. CO2 is colorless at normal pressures and temperatures while at high concentrations it possesses a slightly pungent odor. Liquefaction is attained by cooling and compression by playing on the limits of pressure and temperature at the critical and triple points.

1.2.10 Syrup Preparation Most drink products are regularly prepared as a syrup-plus-water blend, in a ratio of 1-part: 3
6 parts water (volume/volume). Therefore a concentrated batch of syrup is made and then diluted with portions of water to make up the final product. For a sugar-based product

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the syrup conventionally consists of 67 Bx sugar, flavors, acid colorants, water, and preservatives. The different ingredients are weighed out and added to the mixing tank. In the syrup room, syrup is prepared and tested before sending it to the proportioner for mixing with water and carbonation. To accurately proportionate syrup and water, the most common contemporary systems use flow meters. Therefore syrup is dosed up using a mass flow meter while water is dosed up using a volume magnetic induction flow meter. This permits for density variations within the syrup to give the required Bx of the final product. The accuracy of the mass flow meters ensures the product has the required Bx, thus ensuring conformity adherence to specifications.

1.2.11 Deaeration The occurrence of air in a product causes product deterioration as well as giving a false reading of the level of CO2 present due to the partial pressures involved. Therefore by cumulative experience it has been revealed that the level of air within a product should be reduced to less than 0.5 ppm wherever possible. In such away, the risk of deterioration due to the presence of oxygen in beverages will be minimal, which results in an improved shelf life with minimized filling problems. The coexistence of CO2 and air may cause what is called nucleation sites inside the products, which leads to the fobbing phenomenon. The higher the content of air, the harder it is to keep CO2 in the solution. Two main methods of deaeration are vacuum and reflux, and both methods are normally applied to water before mixing with syrup. The most effective de-aeration method used involves atomization of water into a vessel held under a vacuum.

1.2.12 Carbonators The final product (mix) is fed to a vessel pressurized with CO2 gas which is judged by the pressure and flow rate of the CO2, which is critical to ensure the needed carbonation level. Therefore the greater the surface area of the liquid exposed to the CO2, the higher the rate of CO2 absorption will be in the liquid. The CO2 is often flushed into the liquid under pressure, which allows small gas bubbles to form, thus facilitating its absorbance by the liquid. A higher pressure yields smaller gas bubbles at the sparger and so a greater gas bubbles’ surface area will be obtainable from the CO2 gas to be absorbed by the liquid. Earlier carbonators utilized chilling for the carbonation process at about 4 C.

1.2.13 Mixing Procedures For each CB flavor there are special mixing requirements, but certain common principles may apply. Preservatives such as potassium or sodium benzoates are better dissolved in a

Carbonated Beverages 19 nonacidic solution. Thus preservatives are usually dissolved in a mixing vessel before adding acidulants or flavors. On the other hand, aspartame is better dissolved in acidic solutions and is usually added into the mixing containers after adding of the acidulants and flavors. A general mixing system is as follows: The required treated water is added, withholding a sufficient quantity to rinse all containers to remove all traces of ingredients. Afterward, the agitator is started. Preservatives (if applicable) are added and mixed until dissolved. Nutritive sweeteners (if applicable) are then added. Flavor concentrate is added, then containers are rinsed with the water withheld for this purpose. Nonnutritives (if applicable) are added. Any remaining water is added to complete the batch. Agitation is applied until entirely mixed (around 30
90 min). The syrup is tested for quality control parameters and then released to the production if a satisfactory analysis is obtained.

1.2.14 Filling Processes The filling process begins by mixing treated water and the syrup to beverage ratios and then the mixture is carbonated. The water, and occasionally the finished beverage mix, is often cooled to increase the filling speed and simplify the carbonation process. Empty beverage containers are rinsed, washed, and/or air flushed (depending on the package type) and then they are indexed at the filler. Containers are then filled and sealed by crowned (glass containers), capped (PET containers), or seamed (cans containers) methods. Afterward, the filled container is conveyed to packaging, casing, and finally palletizing for distribution. The filling system is fairly simple in terms of its design, but it can be further complicated by the wide range of products, packages, container materials, and various choices of secondary packaging. For example, dozens of brands of soft drinks are manufactured by the same facility. The packaging decision is based on many factors including the marketing plan, promotions, and the local market priorities. Fig. 1.3 shows a flow diagram of the manufacturing process of CBs.

1.2.15 Continuous Blend Production One of the latest advancements in the beverage manufacturing stream is the concentrate continuous blending directly to the beverage. This system is gifted with numerous advantages in comparison to the syrup batch conventional method that the finished syrup holding reservoirs are dispensable and beverage can be instantly blended. Another benefit of this system is that the total time for manufacturing beverages is significantly reduced.

Figure 1.3 Flow diagram of the manufacturing process of carbonated beverages.

Carbonated Beverages 21 In the continuous blend system, powder components and sufficient liquid beverage base components are predissolved. These are continuously measured and driven into the beverage mix. In this system, ingredients are blended using positive displacement pumps which operate by supplying constant flows and can meter exact amounts. The continuous blend process uses in-line ingredient monitors which enable the constant measure of the concentration of the ingredients. Up-to-date technological modernizations have resulted in in-line detectors capable of determining beverage components with the accuracy required for a quality beverage product.

1.2.16 Packaging Food packaging is mainly aimed at the protection of food products from external influences and damage, to contain the food, and to provide consumers with composition and nutritional value information. Other functions including traceability, convenience, and tamper indication are also of increasing importance. The objective of food packaging is to contain the foodstuff in a profitable way that satisfies consumer desires and industry requirements, sustains food safety, and diminishes environmental influence (Marsh and Bugusu, 2007). Competition is very strong in the market and brand equity is used to establish the position of a product. The type, shape, size, and graphics of the beverage’s container can help to differentiate one product from another. Those involved in the development of drink products need to be aware of the challenges concerning the commercial opportunities and marketing requirements so as to ensure that their development efforts line up with the brand’s strategy and costs. New trends in beverage packaging are concentrating on the structure modifying of the packaging materials and the advance of new active or intelligent systems, which can interact with the product or its environment, in turn, improve the conservation of soft drinks such as CBs and customer acceptability, in addition to food security. Glass and metals mostly offer an absolute barrier to environmental agents and other chemicals. The glass container seems to be more resistant to deterioration factors than polythene. In general, glass containers are described to be the best packaging material for liquid foods and beverages. Innovative tendencies in the stream of beverage packaging are being focused on the development of new materials with enhanced properties to control food-package-environment interactions. This can be achieved by surface treating the glass containers, which may be very promising for improving the hydrolytic resistance of the glass surface (Naknikham et al., 2014). Concerning plastic packaging materials, PET is increasingly used in beverage packaging for liquids such as cola and other carbonated drinks due to its excellent mechanical properties, UV resistance, clarity, and good oxygen barrier properties. Moreover, these properties can be improved by combining different films (multilayer PET) or by involving oxygen

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scavengers, which can reduce the oxygen content dissolved in the beverage and in the headspace, as well by limiting oxygen ingression which, in turn, might increase the shelf life (Bacigalupi et al., 2013). Recently, antimicrobials have been used to enhance the quality and safety of beverage packaging by reducing the surface contamination of processed food, reducing the growth of MOs population by the lag phase extension of MOs, or further by inactivating them (Brody et al., 2008). The development of antimicrobial packaging materials has increased over the past few years for use in beverage packaging by using different antimicrobial agents including nisin, natural EOs, silver ions, metal oxides, and organic acids. Recent innovations in packaging research and development have led to the development of novel sustainable materials as an alternative to the classic packaging systems. For example, starch-based packages, which have attracted considerable interest due to their biodegradability. Because of the increasing demand on biodegradability and sustainability, different designs and prototypes of environment-friendly packaging products have arisen to include the green fiber bottle (fabricated from cellulose fibers) and used in packaging of CBs (Bissacco et al., 2017). 1.2.16.1 Active and Intelligent Packages The packaging industry is focusing on providing a firm food security whereas sustaining the nutritional value. As a result, beverage packaging has evolved from simple containers to include different aspects, namely marketing, safety, material reduction, and environmentfriendly materials (Realini and Marcos, 2014). Therefore new technologies are being investigated in this research field, such as smart packaging and active packaging systems (Singh et al., 2011). 1.2.16.2 Active Packages Active packaging is aimed at extending the shelf life of foods by controlling the deterioration inside the package through the inclusion of antioxidants, antimicrobial agents, moisture absorbents, and oxygen scavengers in the packaging material. The innovation of this packaging type is based on reducing the deterioration of the food within the package and to reduce the need for the direct addition of chemicals to foods under controlled conditions (Scientific opinion on the Safety of Caffeine, 2018). 1.2.16.3 Intelligent Systems Currently three major technologies exist for realizing intelligent packaging (IP) of beverages, namely sensors, indicators, and radio frequency identification (RFID) systems. Recent investigations in the field of IP materials for beverages have led to the development of nanosensors and nanomaterials for the detection of food-relevant analytes such as foodborne pathogens, small contaminants, and adulterants or allergens in complex food matrices. Indicators deliver immediate visual information about the packaged food by

Carbonated Beverages 23 means of a color change and color intensity. Unlike sensors, indicators cannot provide information about the time, quantity, and data of measurement. On the other hand, RFID technology is distinguished from sensor and indicator IPs by having a distinct electronic information-based form of IP (Ramos et al., 2018).

1.3 Types of Carbonated Beverages Historically, ready-to-drink soft drinks were refreshing beverages that copied or extended conventional fruit juices. Carbonated drinks typically have about 10%
12% sugar content, mostly with a pleasant balancing acidity that varies from 0.1% to 1%. Addition of Caffeine from 8
10 mg per 100 mL of beverage. About 0.2%
0.5% of acid (i.e., citric or phosphoric acid) is added. A simple form of carbonated beverage should minimally contain such a mix of these basic components in water, with flavoring, coloring, and chemical preservatives added as necessary. To that mix, CO2 is added to give the product sparklingeffervescent-fizziness. For manufacturers to produce a carbonated juice-based product like lemonade, the process will involve adding 5%
10% fruit juice, which has a pleasing effect in appearance and taste.

1.3.1 Cola Carbonated drinks are very popular throughout the world. Cola is one of the most widespread flavors of soft drinks and is extensively offered throughout the world. The first formula of colas was developed by a French pharmacist, A. Mariani, in 1863. Modern colas consist of a blend of carbonated water, sugar or/and artificial sweetener, caramel for color, and acid (usually phosphoric acid) to balance the sweet-sour beverage taste. Colas also contain certain natural flavorings, including extract of cola leaf and other naturally derived flavors such as vanilla and spices such as cinnamon, caffeine (some colas are available without caffeine and are called decaffeinated), and certain food additives. In the EU, these additives are identified on the label as E-numbers. Individual recipes for colas are often strictly guarded secrets (https://www.unesda.eu/lexikon, 2019).

1.3.2 Energy and Sports Drinks The name energy drinks is used for high-caffeine beverages. Energy drinks are considered as functional beverages having a stimulating effect with unique combinations of characterizing ingredients including taurine, caffeine, vitamins, and other substances with a nutritional or physiological effect. They have been marketed for more than 25 years and safely consumed and enjoyed by consumers worldwide. The safety of the main ingredients of energy drinks has been assessed and confirmed by European institutions for risk assessment. Energy beverages only represent around 1% of the total European market of nonalcoholic drinks (Scientific opinion on the safety of caffeine, 2018).

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Sports drinks can prevent dehydration as they are a good source of electrolytes (potassium, sodium, magnesium, calcium) and carbohydrates. They are typically consumed before or during workout and exercise. These drinks normally contain a high sugar content (fructose, glucose, sucrose, and a glucose/maltodextrin mix) (Scientific opinion on the safety of caffeine, 2018). AlCon (besides for their calorific value), their high-caffeine content. Not all products within this category involve herbal extracts. Herbal extracts incorporated into energy drinks are typically obtained from stimulant herbs, the most commonly used being guarana (native to Brazil), which is considered as a natural source of caffeine. Other herbs with comparable levels of caffeine are coffee beans, kola nuts, mate, and teas. In addition to cocoa beans obtained from Theobroma cacao trees, the same family as kola plants except for their content of theobromine and theophylline stimulants, which are identical to caffeine in structure. Other alternative natural sources of effective stimulants having a place in energy drinks are those that support the concept of exercise or vitality in addition to guarana and kola. These are ginseng, muira puama, and damiana. Sports drinks, once accepted and consumed by athletes and gym goers, have seen manufacturers modify their target market to introduce them as everyday replenishments. Therefore new energy and sports drinks are destined to focus the mind and to provide both mental and physical alertness by using natural stimulants to assist consumers to deal with their day-to-day energy demands. Energy drinks have become popular among young people, mainly athletes, university students, and active individuals. Their main objective is to provide nutrition in addition to improved performance, concentration, and endurance (Alsunni, 2015). Numerous energy drinks are widely distributed in the market; of these, the most common ingredient is caffeine, which is frequently conjugated with other energetic substances, including guarana, glucuronolactone, taurine, and B-group vitamins, to formulate a blend that offers functional energy-boosting drinks. Remarkably, guarana also comprises significant amounts of caffeine, thus, its presence in an energy drink is noteworthy because it rises the overall caffeine levels in the drink. Ginseng also has important and manifold drug interactions (Vilela et al., 2018).

1.3.3 Functional Beverages The group of functional drinks includes wellness/lifestyle drinks, isotonic (drinks that rehydrate), medicinal tisanes, and meal substitutes. Currently, there is a growing consumer demand for healthy products that, besides nutritive value, boost human wellness. Recently, high and arising demand on beverage products fortified or enriched with ingredients of added health benefits (i.e. minerals, vitamins, ω-3 fatty acids, antioxidants, dietary fibers, and proteins) has been noticed (Piorkowski and McClements, 2014). Carbonated drinks are the most common category within the soft drinks market, in addition to functional ingredients, diet, and low-calorie varieties. Carbonates are likely to hold a

Carbonated Beverages 25 prestigious place within the functional drink sector in the near future. Similarly, dilutable drinks also account for a large proportion of soft drink consumption and, coupled with health and well-being trends toward functional beverages, dilutables are keeping pace. Here, superfruits, with the addition of vitamins and minerals, can be incorporated to produce cheaper and more convenient in-home functional drink varieties which can be included into the carbonated soft drinks category.

1.3.4 Low and Mid-Calorie beverages Today, low or zero-calorie beverages are favored by consumers since overconsumption of sugar-containing beverages is associated with becoming overweight or obese (Slavin, 2012). One obstacle in the distribution of low or zero-calorie drinks is the unpleasant taste caused by nonnutritive sweeteners. To overcoming this issue, new combinations have been innovated for producing mid-calorie beverages by blending sugars (sucrose or HFCS) with high-potency, nonnutritive sweeteners (sucralose, acesulfame K, and aspartame).

1.4 Balancing of Acidity and Sweetness The ratio of sugars to acids plays a key role in beverage preparation. Balancing sweetness and sourness significantly affects the total flavor profile. Acids add acidity to beverages besides helping to boost flavor and the perception of flavor. Commonly added acids include citric, malic, tartaric, and phosphoric acids. While phosphoric acid is most commonly added to colas, citric acid is added to most fruit-flavored drinks. Labeling requirements and cost can often affect determining which sweetening system to use. Sensory panelists describe the beverages sweetness profiles based on the onset (how fast the sweet taste is first perceived), build (time from onset of sweetness to its maximum intensity), and intensity (overall sweetness). Each sweetener or sweetener blend have their own profile in diverse beverage bases and may greatly impact the total flavor profile. For instance, by changing several combinations of sweeteners, the flavor profile of a cola converts from a mostly spicy blend to a dominant citrus profile. Sweeteners are made in different blends in order to get a synergistic effect of all the blend components and to complete each other’s sweetness character. For example, since ace-K’s sweetness commonly declines relatively quickly, it is often blended with aspartame to achieve longerlasting sweetness. The acid
sugar ratio of beverage bases plays a great role in the perception of the fruit flavors. This ratio may help to give the fruit its typical tartness and sweetness. Keeping in mind that the ratio may vary according to fruit maturity, that is, a ripe fruit will have a sugary and less-acidic taste than when the fruit is immature or green. In order to get a more authentic flavor, acids contained in a fruit may be added to the

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beverage. For example, strawberries contain mostly citric acid and very little malic acid. By blending different types of organic acids typically found in fruits, in such a way, formulators can assimilate the complete the original and natural flavor.

1.5 Quality Standards Quality control and food standards always go hand-in-hand and play a vital role in supplying clean, good, and standard-quality food products and beverages to consumers. Food standards are a body of rules directly concerning the food products whereas quality control helps in the maintenance of quality and composition at levels and tolerance acceptable to the buyers, while minimizing the cost of production as far as possible. Adoption of quality control and stipulation of food standards are very essential. The European Association of Industrial Gases working with the American Association of Compressed Gases and the International Association of Beverage Technologists has prepared a specification for liquid CO2 for use in foods and beverages. This is provided in Table 1.5, which illustrates the minimal standard factors that CO2 delivered to soft drinks and aerated mineral water bottles should fulfill. Table 1.5: Source specification of carbon dioxide used in the beverages industry (https://www. eiga.eu/index.php?eID 5 dumpFile&t 5 f&f 5 2872&token 5 7c1d5f281ad6d876a038a2de 4324 ea74e9961353, 2019). Component Assay Moisture Ammonia Oxygen Nitrogen oxides (NO2/NO) Nonvolatile residue (particulates) Nonvolatile organic residue (oil and grease) Phosphineb Total volatile hydrocarbons(as methane) Acetaldehyde Aromatic hydrocarbon Methanol Hydrogen cyanidea Total sulfur (S) Taste and odor in water Appearance in water Odor and appearance of solid CO2 (snow) a

Concentration 99.9% v/v min 20 ppm v/v max 2.5 ppm v/v max 30 ppm v/v max 2.5 ppm v/v max each 10 ppm v/v max 5 ppm v/v max 0.3 ppm v/v max 50 ppm v/v max of which 20 ppm v/v max nonmethane hydrocarbons 0.2 ppm v/v max 0.02 ppm v/v max 10 ppm v/v max 0.5 ppm v/v max 0.1 ppm v/v max No foreign taste or odor No color or turbidity No foreign odor or appearance

Analysis is necessary just in case CO2 is obtained from coal-gasification sources. Analysis is necessary just in case CO2 is obtained from phosphate rock sources.

b

Carbonated Beverages 27

1.6 Regulatory Issues of Beverages Regulations vary from country to country, and also differ over time as new legislation is decreed. It is a big challenge to give any all-purpose guidance, except to suggest that product development technologists use local food legislation experts, whose should keep up-to-date with the latest progresses in their national regulations. In the Euro zone and the United Kingdom, there are two main issues to address. First, herbal beverages should avoid incorporating levels of herbal extracts that are high enough to deem them liable for consideration as herbal remedies or medicines. The second matter is with regard to the product claims. Amended or new regulations are regularly being updated. Yet, the trend appears to be that manufacturers’ claims might be demanding a degree of authentication grounded on the scientific research.

1.7 Economic Aspects In the United States it is estimated that about 13% of all beverages consumed are alcoholic. Of the remaining nonalcoholic 87%, the most popular continues to be carbonated soft drinks, which accounted for about 30% of the overall total in 2015. However, over the past 7 years carbonated soft drinks’ share has slipped to some extent, while bottled water’s share has augmented by almost half. The global soft beverage market size was valued at about US$967 billion in 2016. The market is projected to grow at an estimated compound annual growth rate (CAGR) of 5.8% from 2017 to 2025 owing to factors including population growth and lifestyle change. Growing concerns about obesity and health awareness are likely to prompt the growth of the functional beverage and bottled water product sector, meanwhile limiting the demand for carbonated drinks. In the United States, the global carbonated soft drinks market had total revenues of US$286,295.7 million in 2015, representing a CAGR of 6.0% between 2011 and 2015. The volume of market consumption has increased to reach a total of 183,790 million liters in 2015. The United States has the world’s largest carbonated soft drinks market in terms of value and growth factors. Even though there is a growing concern about obesity and other health problems, which is reshaping the global nonalcoholic beverage industry, the demand for functional beverages, including relaxation drinks and energy drinks, is gaining popularity due to their low-calorie contents (Kleiman et al., 2011). Growing consumption of energy carbonated drinks due to hectic schedules, urbanization, and rising health concerns are expected to drive market growth. According to US Department of Economic and Social Affairs (2012), about 6 million people of the world’s population were added to the urban population every month. By this trend, roughly 60% of the global population will reside in urban areas by 2022, which is projected to boost industry growth. Population growth and disposable income together with the growing

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number of value-oriented smart consumers are developing the industry in general. The increase in the consumption of takeaway products due to busy lifestyles along with rapid urbanization is also expanding the market. It is anticipated that Asia Pacific, followed by the Middle East and Africa, will experience significant growth during the forecast period due to the presence of developing economies, high reusable income, and several available markets (https://www.prnewswire.com/news-releases/carbonated-soft-drinks-global-industryhad-revenue-of--2862957m-in-2015-and-is-expected-to-grow-further-by-2020-300457882. html 2019; https://www.statista.com/statistics/387318/market-share-of-leading-carbonatedbeverage-companies-worldwide/ 2019).

1.8 Quality Control Food quality control always play vital roles in providing clean, food products and beverages to the consumers. Food standards form a body of rules directly concerning food products, whereas quality control may help in the maintenance of composition, quality, and tolerance satisfactory to the buyers, while minimizing the price of production as much as possible. Quality control adoption and stipulation of food standards are indispensable. Also quality is important in preventing disease-causing microbial transmission in addition to other health consequences due to contaminants/adulterants as well as to limit the sale of unfair/substandard products and to simplify food marketing. Quality maintenance of CBs not only helps consumers in getting the desired quality products, but also promotes sales in the competitive markets. This can be achieved by exercising appropriate quality control measures at the three important phases, namely raw material, control process control, and finished product control.

1.8.1 Ingredients Ingredients used for CB manufacturing must satisfy all specifications of the Food Chemical Codex and also be permitted for use in soft drinks by the FDA or EFSA. In addition to the government specifications stated, CB manufacturers may complete further analyses depending on specific concerns or needs. Drinking water provided to CB manufacturing plants from private or municipal sources must comply with all the regulatory requirements. In the beverage industry, water resources are very important factors and form about 85%
92% of the beverages’ proportion. Rightly, water has been described as the elixir of life. Water obtained from diverse sources and places is not of the same quality and, therefore, detailed analyses are necessary to evaluate its quality, in particular for use in the beverage industry. This makes it compulsory to purify water for a certain purpose by special treatment. The beverage quality is highly dependent on the quality of various ingredients that go into its water, with sweetening agents, acids, flavor, color, and CO2, being the most

Carbonated Beverages 29 important. Besides, from hygienic/aseptic point of view, beverages’ producing units conditions need to be cautiously controlled in order to protect the public health (Kregiel, 2015). Although water is commonly used, the chemical reactions and physical changes brought about in commercial processing and in beverages are extremely complex. Since water is used in the process and is incorporated in many of the products, the various compounds dissolved in the water enter the physical and chemical reactions. Therefore it is of utmost importance that the water used in beverages is both chemically and bacteriologically satisfactory because of the danger of spoilage or the growth of fungi. In general, the quality requirements for water used in beverages are more stringent than those for drinking water or domestic supply. Complete absence or very low concentrations of MOs, organic matters, turbidity, displeasing color, taste and odor, iron, and manganese are highly desired. The water used for beverage manufacturing should have a satisfactory chemical quality comparable to the requirement of potable water. The samples intended for chemical analysis do not need sterilized containers. The water vessels and containers should be rinsed with the sample and then the sample should be filled up and labeled properly and sent to a laboratory for chemical analysis. Treated water must meet all "Environmental Protection Agency" guidelines (or similar legislations of each country) and may also be subject to additional state requirements. Treated water is routinely analyzed for odor, taste, appearance, alkalinity, chlorine, iron, pH, total dissolved solids, hardness, and microbiological contamination. Carbon dioxide used in carbonated drinks must be food-grade and should meet the specifications of the Compressed-Gas-Association commodity for CO2. In addition, CO2 is tested for purity, taste, and odor before being used in the production of beverages.

1.8.2 Syrup In representative manufacturing processes for syrup producing, some analytical parameters must be tested before beverage preparation or packaging. The sucrose or HFCS solids content is verified through the use of refractometers or density meters and reported as  Bx, Baume, % solids, or g/mL. The acidulant level is verified using spectrophotometric methods or titration. The concentration of preservatives may be confirmed using high pressure liquid chromatography. Syrups are also determined for proper color using colorimeters or spectrophotometric methods, besides the microbial contamination being tested.

1.8.3 Beverages The quality control of CBs encompasses all features of the product from the physical condition of the container to the actual chemical components of the drink. Laboratory tests

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are used evaluate in-line monitors. Beverage tests may include taste, syrup
water ratio,  Bx, and microbiological testing. First, beverages must be decarbonated by means of blenders, ultrasonic baths, or air-stone degassing units before evaluating the  Bx by the densometers, refractometers, or hydrometers. The decarbonated beverage is analyzed for acid content by using spectrophotometric methods or titration.

1.8.4 Packaging Incoming beverage packages are tested to ensure that they are in compliance with the specifications of the parent company. Refillable bottles are inspected visually after being washed to confirm that only undamaged and clean bottles are filled with the soft drink. To ensure the bottles integrity before the filling process, electronic inspection machines for bottles using the visual inspection are attached. Carbonation volume, closures, headspace, and weight are regularly checked for the packaged beverages. These latter issues are also usually tested at the startup of production and at different intervals during production. Carbonation in CB bottles is tested by means of Ashcroft or Zahm-Nagel carbonation gauges. The carbonation may be calculated from the temperature values and the pressure measured. In the case of canned beverages, the Zahm air tester is usually used to test for air content and carbonation. Removal torque test is measured for plastic or glass bottles having aluminum or plastic closures. The removal torque denotes the force required for closure removal from the bottle. Closures of bottles (PET or glass) are also tested to ensure their fit to the containers. Proper application test on crown closures is also performed. Packaged CBs are tested for net contents (weights) or fill height (headspace) to ensure that the package comprises the specified volume or weight of beverage. The target value for each package must conform with regulations of the individual state. Long-standing performances of carbonated drinks in plastic bottles may depend on several factors. Containers under evaluation would exhibit a high degree of creep resistance. Visible creep appearances may result in carbonation losses from PET bottles.

1.9 Basic Considerations in the Soda Industry For a liquid
gas mixture in a sealed container, it is said that there is an equilibrium when the gas rates that leave and enter the liquid solution are equal. By shaking a PET bottle of carbonated drink, the liquid
gas interface will fob at first, but then the equilibrium condition is reached. Fobbing is a term used within the CB industry denoting frothing of the product. Liquids with lower temperature will retain a greater amount of CO2. Conversely, the higher the temperature, the greater the pressure required to maintain the CO2 in solution. This phenomenon was expressed by Henry’s law and Charles’s law (D. Steen).

Carbonated Beverages 31

1.10 Sensory Evaluation of Carbonated Soft Drinks Sensory or organoleptic evaluation refers to the evaluation of food product by sense organs. All the sense organs are used in the judgment of food or drinks. Acceptance or rejection is based chiefly on the stimulus of sense organs of an individual. Therefore sensory qualities such as appearance, flavor, color, taste, mouth feel, and overall acceptability are to be evaluated by a trained panel of judges for evaluating the acceptability of the product using score cards established for evaluating the product for its qualities. The most broadly used scale for measuring food acceptability is the so-called 9-point hedonic scale. D. Peryam et al., established the scale at the QMFCI Institute aimed at determining soldiers’ food preferences. The scale was then rapidly adopted by the food industry sector, and is now used for measuring acceptability of food and beverages, among others (Peryam and Pilgrim, 1957). The 9-point hedonic scale is: like extremely; like very much; like moderately; like slightly; neither like nor dislike; dislike slightly; dislike moderately; dislike very much; and dislike extremely. The hedonic scale is the result of extensive research conducted at the University of Chicago and the QMFCI. The validity, reliability, and discriminative ability of the scale was proven in food acceptance tests in the field, laboratory, and in large-scale food preference surveys. Carbonated water represents over 92% of the soft drinks. CO2 adds that special sparkling and biting sense to the beverage besides acting as a preservative. CO2 is an especially fitting gas for soft drinks because it is nontoxic, inert, and relatively low-cost (Abdelazim et al., 2017). The organoleptic properties of carbonated soft drinks may be evaluated by a highly trained panel for color, flavor, taste, sweetness, and overall acceptability. Color is regarded as an important quality indicator, typically because it is the first sensual attribute the consumer experiences. Visual color intensity and tonality can provide more idea about the quality of the raw material used in the food preparation (Mielby et al., 2018).

1.11 Recent and Future Advances and Trends The soft drink sector is altering quickly. In 2001, Mountain Dew Code Red old brands were packaged in new forms when they proved successful. The common soft drinks were packaged in surprising ways. The industry also followed the demands of consumers when the “low-carb” movement began. Several leading brands reduced calories, carbohydrates, and sugars. Sodas fortified with calcium, vitamin C, and fruit juice appeared in 2004. Carbonated soft drink sales have declined, so the large names in the

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industry are trying to address consumer health concerns with new formulations and products. The renowned brands will fortify their drinks with minerals, vitamins, botanicals, and polyphenols. For instance, one drink may contain one ginseng extract along with added caffeine. Probably the most significant trend in soft drink manufacturing in recent years has been oriented toward the use of artificial noncaloric sweeteners. For instance, saccharin was used in soft drinks during and after the World War II, when sugar was scarce. Saccharin, is about 450-times sweeter than table sugar and it can be a significant cost reducer, but its conjugate bitter taste may displease some consumers. Not long ago, other artificial sweeteners were established, and today it is possible to produce soft drinks with almost all the characteristics of the taste of sugar, and while these products are almost free of any energy content, they also lack much of the cariogenic property found in sugary beverages. Innovative packages and packaging materials are being investigated. The search for nonnutritive sweeteners continues with the hope of a better taste for calorie-conscious consumers and a longer shelf life. Low-calorie sodas are obviously an area of improvement. More effectual methods, recipes, products, and equipment are being developed in this stream (Pereira de Abreu et al., 2012). The United States has been the biggest market in volume of CBs, with over 50 billion liters consumed in 2018. Almost all soft drinks are now available in the market in diet, lowcalorie, or lite formulas. These products have a low-energy content and can be cheaper to produce than the corresponding sugar-containing products. Conversely, consumption in Mexico and China, the next two biggest consumers of carbonated drinks, has augmented by 2.5% and 8.1%, respectively, per year since 2009. These growth rates will be less impressive going forward, but volumes in China and Mexico are approximately 40%
45% those of the United States in 2013. Like Mexico, per capita consumption of carbonated drinks in Brazil is high, though growth is limited somewhat as the market reaches maturity and consumer concerns over sugar in soft drinks increase. Emerging markets, such as Nigeria, India, and Iraq are expected to be among the fastest-growing markets, with an annual CAGR through to 2020 in the range of 9%
12% a year. Success in these dynamic markets requires significant capital investments and a long-term commitment to growing per capita consumption. PepsiCo announced by its Chairman that their branch in India will invest US$5 billion until 2020. He declared that Indian consumers, at the time, consumed only 236 mL bottles of Coca-Cola per year, compared with 230 bottles in Brazil and 92 bottles globally. In Mexico the federal government recently passed a tax on sugared soft drinks. This is likely to result in a decline in the volume of carbonated soft drinks produced. In China, the negative health image of carbonated soft drinks has been rising among consumers, leading to muted

Carbonated Beverages 33 growth in this category. The market is projected to grow .5% a year by 2018. Together, Coca-Cola and Tingyi-PepsiCo account for over 90% of the market in China. In the mature markets of Western Europe and North America, main cola companies are struggling to achieve growth in carbonated drinks as consumers shift to healthier alternatives, such as bottled water and ready to-drink teas. In the United States, carbonated soft drinks are expected to decline by an average of 0.3% a year through to 2020, and across Western Europe carbonated soft drinks are projected to grow by an average rate of about 1.5% through the same period. Total CB sales increased 2% to US$80.6 billion as soft drink makers aggressively pushed smaller packs at higher prices per ounce, while lowering the emphasis on large discounts packs, the Beverage Digest reported. To surpass the decline in consumption which may further affect CB sales, main soda makers such as The Coca-Cola Company and PepsiCo have adopted smaller pack sizes and premium packaging to drive margins in developed markets. They are also reformulating drinks with lower sugar levels and launching sugar-free options (D. Steen). Another area of development, and perhaps more obvious, is the constant search for new flavors and Nobel ingredients. Currently there is a great interest in the use of various botanical extracts, such as guarana and ginseng, due to their claimed qualities and healthy reputation, not forgetting the oldest and the most successful flavor, cola, which is a naturalbased extract of kola nuts. The third major area for development is that of soft drinks containing functional ingredients that enable some special nutritional or physiological claim to be made for the product. Of the other nutrients (other than carbohydrates) that can be included, fruit juice, vitamins, and minerals are the most common, but some products may contain significant levels of protein, phytochemicals, and even fibers.

1.11.1 Insights and Perspectives By 2023 it is expected that the global CBs market (GCBM) will reach US$412.5 billion, at a CAGR of 2.8%. Recently, the industry has experienced major changes with regard to product innovations and offerings. To confront the challenges related to such a growing market, companies are innovating new flavors while taking into account the well-being and health concerns of consumers (https://www.businesswire.com/news/home/20180831005393/ en/Global-Carbonated-Beverages-Market-Outlook-2023-Set, 2019). Today, the changing food habits in addition to the raising numbers of young people in developing countries has increased the market demand for carbonated drinks. The consumption of carbonated drinks is also enhanced with the increasing demand for processed foods. Due to the health concerns, consumption of carbonated drinks remains motionless in many parts of developed regions. Owing to consumer-health awareness,

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companies are now more focused on product innovations using natural and plant-based ingredients, for example, stevia sweeteners. The GCBM is segmented by geography, sales channels, product type, and flavor type. The basic flavors contributing to a majority of the market demand were found to be cola, orange, and lemon-lime. Nevertheless, to provide wider product assortment, companies are now focusing on tropical and super fruits-based drink product lines. Recently, new packaging technologies based on active and intelligent concepts will continue to evolve in order to increase the quality and shelf life of beverage products. The energy beverages sector has experienced high growth, which is forecast to continue. In addition to this, there has been significant innovation in this sector in that the energy drinks category is continuing to dominate the functional drinks. The energy drinks market globally reached over 5.8 billion liters in 2018, with an assessed value of US$41 billion alongside a growth in both value and volume. The category is continuing to dominate the functional drinks sector. which is developing after an early explosion on the market of beverages, and thus continuing to innovate and to grow. “Caffeine-free” energy drinks also belong to this category. One of the recent and key emergent topics belonging to this category is natural energy products, besides the increasing use of different plant extracts including ginseng, kola nut, tea, and guarana, most of which are available in CBs. Fig. 1.4 illustrates revenue by-products of the nonalcoholic beverage market estimated for the period from 2014 up to 2025 in US$ billion.

U.S. nonalcoholic beverage market revenue by product, 2014–2025 (USD billion)

162.0

171.8

2014

2015

2016

2017

2018

Carbonated soft drinks (CSDs) Functional beverages

2019

2020

2021

Fruit beverages Soft drinks

2022

2023

2024

2025

Bottled water Others

Figure 1.4 Revenue by-products of the nonalcoholic beverage market estimated in the period between 2014 and 2025 (US$ billion). From https://www.grandviewresearch.com/industry-analysis/nonalcoholic-beverage-market.

Carbonated Beverages 35

1.12 Conclusion Soft drinks are world-widely consumed in ever-increasing quantities and are of great commercial importance forming the basis of a worldwide industry, which carbonated beverages form a major part thereof. To confront the challenges related to this growing market, companies are innovating new flavors in view of the well-being and health concerns of consumers. The energy beverages sector has experienced continued growth and innovation in the CB sector. Particular attention is given to ingredients, including artificial and natural colorings, flavorings, and noncaloric sweeteners. Innovative packages and green-packaging materials seem to be forthcoming. Consumer mouth feel (tasting) a perceptive evaluation of the different products is considered as a quality parameter and used in the products evaluation and a resulting satisfaction guarantee will be essential for the future development and commercial competence throughout the beverages’ industry.

References Abdelazim, S.A.A., Masoud, M.R.M., Youssif, M.R.G., 2017. Micronutrients for natural carbonated and noncarbonated soft drink. J. Nutr. Health Food Eng. 7 (1), 204
212. Alsunni, A.A., 2015. Energy drink consumption: beneficial and adverse health effects. Int. J. Health Sci. 9 (4), 468
474. Ameh, S.J., Obodozie-Ofoegbu, O., Preedy, V.R., 2016. Essential oils as flavors in carbonated cola and citrus soft drinks. Essential Oils in Food Preservation, Flavor and Safety. Academic Press, San Diego, CA (Chapter 11). Appleton, K.M., Tuorila, H., Bertenshaw, E.J., de Graaf, C., Mela, D.J., 2018. Sweet taste exposure and the subsequent acceptance and preference for sweet taste in the diet: systematic review of the published literature. Am. J. Clin. Nutr. 107, 405
419. Bacigalupi, C., Lemaistre, M.H., Boutroy, N., Bunel, C., Peyron, S., Guillard, V., et al., 2013. Changes in nutritional and sensory properties of orange juice packed in pet bottles: an experimental and modelling approach. Food Chem. 141, 3827
3836. Bissacco, P., Stolfi, G., Leonardo, A.D.C., 2017. Characterizing green fiber bottle prototypes using computed tomography saxena. In: Proceedings of the 7th Conference on Industrial Computed Tomography (iCT 2017). Brody, A.L., Bugusu, B., Han, J.H., Sand, C.K., McHugh, T.H., 2008. Innovative food packaging solutions. J. Food Sci. 73, 107
116. Dennis, H.P., Mary, H., John, S., Robert, M., 2004. Palatability and voluntary intake of sports beverages, diluted orange juice, and water during exercise. Int. J. Sport Nutr. Exerc. Metab. 14 (3), 272
284. Keast, R.S.J., Riddell, L.J., 2007. Caffeine as a flavor additive in soft-drinks. Appetite 49 (1), 255
259. Kleiman, S., Ng, S.W., Popkin, B., 2011. Drinking to our health: can beverage companies cut calories while maintaining profits? Obes. Rev.: Offic. J. Int. Assoc. Study Obes. 13 (3), 258
274. Kregiel, D., 2015. Health safety of soft drinks: contents, containers, and microorganisms. BioMed Res. Int. 2015, 15. Article ID 128697. Marsh, K., Bugusu, B., 2007. Food packaging—roles, materials, and environmental issues. J. Food Sci. 72, R39
R55. Massey, L.K., Strang, M.M., 1982. Soft drink consumption, phosphorus intake, and osteoporosis. J. Am. Diet. Assoc. 80, 581.

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Mielby, L.A., Wang, Q.J., Jensen, S., Bertelsen, A.S., Kidmose, U., Spence, C., et al., 2018. See, feel, taste: the influence of receptacle colour and weight on the evaluation of flavoured carbonated beverages. Foods (Basel, Switzerland) 7 (8), 119. Naknikham, U., Jitwatcharakomol, T., Tapasa, K., Meechoowas, E., 2014. The simple method for increasing chemical stability of glass bottles. Key Eng. Mater. 608, 307
310. Pereira de Abreu, D.A., Cruz, J.M., Paseiro Losada, P., 2012. Active and intelligent packaging for the food industry. Food Rev. Int. 28 (2), 146
187. Peryam, D.R., Pilgrim, F.J., 1957. Hedonic scale method of measuring food preferences. Food Technol. 1957, 9
14. Piorkowski, D.T., McClements, D.J., 2014. Beverage emulsions: recent developments in formulation, production, and applications. Food Hydroc. 42, 5
41. Ramos, M., Valde´s, A., Mellinas, A.C., Garrigo´s, M.A.C., 2018. New trends in beverage packaging systems: a review. Beverages 1 (4), 248. Realini, C.E., Marcos, B., 2014. Active and intelligent packaging systems for a modern society. Meat Sci. 98, 404
419. Scientific opinion on the safety of caffeine, EFSA Panel on Dietetic Products, Nutrition and Allergies. ,https:// www.efsa.europa.eu/sites/default/files/scientific_output/files/main_documents/4102.pdf. (accessed 18.11.18.). Singh, P., Wani, A.A., Saengerlaub, S., 2011. Active packaging of food products: recent trends. Nutr. Food Sci. 41, 249
260. Slavin, J., 2012. Beverages and body weight: challenges in the evidence-based review process of the Carbohydrate Subcommittee from the 2010 Dietary Guidelines Advisory Committee. Nutr. Rev. 70, S111
S120. Steen, D., 2016. Carbonated beverages. In: Ashurst, P.R. (Ed.), Chemistry and Technology of Soft Drinks and Fruit Juices, third ed., Wiley-Blackwell. Ullmann’s Food and Feed, 2016. Wiley-VCH, ISBN: 978-3-527-69552-2, 3, 1576. Vilela, A., Cosme, F., Pinto, T., 2018. Emulsions, foams, and suspensions: the microscience of the beverage industry. Beverages 4 (2), 25. White, J.S., Hobbs, L.J., Fernandez, S., 2015. Fructose content and composition of commercial HFCSsweetened carbonated beverages. Int. J. Obes. 39, 76. ,https://www.unesda.eu/lexikon., 2019 (accessed 02.02.19.). ,https://www.eiga.eu/index.php?eID 5 dumpFile&t 5 f&f 5 2872&token 5 7c1d5f281ad6d876a038a2de 4324 ea74e9961353., 2019 (accessed 01.12.18.). ,https://www.prnewswire.com/news-releases/carbonated-soft-drinks-global-industry-had-revenueof
2862957m-in-2015-and-is-expected-to-grow-further-by-2020-300457882.html., 2019 (accessed 15.01.19). ,https://www.statista.com/statistics/387318/market-share-of-leading-carbonated-beverage-companies-worldwide/ ., 2019 (accessed 15.01.19.). ,https://www.businesswire.com/news/home/20180831005393/en/Global-Carbonated-Beverages-MarketOutlook-2023-Set., 2019 (accessed 08.01.19.). ,https://www.grandviewresearch.com/industry-analysis/nonalcoholic-beverage-market., 2019 (accessed 08.02.19.).

Further Reading Strunk Jr., W., White, E.B., 1979. The Elements of Style, third ed. MacMillan, New York, Chapter 4.

CHAPTER 2

CO2 and Bubbles in Sparkling Waters Ge´rard Liger-Belair Equipe Effervescence, Champagne et Applications (GSMA), UMR CNRS 7331, Universite´ de Reims Champagne-Ardenne, Reims, France

Chapter Outline 2.1 Introduction 37 2.2 Materials and Methods

39

2.2.1 Three Batches of Naturally Carbonated Waters 39 2.2.2 Measuring the Kinetics of Dissolved CO2 Progressively Discharging from Water 40 2.2.3 Measuring the Kinetics of Bubbles Growing Stuck on the Bottom of a Plastic Cup 41

2.3 Results and Discussion 2.3.1 2.3.2 2.3.3 2.3.4 2.3.5

42

Deciphering the Thermodynamic Equilibrium in the Sealed Bottles 42 The Kinetics of Dissolved CO2 Escaping from the Water Bulk after Pouring 45 The Kinetics of Bubbles Growing Stuck on the Bottom of a Plastic Cup 48 Is There a Critical Dissolved CO2 Concentration Required for Bubbling? 55 How Many Bubbles in Your Glass of Sparkling Water? 57

2.4 Conclusion 59 Acknowledgments 60 References 60 Further Reading 62

2.1 Introduction Potable water is an incredibly important aspect of our daily lives. Over the past 20 years, the global bottled water market has seen remarkable growth (Euzen, 2006; Storey, 2010; Rani et al., 2012), thus raising, in turn, legitimate environmental concerns regarding the waste management sector (Gleick, 2010). The Forbes magazine even declared that bottled water is expected to become the largest segment of the US liquid refreshment beverage market by the end of this decade (Forbes, 2014). In 2014, the global bottled water market stood at around 290 billion liters, and by value, it is expected to reach approximately US $280 billion by 2020 (Zion Research Analysis, 2015). Currently the sparkling water segment represents about 10% of the whole bottled water industry. Nevertheless, this percentage may vary a lot from country to country. In the Trends in Non-alcoholic Beverages. DOI: https://doi.org/10.1016/B978-0-12-816938-4.00002-1 © 2020 Elsevier Inc. All rights reserved.

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United Kingdom it is close to the global average, whereas in Germany, which is the biggest bottled-water market worldwide for premium waters, around 80% of the market is sparkling waters (Euzen, 2006). Sparkling waters are often seen as a substitute for sweet beverages, and this is particularly true for flavored sparkling waters (Rani et al., 2012). Suffice to say that the bottled sparkling water is a booming, but very competitive market, involving numerous companies throughout the world, with Europe being the largest producer (75%), followed by the United States (20%) (Bruce, 2013). Classification and labeling of bottled carbonated waters must conform with EU regulations (E.C. Council Directive 80/777/EEC and 80/778/EEC; E.C. Council Directive 2009/54/EC). Commercial bottled carbonated
natural mineral waters fall into three categories: (1) “naturally carbonated natural mineral water”, when the water content of carbon dioxide (CO2) comes from a spring and the bottle content is the same as at source; (2) “natural mineral water fortified with gas from the spring,” if the content of CO2 comes from the same resource, but the bottle content is greater than that established at source; and (3) “carbonated natural mineral water,” if CO2 comes from an origin other than the groundwater resource is added. Actually, a method using gas chromatography
isotope ratio mass spectrometry has been proposed to determine the carbon isotope ratio 13C/12C of CO2 (Calderone et al., 2007). This method was successfully applied to differentiate whether or not gas-phase CO2 in the headspace of bottled carbonated water originates from the source spring or is of industrial origin. In carbonated beverages, the concentration of dissolved CO2 is indeed a parameter of paramount importance since it is responsible for the very much sought-after fizzy sensation, and bubble formation (the effervescence). In sparkling waters and carbonated beverages in general, homogeneous bubble nucleation (ex nihilo) is thermodynamically forbidden (Wilt, 1986; Lubetkin, 2003). In order to nucleate, bubbles need preexisting gas cavities immersed in the liquid phase, with radii of curvature larger than a critical size. In carbonated beverages typically holding several grams per liter of dissolved CO2, the critical radius needed to initiate bubble nucleation (under standard conditions for pressure and temperature) is of order of 0.1
0.2 μm (Liger-Belair, 2014, 2016). This nonclassical heterogeneous bubble nucleation process is referred to as type IV nucleation following the classification by Jones et al. (1999). The presence of dissolved CO2 therefore directly impacts consumers of sparkling waters, by impacting several emblematic sensory properties such as: (1) the visually appealing frequency of bubble formation (Liger-Belair et al., 2006); (2) the growth rate of bubbles ascending in the glass (Liger-Belair, 2017); and (3) the characteristic tingling sensation in mouth. Carbonation, or the perception of dissolved CO2, involves a very complex multimodal stimulus (Lawless and Heymann, 2010). During carbonated beverage tasting, dissolved CO2 acts on trigeminal receptors (Dessirier et al., 2000; Kleeman et al., 2009; Meusel et al., 2010) and gustatory receptors via the conversion of dissolved CO2 into carbonic acid (Chandrashekar et al., 2009; Dunkel and Hofmann, 2010) in addition to the

CO2 and Bubbles in Sparkling Waters 39 tactile stimulation of mechanoreceptors in the oral cavity through bursting bubbles. More recently, Wise et al. (2013) showed that the carbonation bite was rated equally strong with or without bubbles under normal or higher atmospheric pressure, respectively. However, a consumer preference for carbonated water containing smaller bubbles has been previously reported in a thorough study on the nucleation and growth of CO2 bubbles following depressurization of a saturated CO2/H2O solution (Barker et al., 2002). Moreover, it was also clearly reported that high levels of inhaled gaseous CO2 become irritant in the nasal cavity (Cain and Murphy, 1980; Commetto-Muniz et al., 1987). For all these reasons, monitoring accurately the losses of dissolved CO2 in a glass poured with sparkling water is of interest for carbonated water elaborators. Over the past 15 years, the physics and chemistry behind effervescence has indeed been widely investigated in champagne and sparkling wines. A recent and global overview can be found in the article by Liger-Belair (2017). Nevertheless, and to the best of our knowledge, the bubbling process itself and the release of gaseous CO2 remained poorly explored under standard tasting conditions in sparkling waters. This chapter reports theoretical developments and experimental observations relevant to common situations involving the conditioning and tasting of commercial carbonated bottled waters. Bubble dynamics and progressive losses of dissolved CO2 were closely examined in a collection of three naturally carbonated waters (holding different levels of CO2) and poured in a plastic cup. The minimum level of dissolved CO2 required in a glass of sparkling water to enable bubble formation was theoretically discussed. Moreover, the issue of the number of bubbles likely to form in a single glass of sparkling water was theoretically derived to evidence the influence of various key parameters at play.

2.2 Materials and Methods 2.2.1 Three Batches of Naturally Carbonated Waters Three batches of various commercial carbonated natural mineral bottled waters from Poland, and provided by Danone Research, were investigated in previous research (LigerBelair et al., 2015). They are described and referenced as follows: 1. A low-carbonated water (labeled LCW). 2. A medium-carbonated water (labeled MCW). 3. A highly carbonated water (labeled HCW). MCW and HCW are conditioned in 1.5-L polyethylene terephthalate (PET) bottles, whereas LCW is conditioned in 0.7-L PET bottles. Concentrations of dissolved CO2 found in water samples were determined by using carbonic anhydrase (labeled C2522 carbonic anhydrase isozyme II from bovine erythrocytes and provided from Sigma-Aldrich in the United States) (Caputi et al., 1970). This method is thoroughly detailed in a previous

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Table 2.1: Concentrations of CO2 and non-CO2 dissolved gases initially held in the three various commercial carbonated waters sealed in PET bottles. Water Sample LCW MCW HCW

[CO2] ci (g/L)

[Non-CO2 Gases] (O2/N2) (mg/L)

3.25 6 0.08 4.53 6 0.15 6.87 6 0.28

17 8.5 9.5

paper (Liger-Belair et al., 2009). Non-CO2 gases (O2 and N2) were also approached through measurements based on the multiple volume expansion method (MVE) deduced from a typical CarboQC beverage carbonation meter (Anton Paar). Table 2.1 compiles the concentrations of CO2 and non-CO2 dissolved gases found in the three commercial carbonated waters used for this study. Actually, the level of dissolved gases found in the liquid phase is the main cause behind bubble nucleation and growth in sparkling beverages (Liger-Belair, 2017). Therefore it is worth noting that the very low concentrations of “non-CO2” dissolved gases compared to the relatively high concentrations of dissolved CO2 in water samples, has absolutely no impact considering the dynamics of CO2 bubbles in these sparkling waters (even with the LCW, which contains twice as much non-CO2 dissolved gases than the two other water samples). More details about the three batches of various commercial carbonated natural mineral bottled waters can be found in the articles by Liger-Belair et al. (2015, 2019).

2.2.2 Measuring the Kinetics of Dissolved CO2 Progressively Discharging from Water 100 6 2 mL of sparkling water was poured into a plastic cup, previously level-marked with 100 mL of distilled water. Experiments were performed at room temperature (20 C 6 1 C). Immediately after pouring, the plastic cup was placed on the chamber base plate of a precision weighing balance (Sartorius—Extend Series ED) with a total capacity of 220 g and a standard deviation of 6 0.001 g. The Sartorius balance was interfaced with a laptop PC recording data every 5 s from the start signal and activated just after the cup was placed on the weighting chamber base plate. The total cumulative mass loss experienced by the cup poured with water was recorded during the first 10 min following pouring. Actually, the mass loss of the cup poured with water is the combination of water evaporation, and dissolved CO2 progressively desorbing from the supersaturated liquid phase. The mass loss attributed to water evaporation only was simply accessible by recording the mass loss in a cup containing a sample of 100 mL of water first degassed under vacuum. Due to likely variations in hygrometric conditions from one day to another, standard evaporation was thus measured with a sample of water first degassed under vacuum, just before each series of total mass loss recordings was done. The cumulative mass loss versus time attributed only to gas-phase CO2 progressively desorbing from a sparkling water sample may, therefore, easily be accessible by subtracting the data series attributed to evaporation only from the

CO2 and Bubbles in Sparkling Waters 41 total mass loss data series. Generally speaking, in the area of sparkling beverages, the parameter which characterizes a sample is its dissolved CO2 concentration, denoted as cL , and usually expressed in g/L. The progressive loss of dissolved CO2 concentration with time after a sample of water was poured in a cup may, therefore, be accessed by retrieving the following relationship: cL ðtÞ 5 ci 2

mðtÞ V

(2.1)

with ci being the initial concentration of dissolved CO2 in water (given in Table 2.1 in g/L), mðtÞ being the cumulative mass loss of CO2 with time expressed in g, and V being the volume of water poured in the cup expressed in L (namely 0.1 L in the present case). Moreover, from a cumulative mass loss
time curve, the mass flux of CO2 desorbing from the water surface (denoted FCO2 ) is, therefore, experimentally deduced all along the degassing process in the flute, by dividing the mass loss Δm between two data recordings by the time interval Δt between two data recordings (i.e., FCO2 5 Δm=Δt). During the tasting of a sparkling water (and sparkling beverages in general), it is nevertheless indeed more pertinent to deal with volume fluxes rather than with mass fluxes of CO2. By considering the gaseous CO2 desorbing out of water as an ideal gas, the experimental total volume flux of CO2 (in cm3/s), denoted FT , is therefore deduced as follows all along the degassing process:
 RT Δm 6 (2.2) FT 5 10 MP0 Δt with R being the ideal gas constant (equal to 8.31 J/K/mol), T being the water temperature (expressed in K), M being the molar mass of CO2 (equal to 44 g/mol), P0 being the ambient pressure (close to 105 N/m2), Δm being the loss of mass between two successive data records (expressed in g), and Δt being the time interval between two data recordings (i.e., 5 s in the present case). To enable a statistical treatment, four successive pouring and time series data recordings were done, for each type of water sample. At each step of the time series (i.e., every 5 s), an arithmetic average of the four data sets provided by the four successive time series corresponding to a single water sample was done to finally produce one single “average” time series which is characteristic of a given water sample (but with standard deviations corresponding to the root-mean-square deviations of the values provided by the four successive data recordings).

2.2.3 Measuring the Kinetics of Bubbles Growing Stuck on the Bottom of a Plastic Cup 100 6 2 mL of sparkling water was poured into a plastic cup previously level-marked with 100 mL of distilled water. Immediately after pouring, the cup was placed on a “cold”

42

Chapter 2

backlight table (identical to the one used to visualize the cloud of bubbles following the pouring process). Experiments were performed at room temperature (20 C 6 1 C). Five minutes after pouring, bubbles growing stuck on the bottom of the plastic cup were monitored with time, through high-speed photography. A standard digital photo camera (Nikon D90) fitted with a macro objective (Nikkor 60 mm) was used for this series of observation. The growth of the bubbles’ diameters was monitored with time (during 30 s, i.e., from 5 up to 5 min and 30 s after pouring the water in the cup). It is worth noting that it was preferable to wait up to 5 min after pouring since the liquid bulk is highly agitated during the first minutes following pouring (mainly due to the turbulences of the pouring step and the high-bubbling activity) thus forbidding to focus accurately on bubbles stuck on the bottom of the cup. It is also worth noting that a close inspection of successive frames must be done in order to exclusively monitor the growth of bubbles growing by diffusion of CO2 (and not by coalescence with neighboring bubbles, which would artificially increase the kinetics of bubble growth).

2.3 Results and Discussion 2.3.1 Deciphering the Thermodynamic Equilibrium in the Sealed Bottles In a bottle of carbonated water hermetically sealed with a crown or a screw cap, the volume VG of gas phase in the headspace cohabits with the volume VL of water (i.e., the liquid phase), as seen in Fig. 2.1. For the sake of simplicity, we suppose that both volumes remain constant (i.e., we neglect the minute changes of the liquid volume due to the progressive dissolution of CO2 or even caused by dilation or retraction due to modifications of the bottle temperature). The capacity of CO2 to get dissolved in water is ruled by Henry’s law equilibrium, which states that the concentration cL of dissolved CO2 in the liquid phase is proportional to the partial pressure of gas-phase CO2 and is denoted as PCO2 : cL 5 kH PCO2

(2.3)

with kH being the strongly temperature-dependent Henry’s law constant of gas-phase CO2 in the liquid phase (i.e., its solubility) (Carroll and Mather, 1992; Diamond and Akinfief, 2003). Thermodynamically speaking, for a given gas species, the temperature-dependence of Henry’s law constant can be conveniently expressed with a Van’t Hoff-like equation as follows: 
 ΔHdiss 1 1 2 (2.4) kH ðTÞ 5 k298K exp 2 T 298 R

CO2 and Bubbles in Sparkling Waters 43

Gas phase with a volume VG, and with PCO2 VG = nG RT

VG

VL Liquid phase with a volume VL , and with n c L = L = k H PCO2 VL

Carbonated water

Figure 2.1 Scheme of the sealed bottle exemplifying the thermodynamic equilibrium experienced by dissolved and gas-phase CO2 between the liquid phase and the bottle gaseous headspace.

with ΔHdiss being the dissolution enthalpy of the gas species in the liquid phase (expressed in J/mol), R being the ideal gas constant (8.31 J/K/mol), and T being the absolute temperature (expressed in K). Under identical conditions of temperature, and applying Eq. (2.3), bottled water can therefore hold different levels of dissolved CO2 depending on the pressure of gas-phase CO2 found in the headspace below the crown or screw cap. Moreover, in the bottle hermetically sealed, the total number of moles of CO2 nT is a conserved quantity that decomposes into nG moles in the gaseous phase and nL moles in the liquid phase. Therefore nT 5 nG 1 nL

(2.5)

Moreover, in the realistic pressure range found in a bottle of carbonated water (a few bars), we may safely suppose that the gas phase is ruled by the ideal gas law. Thus

44

Chapter 2 PCO2 VG 5 nG RT

(2.6)

with T being the champagne temperature (in K), and nG being the number of gas phase CO2 found in the bottle headspace. Finally, in the bottle hermetically sealed, the thermodynamic equilibrium of dissolved and gas-phase CO2 always verifies the following system of equations, as schematized in Fig. 2.1: 8 n 5 n 1 nG > < T nLL cL 5 5 kH PCO2 (2.7) VL > : PCO2 VG 5 nG RT With the knowledge of the level of dissolved CO2 initially found in the three various carbonated waters used in connection with this study (see Table 2.1), the partial pressure of gas-phase CO2 in the sealed bottles can simply be determined through Henry’s law as PCO2 5 cL =kH . Actually, the Henry’s law constant of CO2 in water at 25 C (i.e., 298K) is close to 1.49 g/L/bar and the subsequent dissolution enthalpy of CO2 in water is ΔHdiss  19.9 kJ/mol (Lide and Frederikse, 1995). As a result, for bottles stored at 25 C, the partial pressures of gas-phase CO2 found in the three carbonated waters showing increasing levels of dissolved CO2 are expected to be 2.18, 3.04, and 4.61 bar, respectively. Moreover, with the knowledge of the respective headspace and liquid phase volumes found in each bottled water, and by using the system of Eq. (2.7) combined with Eq. (2.4), it becomes possible to determine the dependence on temperature of the partial pressure of gas-phase CO2 in the sealed bottles (see Fig. 2.2). Otherwise, and strictly speaking, in the sealed medium of bottled carbonated waters, water vapor in the headspace under the crown or screw cap is indeed under equilibrium with the liquid-phase water. Above the melting point of water, the strongly temperature-dependent 2O saturated water vapor pressure PH sat found in the bottle headspace is accurately determined according to the following and so-called Antoine equation:  O 2 5A2 log10 PH sat

B T 1C

(2.8)

 2O with PH sat being expressed in mmHg, T being expressed in degrees Celsius ( C), and the coefficients A, B, and C being provided by the NIST database (http://webbook.nist.gov/ chemistry). In the range of temperatures comprised between 1 C and 99 C, Antoine coefficients A, B, and C are 8.07131, 1730.63, and 233.426, respectively.

Nevertheless, by using the latter equation, it appears that the saturated water vapor pressure found in the headspace of the sealed bottles remains at least two orders of magnitude below the partial pressure of gas-phase CO2, as already noticed in the headspace of champagne bottles (Liger-Belair et al., 2017). Finally, the total pressure of the CO2/H2O gas mixture

CO2 and Bubbles in Sparkling Waters 45 6 LCW MCW HCW

5

2

PCO (bar)

4 3 2 1 0 0

5

10

15

20

25

30

T (°C)

Figure 2.2 Partial pressure of gas-phase CO2 within the sealed carbonated waters bottles in connection with the present study, as a function of the water temperature in the range between 0 C and 30 C.

found in a sealed bottle of carbonated water may safely be considered as being equivalent to the partial pressure of gas-phase CO2, whatever the bottle temperature in a reasonable range of tasting temperatures.

2.3.2 The Kinetics of Dissolved CO2 Escaping from the Water Bulk after Pouring As long as the carbonated water bottle is hermetically closed the capacity of a large quantity of CO2 to remain dissolved in the liquid phase is achieved by the relatively high pressure of gas-phase CO2 in the bottle headspace (through Henry’s equilibrium). The situation is thermodynamically stable. But, as soon as the bottle is opened and water is served in a glass the thermodynamic equilibrium of gas-phase CO2 is broken. Dissolved CO2 progressively escapes from the liquid phase to get into equilibrium with the partial pressure Patm CO2 of gas-phase CO2 found in ambient air (in the order of 0.4 mbar only). The corresponding new stable concentration of dissolved CO2 is ceq 5 kH Patm CO2  0:7 mg/L only  (following Henry’s law, at 20 C). Suffice to say that almost all dissolved CO2 initially held by sparkling water must desorb from the liquid phase. This progressive desorption is usually achieved after several hours. It is worth noting that dissolved CO2 escapes from the sparkling water into the form of heterogeneously nucleated bubbles, but also by “invisible” diffusion, through the free air
water interface (see Fig. 2.3). In Fig. 2.4, the progressive decrease of dissolved CO2 concentrations in the three water samples are displayed with time, all along the first 10 min following the pouring process. Quite logically, it is clear

Invisible diffusion of dissolved CO2 through the water surface

Gas desorption through heterogeneously nucleated CO2 bubbles

Figure 2.3 When the water is served in the plastic cup, dissolved CO2 escapes from the liquid phase through (A) the water free surface, and (B) bubbles heterogeneously nucleated on the cup’s wall. HCW MCW LCW

7

cL (g/L)

6

5

4

3 0

100

200

300

400

500

600

t (s) Figure 2.4 Progressive losses of dissolved CO2 concentrations (in g/L) with time, as determined with Eq. (2.1) from 100 mL of each of the three carbonated water samples poured into a plastic cup.

CO2 and Bubbles in Sparkling Waters 47 from Fig. 2.4 that the higher the initial dissolved CO2 level is, the more rapid the corresponding loss of dissolved CO2 is. Nevertheless, it is worth noting that the concentration of dissolved CO2 constantly remains higher in the HCW water, which holds the higher initial concentration of dissolved CO2, all along the first 10 min following pouring. This set of analytical data correlating the progressive loss of dissolved CO2 from carbonated water with time (under standard tasting conditions) could be of interest for consumers. Depending on the intensity of the tingling sensation promoted by dissolved CO2 in the mouth, the time to wait after pouring could be deduced for a given water type (depending on its initial level of dissolved CO2). Moreover, another pertinent analytical parameter which characterizes the release of CO2 from a sparkling beverage is the volume flux of gaseous CO2 escaping from the air/liquid interface (Mulier et al., 2009; Liger-Belair et al., 2013; Moriaux et al., 2018). Fig. 2.5 shows average CO2 volume fluxes outgassing from the cup poured with the three samples of various waters, respectively, as determined with Eq. (2.2). Moreover, since the driving force behind the desorption of dissolved gas species from a supersaturated liquid phase is its bulk concentration of dissolved CO2 (Liger-Belair et al., 2013), it seemed pertinent to propose a correlation between the CO2 volume flux outgassing from a cup poured with sparkling water and the continuously decreasing bulk concentration of dissolved CO2. To do so, time series data recordings displayed in Figs. 2.4 and 2.5 were combined. 1

CO2 volume flux (cm3/s)

HCW MCW LCW

0.1

0.01 0

100

200

300 t (s)

400

500

600

Figure 2.5 Gaseous CO2 volume fluxes (in cm3/s) desorbing with time, as determined with Eq. (2.2), from 100 mL of a carbonated water sample poured into a plastic cup.

48

Chapter 2 1

CO2 volume flux (cm3/s)

HCW MCW LCW

0.1

0.01 3

4

5

6

7

c L (g/L)

Figure 2.6 Gaseous CO2 volume fluxes (in cm3/s) desorbing with time as a function of the dissolved CO2 concentration (in g/L) found in 100 mL of a carbonated water sample poured into a plastic cup; standard deviations correspond to the root-mean-square deviations of the values provided by the four successive data recordings.

Time was eliminated so that the CO2 volume flux outgassing from the cup was plotted as a function of cL . Correlations between total CO2 volume fluxes outgassing from the cup, and dissolved CO2 concentrations found in the carbonated water are displayed in Fig. 2.6. It is evident from Fig. 2.6, that the three sparkling water samples explore three significantly different zones of dissolved CO2 concentrations and, therefore, clearly differentiate from one another from an analytical point of view.

2.3.3 The Kinetics of Bubbles Growing Stuck on the Bottom of a Plastic Cup 2.3.3.1 Required Background Bubbles stuck on the bottom of a plastic cup are considered as portions of spherical caps, with a radius r and a volume v ~ r 3 . Gaseous CO2 inside a bubble is considered as an ideal gas, which obeys the following relationship: PB v 5 nRT

(2.9)

with PB being the CO2 pressure in the bubble and n the number of gaseous CO2 moles in the bubble.

CO2 and Bubbles in Sparkling Waters 49 Actually, for bubbles with a radius greater than several tens of micrometers, the CO2 pressure in the bubble is in the order of ambient pressure P0 . Due to the spherical geometry of the bubble, the variation of the number of moles which crosses the bubble interface per unit of time, therefore, finally obeys the following relationship: dn P0 dv P0 2 dr  ~ r dt RT dt RT dt

(2.10)

The mechanism behind the growth of a bubble being molecular diffusion, the flux J of gaseous CO 2 which crosses the bubble interface obeys Fick’s law, which stipulates that: J 5 2 Drc  D

Δc λ

(2.11)

with D being the diffusion coefficient of CO2 in water, in the order of 1:8 3 1029 m2/s, at 20 C, as determined through 13C nuclear magnetic resonance by Liger-Belair et al. (2003), Δc 5 cL 2 c0 being the dissolved CO2 molar concentration difference between the water bulk and the bubble interface in Henry’s equilibrium with gas-phase CO2 in the bubble (see Fig. 2.7) and λ being the thickness of the diffuse boundary layer where a gradient of dissolved CO2 exists.

λ r

PB ≈ P0 CO2 bubble

Diffusion boundary layer

Water bulk supersaturated with dissolved CO 2

cL > c 0 c0

Layer in Henry’s equilibrium with gas phase CO2in the bubble, i.e., c0 ≈ kH P0 ≈ 1.7 g/L

Figure 2.7 Close to the bubble interface, the concentration of dissolved CO2 is in equilibrium with gas-phase CO2 into the bubble and equals c0 ; far from the bubble interface, the concentration of dissolved CO2 equals that of the liquid bulk cL ; in the diffusion boundary layer between, a gradient of dissolved CO2 exists, which is the driving mechanism behind the CO2 diffusion and therefore bubble growth.

50

Chapter 2

Therefore according to the spherical geometry of the growing CO2 bubble, the number of CO2 moles which crosses the bubble interface per unit of time can be expressed as: dn Δc ~ r2 J ~ r2 D dt λ

(2.12)

Generally speaking, diffusion of dissolved gas species may be ruled by pure diffusion or diffusion
convection whether the liquid phase is perfectly stagnant or in motion (Incropera et al., 2007). These two situations must therefore, a priori, be taken into account in our discussion. Pure Diffusion

In a purely diffusive case, a boundary layer depleted with dissolved gas molecules progressively expands near the bubble interface, that is, λ progressively increases so that the diffusion of gas species desorbing from the liquid bulk inexorably and quickly slows down. In case of a spherical geometry, the boundary layer depleted with dissolved CO2 progressively expands around the bubble cap in the form of a portion of spherical shell with a thickness λ. The mass conservation between the diffuse boundary layer and the spherical bubble cap may, therefore, be written as: dn ~ ðr1λÞ2 dλΔc

(2.13)

By combining Eqs. (2.12) and (2.13) and by integrating the corresponding equation, the progressive growth of the diffuse boundary layer may be deduced as time proceeds as follows:  λST  ðDtÞ1=2 for short times; i:e:; λ{r (2.14) λLG  r1=2 ðDtÞ1=4 for long times; i:e:; λcr Finally, by combining Eqs. (2.10), (2.12), and (2.14) and by integrating, the progressive growth of the spherical bubble cap growing by pure diffusion may be deduced through the following relationships: 8 RTΔc 1=2 > > for short times; i:e:; λ{r > < rðtÞ  P0 ðDtÞ (2.15)
2=3 > > 1=2 RTΔc > ðDtÞ for long times; i:e:; λcr : rðtÞ  P0

Finally, in case of a bubble growing stuck on the glass wall by pure diffusion, the bubble radius increases proportionally to the square root of time, that is, ~ t1=2 , as demonstrated in the pioneering work done by Scriven (1959) and conducted with a spherically capped bubble growing by pure diffusion on a solid substrate. When Convection Plays Its Part

In the case of a liquid medium agitated with flow patterns, convection forbids the growing of the diffusion boundary layer, thus keeping it roughly constant by continuously supplying the liquid around the bubble with dissolved CO2 freshly renewed from the liquid bulk.

CO2 and Bubbles in Sparkling Waters 51 By combining Eqs. (2.10) and (2.12) (with λ being constant), and by integrating, the progressive growth of the spherical bubble cap growing under natural convection conditions may be deduced through the following relationships: rðtÞ ~

RTD Δc t P0 λ

(2.16)

Finally, in case of a bubble growing under convection conditions, the bubble radius increases linearly with time, that is, ~ t. Therefore, by closely examining the kinetics of a bubble growth (via the critical exponent of the dependence of bubbles’ radii with time), it becomes possible to determine whether bubbles grow by pure diffusion or under convection conditions. 2.3.3.2 Experimental Results and Discussion A series of snapshots showing the progressive growth of bubbles stuck on the bottom of a plastic cup poured with HCW (during a 30 s period of time) are displayed in Fig. 2.8.

Figure 2.8 Time sequence showing bubbles growing stuck on the bottom of a plastic cup poured with the HCW carbonated water sample; the time interval between successive frames is 10 s (scale bar 5 1 cm).

52

Chapter 2

Figure 2.9 Time sequences extracted from the same global time sequence displayed in Fig. 2.8, aiming to compare the growth rates of different bubbles stuck on the bottom of the plastic cup. There is no doubt that the diameter of the single bubble far from neighboring bubbles (A) grows faster than the diameters of the three bubbles growing close to each other (B); the time interval between successive frames is 10 s (scale bar 5 1 mm).

A close examination of the time sequence displayed in Fig. 2.8 shows several coalescence events between bubbles growing close to each other. Coalescence events artificially increase the growth rate of bubbles and, therefore, the average bubble size distribution on the bottom of the cup. Moreover, it is also worth noting that bubbles growing very close to each other’s, but without coalescing, show growth rates much smaller than single bubbles growing far from their neighbors (see Fig. 2.9). In such cases, bubbles compete with each other for dissolved CO2. Bubbles literally “feed” with dissolved CO2 coming from the same environment, which contributes to decrease their respective growth rates. Such observations were also clearly evidenced in the article by Moreno Soto et al. (2018) where the growth of a pair of neighboring bubbles was accurately compared with the growth of a single bubble. Actually, it is clear by examining the growing bubbles displayed in Fig. 2.9 that, in the same period of time, the single bubble (S) grows faster than the three bubbles growing close to each other. Otherwise, in order to compare the respective bubble growth rates with each other in the various water samples, the progressive increase of various bubble diameters was systematically followed with time (for single bubbles growing as far as possible from neighboring bubbles, to prevent both coalescence and competition with regard to diffusion of dissolved CO2). Fig. 2.10 compiles the three various kinetics of bubble diameters’ increase with time (during a 30 s period of time, and 5 min after pouring) in the three various carbonated water samples. The general trend of data series unambiguously shows that bubble diameters increase linearly with time, thus confirming the likely growth of CO2 bubbles under convection conditions, as expressed in Eq. (2.16). It is indeed not really surprising to realize that bubbles stuck on the bottom of the cup grow under convection

CO2 and Bubbles in Sparkling Waters 53 3000 HCW MCW LCW

2500

d (μm)

2000

1500

1000

500

0 0

5

10

15

20

25

30

35

t (s) Figure 2.10 Bubble diameter versus time for single bubbles (far from neighboring bubbles) growing stuck on the bottom of the plastic cup, 5 min after pouring. The growth rate of bubbles from the three various carbonated water samples were compared with each other.

conditions. Actually, bubbles continuously detach from the plastic wall (through buoyancy), thus disturbing the whole water bulk with continuously renewed convection patterns. Such patterns forbid the growing of the diffuse boundary layer and keep it roughly constant around the bubble. Such growth under convection conditions has already been observed for heterogeneously nucleated bubbles in a glass of champagne (Liger-Belair et al., 2006). Nevertheless, and most interestingly, it is worth noting that in the work by Barker et al. (2002) the growth rate of CO2 bubbles following depressurization of a saturated CO2/H2O solution was not constant with time, despite dissolved CO2 concentrations comparable to those found in our set of experiments (i.e., several grams per liter). In the time data series compiled by Barker et al. (2002), bubble diameters rather followed a trend proportional to the square root of time, as in the purely diffusive case. Why is there such a big difference of scaling law, despite comparable dissolved CO2 concentrations in both studies? We are tempted to propose an explanation based on the liquid phase around CO2 bubbles growing by diffusion. In the work by Barker et al. (2002), before the sudden depressurization of the CO2/H2O solution, the liquid phase is indeed perfectly stagnant and therefore at rest. Bubbles, therefore, nucleate and grow in a liquid environment free from convection, thus leading to pure diffusion conditions (i.e., with a diffusion boundary layer growing around bubbles as the zone around bubbles progressively gets depleted with

54

Chapter 2

dissolved CO2). In our situation, under standard tasting conditions, the bubbling environment (i.e., bubbles detaching periodically from the bottom of the cup) continuously drives flow patterns around bubbles growing stuck on the cup. The liquid phase is far from being stagnant, thus keeping the diffusion boundary layer roughly constant, and forbidding purely diffusive conditions for bubble growth. In our set of diameters versus time data series, bubble growth rates may easily be accessed by linearly fitting the bubbles’ diameter increase with time (see Fig. 2.10 which compiles three various diameters vs time data series, in the three water samples). The slope of each data series, therefore, corresponds to the experimental growth rate, denoted as k 5 dr=dt, of a given bubble growing in the corresponding water sample. As seen in Fig. 2.10, the three water samples experience significantly different bubble growth rates. Logically, and as could have been expected, the higher the concentration of dissolved CO2 in the water bulk is, the more rapidly a bubble expands. Moreover, and following Eq. (2.16), the slopes of the various diameters versus time data series correspond to the theoretical prefactor in Eq. (2.16), that is, ðRTDΔcÞ=ðP0 λÞ. The only unknown parameter in this prefactor is the thickness λ of the diffuse boundary layer (kept roughly constant under convection conditions). Interestingly, the thickness of the diffuse boundary layer may, therefore, indirectly be approached in each water sample by equaling this theoretical prefactor with corresponding experimental bubble growth rates (k) as follows: λ

RTD Δc P0 k

(2.17)

By replacing in Eq. (2.17) each parameter by its numerical value, the thickness of the diffuse boundary layer has been determined for each carbonated water sample. It is worth noting that, because experimental growth rates (k) have been determined for bubbles growing stuck on the plastic cup 5 min after pouring, Δc in Eq. (2.17) should also be determined 5 min after pouring water in the cup (through the losses of dissolved CO2 with time given in Fig. 2.4 for the three carbonated water samples). Table 2.2 compiles the Table 2.2: Experimental bubble growth rates and corresponding thickness of the diffusion boundary layer around the growing bubble, as determined following Eq. (2.17) 5 min after pouring the three various carbonated waters (both parameters depending indeed on the difference in dissolved CO2 between the water bulk and the bubble surface in Henry’s equilibrium with gas-phase CO2 within the bubble). Water Sample LCW MCW HCW

Δc 5 cL 2 c0 (5 min After Pouring, g/L)

Bubble Growth Rate, k (µm/s)

Diffusion Boundary Layer Thickness, λ (µm)

1.36 6 0.09 2.45 6 0.18 3.88 6 0.42

962 13 6 2 28 6 6

155 6 47 187 6 45 136 6 47

CO2 and Bubbles in Sparkling Waters 55 pertinent data needed to reasonably approach λ in the three carbonated water samples. The thicknesses of diffuse boundary layers were found to be in the order of 100
200 μm around bubbles growing stuck on the plastic cup.

2.3.4 Is There a Critical Dissolved CO2 Concentration Required for Bubbling? Bubbling is the hallmark of sparkling waters. From the consumer point of view, the number and the size of bubbles likely to form in your glass are parameters of importance under standard tasting conditions. In a glass poured with sparkling water or a carbonated beverage in general, both the frequency of bubble formation and the growth of bubbles in your glass were found to strongly depend on the level of dissolved CO2 in the liquid phase (LigerBelair, 2014, 2016). The higher the level of dissolved CO2, the higher the frequency of bubble formation and the subsequent growth rate of the ascending bubbles. But is there a critical concentration of dissolved CO2 below which bubble production could become thermodynamically impossible? In other words, is there a minimum level of dissolved CO2 to overcome in your glass of sparkling water to enable the highly sought-after bubbling process? Bubble formation in a liquid phase supersaturated with dissolved CO2 is limited by an energy barrier to overcome—for exhaustive reviews about bubble nucleation, see the papers by Jones et al. (1999) and Lugli and Zerbetto (2007), and references therein. In sparkling waters, and carbonated beverages in general, bubble formation and growth require preexisting gas cavities, immersed in the liquid phase, with radii of curvature large enough to overcome the nucleation energy barrier and grow freely. It is the so-called nonclassical heterogeneous bubble nucleation, or type IV bubble nucleation, following the nomenclature defined by Jones et al. (1999). The critical radius required to enable type IV bubble nucleation, denoted r , can be determined by using simple arguments based on classical diffusion principles according to the following relationship, with every parameter being expressed in the MKS system of units (Liger-Belair, 2014): r 

2γkH cL 2 kH P0

(2.18)

with γ being the surface tension of the liquid
gas interface (  70 mN/m in sparkling waters), kH being the strongly temperature-dependent Henry’s law constant of CO2 in water (expressed in mol=m3 =Pa), P0 being the atmospheric pressure ( 105 Pa), and cL being the concentration of dissolved CO2 found in the liquid phase (expressed in mol/m3). Consider, for example, the LCW with a concentration of dissolved CO2 in a sealed bottle of 3.25 g/L (i.e., cL  74 mol=m3 ). Applying the latter equation, at 20 C, leads to a critical radius required to enable bubble nucleation of the order of 1.5 μm. Actually, closer inspection of glasses poured with carbonated beverages revealed that most of the bubble

56

Chapter 2

Figure 2.11 Two characteristic cellulose fibers stuck on the wall of a glass poured with champagne and providing nonclassical heterogeneous bubble nucleation from tiny preexisting gas cavities trapped within the fibers (reprinted from Perret, 2014) (bar 5 20 μm).

nucleation sites were located on preexisting gas cavities trapped inside hollow and roughly cylindrical cellulose-fiber structures of the order of 100 μm long with a cavity mouth of several μm. Two characteristic immersed particles acting as bubble nucleation sites in a glass poured with champagne are displayed in Fig. 2.11. It can be clearly noticed from Fig. 2.11 that the radius of curvature of the gas pockets trapped within the fibers is much higher than the critical radius r required for type IV bubble nucleation at 20 C (of the order of 0.15 μm for a typical champagne wine holding a high level of dissolved CO2 of the order of 11 g/L). Following Eq. (2.18), because the level of dissolved CO2 progressively decreases in a glass poured with sparkling water (as seen in Fig. 2.4), the corresponding critical radius required to enable type IV bubble nucleation progressively increases as time proceeds. Therefore under standard tasting conditions and for a given preexisting gas cavity with a radius of curvature r, the concentration of dissolved CO2 in the liquid phase will inexorably reach a critical value below which bubble nucleation will become thermodynamically impossible and, thus, precluding bubble formation. By considering a preexisting gas cavity immersed in the liquid phase (with a typical radius of curvature denoted r), the critical concentration of dissolved CO2 below which bubble formation becomes impossible derives from Eq. (2.18) as:
 2γ  (2.19) cL  kH P0 1 r

CO2 and Bubbles in Sparkling Waters 57 8 7

= 1 μm = 2 μm = 5 μm = 10 μm

20

25

5

*

c L (g/L)

6

r r r r

4 3 2 1 0

5

10

15

30

T (°C)

Figure 2.12 Temperature dependence of the critical dissolved CO2 concentration below which bubble nucleation becomes thermodynamically impossible from a preexisting gas cavity (with a radius of curvature r) immersed in the liquid phase. Gas cavities with four various radii of curvature were investigated (namely 1, 2, 5, and 10 μm, respectively). 

It is worth noting that cL is highly temperature dependent, because kH is highly temperature  dependent (Liger-Belair, 2016). The temperature dependence of the critical concentration cL below which bubbling would become thermodynamically impossible is plotted in Fig. 2.12 for a preexisting gas cavity with a radius of curvature of 1, 2, 5, and 10 μm, respectively. It can, thus, be concluded that the colder the sparkling water, the higher the critical concentration of dissolved CO2 below which bubbling becomes thermodynamically impossible in your glass. Moreover, the smaller the radius of curvature of the preexisting gas cavity (and, therefore, the smaller the particle or the glass anfractuosity responsible for the bubble nucleation process), the higher the subsequent critical concentration of dissolved CO2 below which bubbling becomes impossible. From the point of view of the consumer, the bubbling process will simply stop from a given bubble nucleation site as the level of dissolved CO2 (which continuously decreases after pouring the sparkling water in a glass) will reach the critical dissolved CO2 concentration defined above.

2.3.5 How Many Bubbles in Your Glass of Sparkling Water? The falsely naı¨ve question of how many bubbles are likely to form in a single glass of bubbly was investigated recently (Liger-Belair, 2014). This number was found to be the

58

Chapter 2

result of a complex interplay between the initial level of dissolved CO2 found in the glass after pouring, tiny preexisting gas cavities trapped within particles or glass anfractuosities acting as bubble nucleation sites, and ascending bubble dynamics. In a glass of sparkling water, the physicochemical processes being basically the same, the same reasoning set out for champagne poured into glasses may, therefore, apply to address this question with confidence. Under standard champagne tasting conditions, the whole number of bubbles likely to form per glass was found to depend on various parameters of both the liquid phase and the glass itself, according to the relationship (Liger-Belair, 2014):
 2 3 107 V ρg 2=3 cL 2 kH P0 ln  (2.20) N h T cL 2 kH P0 With V being the volume of water served in the glass, ρ being the champagne density (close to 103 kg/m3, very close to the density of water), g being the gravity acceleration (close to 10 m/s2), and h being the distance traveled by a bubble from its nucleation site to the liquid surface (considered as being the water depth in the glass, if most of the bubble nucleation sites are located on the bottom of the glass). 

Replacing in Eq. (2.20) cL by its expression given in Eq. (2.19), and replacing ρ and g by their respective numerical values finally leads to the following relationship, which provides the total number of bubbles likely to form in the glass as a function of various parameters depending on both glass and liquid properties (expressed in the MKS system of units):
 1010 V rðcL 2 kH P0 Þ N ln (2.21) 2kH γ hT 2=3 with V being expressed in m3, T in K, h in m, r in m, cL in mol/m3, P0 in Pa, kH in mol/m3/Pa, and γ in N/m. In Fig. 2.13, the total number of bubbles likely to form in a very typical glass poured with 20 cL of sparkling water and with a reasonable water depth of 10 cm, is plotted as a function of the dissolved CO2 concentration found in the liquid phase. Four tasting temperatures were investigated (namely 5 C, 10 C, 15 C, and 20 C). An identical average radius of curvature r  5 μm was considered for the preexisting gas cavities immersed in the liquid phase and acting as bubble nucleation sites. It is worth noting from Fig. 2.13 that the total number of bubbles likely to nucleate in a glass poured with a sparkling water logically increases with the level of dissolved CO2 found in the water. Moreover, and most interestingly, the total number of bubbles likely to nucleate in a glass increases with the tasting temperature of water (for a given level of dissolved CO2). As shown in Fig. 2.12,  the critical dissolved CO2 concentration cL decreases with increasing liquid-phase temperature. Therefore by increasing the tasting temperature of water, the total number of

CO2 and Bubbles in Sparkling Waters 59

N (bubbles)

106

5°C 10°C 15°C

10

5

20°C

2

3

4

5 cL(g/L)

6

7

8

Figure 2.13 Theoretical total number of CO2 bubbles likely to form in a typical glass poured with 20 centiliters of sparkling water (and with a water depth of 10 cm) plotted as a function of the dissolved CO2 concentration found in the liquid phase. Four tasting temperatures were investigated (namely 5 C, 10 C, 15 C, and 20 C). It is noteworthy to mention that an identical average radius of curvature r  5 μm was considered for all the preexisting gas cavities acting as bubble nucleation sites in the glass poured with sparkling water.

bubbles likely to form in the glass will increase because bubbles will be able to form at increasingly low dissolved CO2 concentrations.

2.4 Conclusion The thermodynamic equilibrium of gas-phase and dissolved CO2 relevant to the conditioning of carbonated bottled waters was presented in this chapter. In the range between 0 C and 30 C, the dependence in temperature of the CO2 pressure found in three various carbonated bottled waters sealed with a screw cap and holding different levels of dissolved CO2, was described. Under standard tasting conditions, the three commercial carbonated natural mineral bottled waters presented here clearly showed very significant differences regarding their bubbling behavior as well as their kinetics of dissolved CO2 escaping the water bulk. It is no wonder then that such differences impact the sensory properties experienced by a consumer enjoying a glass of carbonated water. Moreover, and most interestingly, the diameter of bubbles stuck on a plastic cup was found to increase linearly with time (i.e., with d ~ t), thus betraying a diffusion process of dissolved CO2 from

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the water bulk to the bubbles operating under convection conditions (likely because bubbles continuously detaching from the plastic cup give rise to renewed flow patterns in the water bulk, thus forbidding the growing of the diffuse boundary layer around the bubbles). The minimum level of dissolved CO2 to overcome in your glass of sparkling water to enable bubble formation was theoretically derived and was found to strongly depend on the tasting temperature of water. Finally, based on a previous study conducted on the physicochemical processes at play in a single glass of champagne, the falsely naı¨ve question of how many bubbles are likely to form in a glass of sparkling water was theoretically discussed and modeled as a function of several parameters of both the liquid phase and the glass itself. These experimental observations and theoretical developments, relevant to common situations involving the service of commercial carbonated bottled waters, could certainly be extended more generally to the very large area of nonalcoholic sparkling beverages, also looking for new insight and novelties. Actually, bubble dynamics in sparkling alcoholic beverages have indeed been widely investigated over the past decade, mainly with champagne, sparkling wines, and beers. Nonalcoholic sparkling beverages such as soft drinks, which can be viewed (regarding their chemical complexity) as intermediate between sparkling alcoholic beverages and sparkling waters, could also benefit from further development regarding bubble dynamics and gas-solution thermodynamics.

Acknowledgments Ge´rard Liger-Belair is indebted to the CNRS, and to the Association Recherche Oenologie Champagne Universite´ (AROCU) for supporting his team and research.

References Barker, G.S., Jefferson, B., Judd, S.J., 2002. The control of bubbles in carbonated beverages. Chem. Eng. Sci. 57, 565
573. Bruce, B., 2013. Growth Potential for Global Bottled Water Industry. Available from: ,http://www.foodbev. com/news/growth-potential-for-global-bottled-wate#.VCq-d74WmJY.. Cain, W.S., Murphy, C.L., 1980. Interaction between chemoreceptive modalities of odour and irritation. Nature 284, 255
257. Calderone, G., Guillou, C., Reniero, F., Naulet, N., 2007. Helping to authenticate sparkling drinks with 13C/12C of CO2 by gas chromatography-isotope ratio mass spectrometry. Food Res. Int. 40, 324
331. Caputi, A., Ueda, M., Walter, P., Brown, T., 1970. Titrimetric determination of carbon dioxide in wine. Am. J. Enol. Vitic. 21, 140
144. Carroll, J.J., Mather, A.E., 1992. The system carbon dioxide/water and the Krichevsky
Kasarnovsky equation. J. Solut. Chem. 21, 607
621. Chandrashekar, J., Yarmolinsky, D., von Buchholtz, L., Oka, Y., Sly, W., Ryba, N.J., et al., 2009. The taste of carbonation. Science 326, 443
445. Cometto-Muniz, J.E., Garcia-Medina, M.R., Calvino, A.M., Noriega, G., 1987. Interactions between CO2 oral pungency and taste. Perception 16, 629
640.

CO2 and Bubbles in Sparkling Waters 61 Dessirier, J.M., Simons, C., Carstens, M., O’Mahony, M., Carstens, E., 2000. Psychophysical and neurobiological evidence that the oral sensation elicited by carbonated water is of chemogenic origin. Chem. Senses 25, 277
284. Diamond, L.W., Akinfief, N.N., 2003. Solubility of CO2 in water from 1.5 to 100 C and from 0.1 to 100 MPa: evaluation of literature data and thermodynamic modelling. Fluid Phase Equilib. 208, 265
290. Directive 2009/54/EC of the European Parliament and of the Council of 18 June 2009on the exploitation and marketing of natural mineral waters. Dunkel, A., Hofmann, T., 2010. Carbonic anhydrase IV mediates the fizz of carbonated beverages. Angew. Chem. Int. Ed. 49, 2975
2977. Euzen, A., 2006. Bottled water, globalization and behaviour of consumers. Eur. J. Water Qual. 37, 143
155. Forbes, 2014. Available from: ,http://www.forbes.com/sites/greatspeculations/2014/01/14/coca-cola-eyesgrowth-in-the-sparkling-bottled-water-market/.. Gleick, P.H., 2010. Bottled and Sold: The Story Behind Our Obsession with Bottled Water. Island Press, Washington. Incropera, F., Dewitt, D., Bergman, T., Lavine, A., 2007. Fundamentals of Heat and Mass Transfers. Wiley, New York. Jones, S.F., Evans, G.M., Galvin, K.P., 1999. Bubble nucleation from gas cavities: a review. Adv. Colloid Interface Sci. 80, 27
50. Kleeman, A., Albrecht, J., Scho¨pf, V., Haegler, K., Kopietz, R., Hempel, J.M., et al., 2009. Trigeminal perception is necessary to localize odors. Physiol. Behav. 97, 401
405. Lawless, H.T., Heymann, H., 2010. Sensory Evaluation of Food: Principles and Practices. Springer, New York. Lide, D.R., Frederikse, H.P., 1995. CRC Handbook of Chemistry and Physics, 76th ed CRC Press, Boston. Liger-Belair, G., 2014. How many bubbles in your glass of bubbly? J. Phys. Chem. B 118, 3156
3163. Liger-Belair, G., 2016. Modeling the losses of dissolved carbon dioxide from laser-etched champagne glasses. J. Phys. Chem. B 120, 3724
3734. Liger-Belair, G., 2017. Effervescence in Champagne and sparkling wines: from grape harvest to bubble rise. Eur. Phys. J.
Spec. Top. 226, 3
116. Liger-Belair, G., 2019. Carbon dioxide in bottled carbonated waters and subsequent bubble nucleation under standard tasting condition. J. Agric. Food Chem. 67, in press. Liger-Belair, G., Prost, E., Parmentier, M., Jeandet, P., Nuzillard, J.-M., 2003. Diffusion coefficient of CO2 molecules as determined by 13C NMR in various carbonated beverages. J. Agric. Food Chem. 51, 7560
7563. Liger-Belair, G., Parmentier, M., Jeandet, P., 2006. Modeling the kinetics of bubble nucleation in champagne and carbonated beverages. J. Phys. Chem. B 110, 21145
21151. Liger-Belair, G., Villaume, S., Cilindre, C., Jeandet, P., 2009. Kinetics of CO2 fluxes outgassing from champagne glasses in tasting conditions: the role of temperature. J. Agric. Food Chem. 57, 1997
2003. Liger-Belair, G., Conreux, A., Villaume, S., Cilindre, C., 2013. Monitoring the losses of dissolved carbon dioxide from laser-etched champagne glasses. Food Res. Int. 54, 516
522. Liger-Belair, G., Sternenberg, F., Brunner, S., Robillard, B., Cilindre, C., 2015. Bubble dynamics in various commercial sparkling bottled waters. J. Food Eng. 163, 60
70. Liger-Belair, G., Cordier, D., Honvault, J., Cilindre, C., 2017. Unveiling CO2 heterogeneous freezing plumes during champagne cork popping. Sci. Rep. 7, 10938. Lubetkin, S.D., 2003. Why is it much easier to nucleate gas bubbles than theory predicts? Langmuir 19, 2575
2587. Lugli, F., Zerbetto, F., 2007. An introduction to bubble dynamics. Phys. Chem. Chem. Phys. 9, 2447
2456. Meusel, T., Negoias, S., Scheibe, M., Hummel, T., 2010. Topographical differences in distribution and responsiveness of trigeminal sensitivity within the human nasal mucosa. Pain 151, 516
521. Moreno Soto, A., Maddalena, T., Fratters, A., van der Meer, D., Lohse, D., 2018. Coalescence of diffusively growing gas bubbles. J. Fluid Mech. 846, 143
165.

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Moriaux, A.-L., Vallon, R., Parvitte, B., Ze´ninari, V., Liger-Belair, G., Cilindre, C., 2018. Monitoring gas-phase CO2 in the headspace of champagne glasses, through combined diode laser spectrometry and micro gas chromatography. Food Chem. 264, 255
262. Mulier, M., Zeninari, V., Joly, L., Decarpenterie, T., Parvitte, B., Jeandet, P., et al., 2009. Development of a compact CO2 sensor based on near-infrared laser technology for enological applications. Appl. Phys. B Lasers Opt. 94, 725
733. Perret, A., 2014. Etude des proprie´te´s de transport du CO2 et de l’e´thanol en solution hydroalcoolique par dynamique mole´culaire classique: application aux vins de Champagne (Ph.D. Thesis), Reims, France. Rani, B., Maheshwari, R., Garg, A., Prasad, M., 2012. Bottled water—a global market overview. Bull. Environ. Pharmacol. Life Sci. 1 (6), 1
4. Scriven, L.E., 1959. On the dynamics of phase growth. Chem. Eng. Sci. 10, 1
13. Storey, M., 2010. The shifting beverage landscape. Physiol. Behav. 100, 10
14. Wilt, P.M., 1986. Nucleation rates and bubble stability in water-carbon dioxide solutions. J. Colloid Interface Sci. 112, 530
538. Wise, P.M., Wolf, M., Thom, S.R., Bryant, B., 2013. The influence of bubbles on the perception carbonation bite. PLoS One 8, e71488. Zion Research Analysis, 2015. Available from: ,https://www.marketresearchstore.com/report/bottled-watermarket-z39681..

Further Reading Rodwan, J.G., 2012. Bottled water 2011: the recovery continues. Bottled Water Recov. (BWR) April/May 12
21.

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Cereal-Based Nonalcoholic Beverages Loreta Basinskiene and Dalia Cizeikiene Department of Food Science and Technology, Kaunas University of Technology, Kaunas, Lithuania

Chapter Outline 3.1 Introduction 63 3.2 Nonfermented Cereal-Based Beverages

66

3.2.1 Cereal-Based Milk Substitutes 66 3.2.2 Roasted Grain Beverages 71

3.3 Fermented Nonalcoholic Beverages

73

3.3.1 Traditional Cereal-Based Fermented Beverages 73 3.3.2 Nutritional Properties 76 3.3.3 Nontraditional Cereal-Based Probiotic Beverages 81

3.4 Future Trends 3.4.1 3.4.2 3.4.3 3.4.4

86

New Probiotic Cultures Selection and Application for Beverages Production 86 Micro- and Nanoencapsulation Techniques for Improved Probiotics Surveillance 88 Nanotechnology Application for Functional Cereal-Based Beverages 90 Colloidal Delivery Systems for Food-Grade Nanoparticles 90

References 91 Further Reading

99

3.1 Introduction Cereals are plants that belong to the monocot Gramineae family, including maize (Zea mays L.), wheat [mostly common wheat (Triticum aestivum L.) and durum wheat (Triticum durum Desf.)], rice (Oryza sativa L.), barley (Hordeum vulgare L.), sorghum (Sorghum bicolor L. Moench), millet [mostly pearl millet (Pennisetum glaucum L.) and finger millet (Eleusine coracana L.)], teff (Eragrostis tef), oats (Avena sativa L.), rye (Secale cereale L.), and triticale (X Triticosecale Wittmack). In recent years, pseudocereals such as amaranth (Amaranthus sp.), buckwheat (Fagopyrum esculentum Moench), chia (Salvia hispanica L.), and quinoa (Chenopodium quinoa Willd), have attracted much research attention, primarily because of their desirable nutritional properties and application

Trends in Non-alcoholic Beverages. DOI: https://doi.org/10.1016/B978-0-12-816938-4.00003-3 © 2020 Elsevier Inc. All rights reserved.

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as nutrient-rich, gluten-free ingredients (Alvarez-Jubete et al., 2010; Capriles et al., 2016). Although pseudocereals are used in a similar manner to cereal grains, they are not members of the Gramineae family. Cereal grains are an important food source in most cultures and the global food trade offers many types of cereals available for consumption. Generally, in most parts of the world cereal-based diets are adopted as caloric and protein sources. Wheat, maize, rice, barley, sorghum, oats, rye, and millet are highly acceptable cereal grains which provide 56% of the food energy and 50% of the protein to the human population (Cordain, 1999). Inclusion of cereal grains in the diet provides bioactive compounds to the body. Cereal grains can be viewed as packages of major nutrients (carbohydrates, proteins, lipids), micronutrients (vitamins and minerals), and other phytochemicals (carotenoids and phenolic compounds). Carbohydrates such as digestible starch and simple sugars serve as energy sources. Indigestible forms of carbohydrates including high-molecular-weight polysaccharides and low-molecular-weight oligosaccharides can be used to increase the dietary fiber content of foods. Some cereal dietary fibers (oats and barley β-glucans) already attract health claims. The micronutrients in cereals include B vitamins (thiamine, riboflavin, niacin, pyridoxine, pantothenic acid, and folates) and tocopherols. Whole grains also contributed to the overall mineral content of human diets (including K, Mg, P, Ca, Zn, Fe, Cu, Mn, and S), although the location and/or accumulation of minerals within the grain tissue may influence their dietary availability (Arendt and Zannini, 2013; Serna-Saldivar, 2010). Phenolic compounds, the main phytochemicals in grains, include phenolic acids, flavonoids, anthocyanidins, and phytosterols. The phenolic acids are mostly bound to cell-wall polysaccharides as part of dietary fiber. Ferulic acid is a dominant phenolic antioxidant in cereals. The slow and continuous release of antioxidants bound to dietary fiber in the gut determines their nutritional benefits (Vitaglione et al., 2008). Carotenoids (lutein, zeaxanthin, β- and α-carotene) display provitamin A activity and antioxidant properties. Cereal grains are rich sources of bioactive, health-promoting compounds. Studies have shown that increased consumption of whole grains and their products is associated with reduced risk of developing chronic diseases such as cardiovascular disease, type 2 diabetes, obesity, and cancer which are major causes of death and morbidity (Adil et al., 2012; Middleton et al., 2000; Okarter and Liu, 2010). It has been suggested that the combined effects of bioactive compounds in whole grains may be more healthful than individual isolated components. The health benefits have been attributed to the dietary fiber, phenolic compounds, and carotenoids due to their antioxidant and antiinflammatory actions (Brennan, 2009; Fardet, 2010; Guo and Beta, 2013; Harris and Kris-Etherton, 2010; Liu, 2004; Ndolo and Beta, 2013).

Cereal-Based Nonalcoholic Beverages 65 Although many plant foods may be consumed raw, cereals require transformation to become edible. Several traditional and nontraditional methods (steeping, malting, roasting, fermentation, boiling, baking, frying, nixtamalization, micronization, extrusion, etc.) are used to process whole grains into food. The preparation of grains into finished food products usually requires a combination of several methods. Over the centuries diverse cultures have created various cereal-based foods and beverages, but most processes involve some baking of the exterior bran and gelatinization of the starchy endosperm. Different processing methods affect the content and composition of bioactive compounds and antioxidant activity in cereals (Beta et al., 2005; Giordano et al., 2016; Liyana-Pathirana and Shahidi, 2006). Cereals have recently gained a lot of attention as raw material for nonalcoholic and functional beverage production. They may be in the form of stimulants such as tea and coffee, as refreshers like soft drinks and water, or as nutritional drinks such as milk. Beverage processing could be by simple nonmicrobial processes (such as application of physical techniques) or may involve microbial fermentation and/or enzyme clarification (Blandino et al., 2003; Tafere 2015; Tamang and Kailasapathy, 2010). Depending on the processing steps involved, beverages are classified as nonfermented or fermented (alcoholic or nonalcoholic). Furthermore, based on whether the processes are technologically scaled-up or not, to meet wider consumer demands, they could be regarded as either industrially or traditionally processed. Traditional processing methods as well as constituents and consumption patterns differ across ethnicities in countries and regions (Aka et al., 2014; Amadou et al., 2011; Nzigamasabo and Nimpagaritse, 2009; Tafere, 2015). Cereal-based beverages mostly contain only natural sugar and are excellent sources of antioxidants, vitamins, and other health-promoting substances. The characteristics of these cereal-based products can be varied widely by using different functional constituents. Cereal beverages are based on a grain suspension. An extract of grain suspension can already be drunk as a food supplement rich in dietary fibers, but sifting and filtering of the extract open up further possibilities of creating interesting beverages. The addition of oil emulsions to the filtrate produces beverages similar to milk or cream, but without animal protein and lactose. Because of these properties, “cereal milk” is very well tolerated by lactose intolerance (LI) and cow’s milk allergy (CMA) sufferers. Moreover, innovative flavors can be created by fermenting the extract with microorganisms. Fermentation of cereals with lactic acid bacteria (LAB) improves sensory and nutritional properties, and the microbial shelf life of foods (Leroy and De Vuyst, 2004; Ma˚rtensson et al., 2000; Zannini et al., 2012). Fermentation leads to a decrease in the level of carbohydrates as well as some nondigestible poly- and oligosaccharides. Certain amino acids may be synthesized and the

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availability of B group vitamins may be improved. Fermentation also provides optimum pH conditions for enzymatic degradation of phytates that may increase the amount of soluble Fe, Zn, and Ca. Also, organic acids resulting from fermentation give the drink a fresh, fruity note. The fermentation products also create a feeling of wellbeing and stimulate the metabolic system. This chapter reviews the production technologies and nutrition properties of cereal-based, nonalcoholic beverages, fermented and nonfermented, used as dairy milk substitutes, or tea/coffee substitutes. Innovative cereal-based beverages with enhanced health properties are also discussed.

3.2 Nonfermented Cereal-Based Beverages 3.2.1 Cereal-Based Milk Substitutes Cereal-based milk substitutes are water extracts of cereals or pseudocereals that resemble cow’s milk in appearance. There is several such traditional cereal-based beverages around the world, for example, Sikhye—a beverage made of cooked rice, malt extract, and sugar in South Korea; Kunu (Kunun zaki)—a Nigerian beverage made from sprouted millet, sorghum, or maize (Gaffa et al., 2002; Kim et al., 2012). Rice milk and oat milk are popular examples of dairy substitutes. Rice milk is mostly made from brown rice and is usually unsweetened. The sweetness in most rice milk varieties is generated by a natural enzymatic process that cleaves the carbohydrates into sugars, especially glucose. There are some rice milk varieties that are sweetened with sugarcane syrup or other sugars. Commercial brands of rice milk are available in vanilla, chocolate, and almond flavors, as well as the original unflavored form, and can be used in many recipes as an alternative to cow’s milk. Oat milk is made from whole oat grains by soaking the plant material to extract its nutrients (Deswal et al., 2014; Ma¨kinen et al., 2016). Oat milk naturally has a creamy texture and a characteristically oatmeal-like flavor, although it is sold commercially in various flavor-varieties such as sweetened, unsweetened, vanilla, or chocolate. Unlike other plant milks, whose origins date as early as the 13th century, oat milk was first developed by the Swedish scientist Rickard Oste in the early 1990s (Shurtleff and Aoyagi, 2013). Oats contain high amounts of functional protein, dietary fiber (β-glucan), and unsaturated fatty acids which make it a significant source of nutrients, although uncertainty surrounds its practical use as a dairy substitute (Deswal et al., 2014). Oat milk is also a viable substitute for cow’s milk for producing fermented milk products such as yogurts, kefir, prebiotics, and probiotics while retaining its characteristic nutrient content (Ma˚rtensson et al., 2000, 2001).

Cereal-Based Nonalcoholic Beverages 67 3.2.1.1 Nutritional Properties Rice milk and oat milk are often consumed by people who suffer from LI, CMA, radioiodine cancer treatment, eczema, and possibly other conditions which react poorly to dairy (Ma¨kinen et al., 2016). Oat milk is a recommended dairy milk substitute for individuals who suffer from irritable bowel syndrome (IBS), and inflammatory bowel disease (IBD), as part of the antiinflammatory diet, thus IBS and IBD patients report a much higher intake of oat milk than other consumers (Olendzki et al., 2014). Cereal-based beverages are also used as a dairy substitute by vegans. It is estimated that 15% of European consumers avoid dairy products for a variety of reasons, including medical reasons such LI, CMA, cholesterol issues, and phenylketonuria, as well as lifestyle choices such as a vegetarian/vegan diet or concerns about growth hormone or antibiotic residues in cow’s milk (Jago, 2011; Leatherhead Food Research, 2011). The nutritional properties of cereal-based milk substitutes vary greatly as they depend strongly on the raw material, processing, fortification, and the presence of other ingredients such as sweeteners and oils (Bus and Worsley, 2003). However, the nutritional quality of these types of beverages is sometimes inferior or poor in comparison with milk and milk products. Cereal-based milk substitutes are low in protein, which may pose a risk if they are used to replace dairy milk without knowledge about the differences. Several cases of kwashiorkor, a protein-energy malnutrition typical in areas of famine, have been reported in Western countries as a result of using rice milk (0.1%
0.2% protein) as a weaning food (Carvalho et al., 2001; Katz et al., 2005). Although cereal-based milk substitutes are low in saturated fats and most products have caloric counts comparable to skim milk, some products contain as much energy as full milk, originating mostly from sugars and other carbohydrates. Cereal proteins are generally of a lower nutritional quality compared with animal-derived proteins due to limiting amino acid lysine and poor digestibility (Friedman, 1996). In addition to containing high-value protein, milk and other dairy products provide 30%
40% of dietary calcium, iodine, vitamin B12, and riboflavin, and population groups with low milk intakes often have a poor status for these nutrients (Black et al., 2002). Therefore cereal-based milk substitutes are fortified with calcium and vitamins, mainly vitamins B12, B2, D, and E. Calcium absorption depends on the salt used for fortification as well as the food matrix (Rafferty et al., 2007). Cereals also contain antinutritive compounds, such as phytates and trypsin inhibitors. Trypsin inhibitors decrease the digestibility of protein, but are inactivated by heat

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treatments (Friedman, 1996). Phytates bind divalent cations such as Ca, Zn, Fe, and Mg, and reduce their physiological availability (Sandberg et al., 2006). Mineral bioavailability can be improved by germination, fermentation, or by using chelating agents or exogenous phytase. Zhang et al. (2007a) obtained the highest increase in iron bioavailability. Processing also influences the nutritional properties of cereal-based milk substitutes. Water-soluble vitamins are lost when the raw material is soaked and high amounts of minerals (Ca, Fe, P, and Zn; 45%
74%) are lost during the decanting step (Zhang et al., 2007b). The destruction of heat-sensitive vitamins also depends on the time
temperature exposure. Significant loss of vitamins A, D3, and B12 occurred during the storage of oat milk (Zhang et al., 2007b). The beneficial effects of oat β-glucan on serum low-density lipoprotein (LDL) cholesterol and postprandial glucose levels are mainly attributed to its viscosity in aqueous solutions, which is sensitive to homogenization and thermal treatments (Kivela¨ et al., 2010, 2011; Wood, 2010). Several methods have been employed with the aim to improve the nutritional quality of cereal-based beverages. These include supplementation with nutrients such as protein concentrates or other protein-rich sources, vitamins, and minerals. Also, additional processing technologies, which include sprouting and fermentation, could be used to improve the nutritional properties of cereal-based beverages, although probably the best one is fermentation. 3.2.1.2 Production Technology The production process of cereal-based milk substitutes is similar to the production process of other plants milk substitutes. These are prepared traditionally by grinding the raw material into slurry and straining it to remove coarse particles. Although different variations of the process exist, the general steps of a modern industrial-scale process are the same (Fig. 3.1), that is, the plant material is soaked and wet-milled to extract the nutrients, or alternatively the raw material is dry-milled and the flour is extracted in water, and the grinding waste is separated by filtering or decanting. Depending on the product, standardization and/or addition of other ingredients such as sugar, oil, flavoring, and stabilizers may take place, followed by homogenization and pasteurization/ultrahightemperature (UHT) treatment to improve suspension and microbial stabilities. Extraction. Most of cereal grains are indigestible when unprocessed due to their hard, outer hull, so processing is necessary to create a product with nutrients which are bioavailable (Decker et al., 2014). The procedure starts by grinding or milling to break apart the outer hull. Soluble grain material can be extracted either by grinding of plant material with water or by wet-grinding soaked grains into a slurry.

Cereal-Based Nonalcoholic Beverages 69

Figure 3.1 The general manufacturing process of cereal-based milk substitutes. Adapted from Ma¨kinen, O.E., Wanhalinna, V., Zannini, E., Arendt, E.K., 2016. Foods for special dietary needs: non-dairy plant-based milk substitutes and fermented dairy-type products. Crit. Rev. Food Sci. Nutr. 56 (3), 339
349.

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The extraction step has the most direct implications on the composition of the resulting product. To increase the yield of the process, the efficiency of this step may be improved by increasing the pH (with bicarbonate or NaOH) or temperature, or the use of enzymes. Alkaline pH during extraction increases protein extractability, but a neutralization step may be required in the process. A higher extraction temperature increases the reaction rate and extractability of fat, but the denaturation of proteins decreases their solubility and yield. Partial hydrolysis of proteins using proteolytic enzymes increases the extraction yields and improves the suspension stability. In addition to proteolytic enzymes, a mixture of an amyloglucosidase and cellulase cocktail increases the carbohydrate recovery (Deswal et al., 2014). Also, cellulase treatment has been reported to decrease the particle size and yield a more stable suspension (Rosenthal et al., 2003). When using cereals or pseudocereals, the starch forms a thick slurry when heated above the gelatinization temperature (55 C
65 C). To prevent this in the further processing steps, starch has to be gelatinized, liquefied and saccharified with amylases or a malt enzyme extract (Mitchell and Mitchell, 1990). The patented process by Lindahl et al. (2001) employs α- and β-amylases to hydrolyze the starch until a desired level of sweetness and viscosity is reached. The saccharification step may take place before or after the removal of coarse particles. However, according to Mitchell and Mitchell (1990), heating the slurry above 50 C before filtration compromises the mouthfeel of rice milk. α-Amylase is used to liquefy the starch. The α-amylase attacks the amorphous structure of the starch, hydrolyzes the α-1,4-glycosidic bonds of amylose and amylopectin at arbitrary distances and releases water-soluble dextrins, which gelatinize at higher, more suitable temperatures. By adding the hemicellulase and the protease it is possible to adjust the mouthfeel and digestibility of the cereal beverage. The choice of the enzymes used for saccharification determines the percentages of the different sugars in the end product. β-Amylase releases chiefly maltose and maltotriose from dextrins. Glucoamylase, on the other hand, hydrolyzes dextrins into glucose. Through the combination of these enzymes the cereal beverage acquires a sweetness which can be adjusted optimally in respect of its perception and intensity. After the extraction step, coarse particles are removed from the slurry by filtration, decanting, or centrifugation (Lindahl et al., 2001). Product formulation. Other ingredients can be added to the product base after the removal of the coarse plant material. These include vitamins and minerals used for fortification as well as sweeteners, flavorings, salt, oils, and stabilizers. The addition of nutrients may be necessary to ensure the nutritional quality of the product. Cereal-based milk substitutes are naturally lower in calcium, iron, and vitamin A than dairy milk, so the addition of these nutrients is necessary in order to be a viable dairy substitute.

Cereal-Based Nonalcoholic Beverages 71 The nutrients used must be bioavailable and sufficiently stable, and not cause excessive changes in product quality. The stability of vitamins is influenced by several factors during processing and may be reduced as a result of, for example, heating oxygen exposure (Richardson, 1990). The mineral sources used in cereal-based milk substitutes include ferric ammonium citrate and ferric pyrophosphate as iron sources and tricalcium phosphate and calcium carbonate as calcium sources (Zhang et al., 2007a). The metal ions can react with other food components, therefore the use of sequestrants such as citric acid may be necessary (Richardson, 1990; Zhang et al., 2007a). Cereal-based milk substitutes contain insoluble particles, such as protein, starch, fiber, and other cellular material. These particles, being denser than water, can sediment, making the product unstable, or can coagulate when heated. The suspension stability can be increased by decreasing the particle size (homogenization), or by using hydrocolloids and emulsifiers (Durand et al., 2003; Ma¨kinen et al., 2015). Lee and Rhee (2003) used pine nuts to improve the stability of a rice-based beverage as these contain proteins with good emulsifying properties. Sodium stearoyl-2 lactylate, a lipid surfactant, has been found to bind specifically to partially hydrolyzed oat proteins and, thus, enhance the stability of oat protein suspensions (Chronakis et al., 2004). Homogenization improves the stability by disrupting aggregates and lipid droplets and, thus, decreasing the particle size distribution. Homogenization in the conventional dairy-processing pressure range (c.20 MPa) increases the suspension stability sufficiently of rice milk substitutes (Lee and Rhee, 2003). Shelf life extension. Commercial plant milk substitutes are pasteurized or UHT-treated to extend their shelf life. However, heat may cause changes in protein properties that can influence the stability, as well as changes in flavor, aroma, and color (Kwok and Niranjan, 1995; Ma¨kinen et al., 2015). Pasteurization is carried out at temperatures below 100 C, which destroys enough microorganisms to enable a shelf life of about one week at refrigerated temperatures. In the UHT treatment the product is heated to 135 C
150 C for a few seconds, yielding a sterile product. The manufacturing process of sikhye takes another approach. The product is commonly sold frozen to avoid UHT-related changes in flavor. However, Bacillus cereus spores are a risk and their number can been reduced by tyndallization with CO2 injection, a procedure consisting of heating to 80 C to activate spore germination, followed by heating to 95 C (Kim et al., 2012).

3.2.2 Roasted Grain Beverages A roasted grain beverage is a hot drink made from one or more cereal grains roasted and boiled in water or steeped in hot water. They are commercially available in crystal or powder form to be reconstituted later in hot water. The product is often marketed as a

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caffeine-free alternative to coffee and tea, or in other cases where those drinks are scarce or expensive. Roasted grain beverages are popular in East Asian countries like Korea, Japan, and China. They are consumed either hot or cold, often taking the place of drinking water in many homes and restaurants. The most popular are barley tea, rice tea, corn tea, and buckwheat tea. In China, barley tea is called da`ma`i-cha´ or ma`i-cha´, in Japan it is mugi-cha or mugi-yu, and in Korea bori-cha and Sino-Korean cha. In Korea, roasted barley is also often combined with roasted corn, as the corn sweetens the slightly bitter flavor of the barley. The tea made from roasted corn is called oksusu-cha and the tea made from roasted corn and roasted barley is called oksusu-bori-cha. Other similar drinks made from roasted grains typically used in Korea are hyeonmi-cha (brown rice tea) and memil-cha (buckwheat tea). Sungnyung is a drink made from scorched rice. Water is directly added to a pot where the scorched crust of rice (most commonly white rice) is left in the bottom when it is still hot. Unlike hyeonmi-cha, the rice grains are simmered for a relatively long time until soft, and may be consumed together with the liquid. Roasted barley tea manufactured in ground form and sometimes combined with chicory or other ingredients, is also sold as a coffee substitute (barley coffee). Barley coffee is popular in Europe. In Italy it is known as coffe d’orzo and is commonly used as a breakfast drink for children when mixed with milk. Another popular roasted grain drink is inka developed in Poland in the late 1960s. Inka is a roasted mixture of rye, barley, chicory, and sugar beet (cereals make up 72% of the mixture content) and is used as a caffeine-free coffee substitute. 3.2.2.1 Nutritional Properties Roasting is a process involving high, dry heat. When grains are roasted to darker colors at about 150 C, they can lose significant amounts of thiamine and riboflavin (Hucker et al., 2012). The dark-roasted grains can also have high levels of acrylamide. Acrylamide is a low-molecular-weight, highly water-soluble, organic compound which forms from the naturally occurring constituents of asparagine and sugars in certain foods when prepared at temperatures typically higher than 120 C and low moisture. It forms mainly in baked, roasted, or fried carbohydrate-rich foods where raw materials contain its precursors, such as cereals, potatoes, and coffee beans. The substance has raised health concerns as, based on animal studies, it was concluded that acrylamide in food potentially increases the risk of developing cancer for consumers in all age groups (EFSA, 2015). Mizukami et al. (2016) investigated acrylamide elution from roasted barley grain into mugi-cha and its formation during roasting of the grain. Highly water-soluble acrylamide was easily extracted to

Cereal-Based Nonalcoholic Beverages 73 mugi-cha from milled roasted barley grains. During roasting in a drum roaster, the acrylamide concentration of the grain increased as the surface temperature rose, reaching a maximum at 180 C
240 C. Above this temperature, the acrylamide concentration decreased with continued roasting. The level of asparagine in barley grains was found to be a significant factor related to acrylamide formation in roasted barley products. On the other hand, it has been reported that roasting increases the total phenolic compounds and antioxidant activity (Ragaee et al., 2014). Papetti et al. (2007) found that barley coffee possesses antimicrobial and bactericidal activity against oral pathogens such as Streptococcus mutans and Streptococcus sobrinus as well as high antiadhesive properties, therefore its consumption may decrease the buildup of cariogenic bacteria on teeth. The α-dicarbonyl compounds formed during the barley roasting process were responsible for the antibacterial and antiadhesive properties (Daglia et al., 2007). Wu et al. (2013) investigated the effect of traditional processing techniques (soaking, steaming, roasting) on phytochemical levels, antioxidant activity, and type 2 diabetes related to α-glucosidase and α-amylase inhibitory activities of sorghum tea. Soaking and steaming promoted the loss of phytochemicals levels; however, roasting caused significant increases of phenolic compound levels, antioxidant, α-glucosidase, and α-amylase inhibitory activities compared to the other two processes.

3.3 Fermented Nonalcoholic Beverages 3.3.1 Traditional Cereal-Based Fermented Beverages Fermented beverages are produced worldwide and can be alcoholic or nonalcoholic using numerous manufacturing techniques, various raw materials, and microorganisms (Baschali et al., 2017; Blandino et al., 2003). In most European countries, “nonalcoholic” beverages contain a maximum of 0.5% by the volume of ethyl alcohol (Baschali et al., 2017). A few of the cereal-based fermented drinks consumed worldwide are presented in Table 3.1. Each product provides its unique and specific health benefits depending on the fermentation medium and probiotic cultures applied for fermentation. Moreover, cerealbased products fermented with LAB could be a perfect alternative for people who are allergic to milk proteins (Gambu´s et al., 2015). Such products are kvass, boza, bushera, pozol, Tanzanian togwa, mahewu, and others. 3.3.1.1 Kvass Kvass is a cereal-based beverage traditionally made from fermented barley and rye malt, rye flour, and stale rye bread (Basinskiene et al., 2016). This cereal-based fermented beverage has achieved much commercial success and is widely producible in eastern European countries such as Russia, Poland, and Baltic countries, especially Latvia and

Table 3.1: A few traditional cereal-based fermented drinks. Beverage

Substrate

Microorganisms of Fermentation

References

Amahewu Boza

Maize Wheat, millet, rye, maize, barley, semolina

Spontaneous fermentation Lactobacillus acidophilus, Lactobacillus fermentum, Lactobacillus plantarum, Lactobacillus rhamnosus, Lactobacillus casei, Leuconostoc raffinolactis, Leuconostoc mesenteroides, Bifidobacterium longum, Bifidobacterium bifidum, Bifidobacterium breve, Saccharomyces cerevisiae, Saccharomyces boulardii, Candida tropicalis, Candida glabrata, Geotrichum penicillatum, Geotrichum candidum Lactobacillus plantarum, Lactobacillus paracasei subsp. paracasei, Lactobacillus brevis, Lactobacillus fermentum, Lactobacillus delbrueckii subsp. delbrueckii, Streptococcus thermophiles, Enterococcus genera Pediococcus pentosaceus Spontaneous fermentation Lactobacillus casei, Leuconostoc mesenteroides, Saccharomyces cerevisiae, Lactococcus lactis var. diacetylactis, Lactobacillus sakei, Pediococcus pentosaceus, Candida milleri, Torulaspora delbrueckii

Franz et al. (2014) Petrova and Petrov (2017), Tangu ¨ler (2014)

Bushera

Millet, sorghum

Fufu Hulumur Kvass

Maize Sorghum, rice, millet Rye bread, rye, barley malt/flour, stale rye bread, extruded wholemeal rye flour Maize

Pozol Mahewu

Maize

Mawe

Maize

Ogi

Maize

Taar Tanzanian togwa Uji

Rye, barley, oats Sorghum, maize, millet

Maize

Lactobacillus plantarum, lactic acid bacteria included amylolytic strains Lactobacillus fermentum, Pediococcus pentosaceus, Lactococcus lactis Lactococcus lactis subsp. lactisLactobacillus bulgaricus var. delbrueckii, Lactobacillus brevis Spontaneous fermentation, Lactobacillus fermentum, Lactobacillus brevis, Lactobacillus curvatus, Lactobacillus buchneri, Weissella confusa, Candida krusei, Candida kefyr, Candida glabrata, Saccharomyces cerevisiae, pediococci Lactobacillus plantarum Spontaneous fermentation Lactobacillus plantarum, Weissella confuse, Pediococcus pentosaceus, Issatchenkia orientalis, Saccharomyces cerevisiae, Candida tropicalis, Candida pelliculosa Lactobacillus plantarum, Lactobacillus fermentum, Lactobacillus cellobiosus, Lactobacillus buchneri, Pediococcus acidilactici, Pediococcus pentosaceus

Muyanja et al. (2003)

Franz et al. (2014), Sanni et al. (2013) Battock and Azam-Ali (1998) Basinskiene et al. (2016), Czerwi´ nska (2008), Dlusskaya et al. (2008), Gotcheva et al. (2002), Marsh et al. (2014)

Bansal et al. (2016), Franz et al. (2014), Oyewole (1997), Steinkraus (1996) Hounhouigan et al. (1993, 1994)

Franz et al. (2014), Odunfa and Adeyele (1985) ˜ukand et al. (2015) So Mugula et al. (2001)

Franz et al. (2014), Mbugua (1985)

Cereal-Based Nonalcoholic Beverages 75 Lithuania. Kvass is a “nonalcoholic” beverage, therefore the ethanol content should be minor and, consequently, it is considered to be spoiled if the content of alcohol accumulates to higher levels (Basinskiene et al., 2016). Generally, kvass could contain 1% or less amount of alcohol (Baschali et al., 2017). Kvass undergoes no heat processing after fermentation and, thus, contains high amount of viable yeast and LAB cells over 107 cfu/mL (Basinskiene et al., 2016). The microflora of kvass fermentation is normally composed of Saccharomyces cerevisiae and LAB, for example Lactobacillus casei, Leuconostoc mesenteroides (Marsh et al., 2014). The composition of LAB species is expected to be quite variable due to differences in fermentation techniques and fermentation media. Kvass southern is made from rye bread, sugar, yeast, raisins, juniper berries, and water (Albuquerque et al., 2013), whereas mint kvass is another version to which mint leaves are added. Kvass is naturally carbonated with a rye bread flavor and has a golden-brown color and sweet
bitter taste (Baschali et al., 2017). The taste is more or less seasoned and is strongly dependent on the time and temperature of fermentation (Gambu´s et al., 2015). Nutritional properties

Kvass mainly contains arabinose, maltose, glucose, maltotriose, fructose and xylose, arabinoxylooligosaccharides, maltooligosaccharides, proteins and amino acids, lactic acid and acetic acid, ethanol, minerals, and vitamins originating from the raw materials or from the microbial metabolic activity (Basinskiene et al., 2016; Dlusskaya et al., 2008). Especially it is rich with B vitamins such as thiamine, niacin, riboflavin, and pyridoxine (Gambu´s et al., 2015). During production of kvass, bacteria and yeast, remaining in a symbiotic coexistence, favors not only the development of distinctive aroma and flavor compounds of the beverage, whereas microorganisms produce metabolites beneficial for health (Dziugan, 2006). Kvass eliminates flatulence, hyperacidity, and other digestive disorders and, at the same time, has a positive effect on metabolism, increases the bioavailability of calcium and other minerals, and possesses antioxidant properties (Czerwi´nska, 2008; Gambu´s et al., 2015). Moreover products of yeast autolysis, such as superoxide dismutase, are able to “scavenge” excess of superoxide radicals (Dziugan, 2008). As it is a product of lactic and alcohol fermentation it does not require pasteurization and, therefore, contains LAB, which are useful microflora for human health. Therefore kvass can be considered as a probiotic beverage. Production technology

Two main traditional kvass-making techniques that are well-liked use, as a raw material, either stale sourdough rye bread or rye malt/flour (Dlusskaya et al., 2008). Moreover, Basinskiene et al. (2016) described a new modified technology of kvass production using wholemeal rye flour previously extruded by a single-screw extruder and treated by enzymatic hydrolysis (applying α-amylase, amyloglucosidase, and β-xylanolytic enzymes)

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and LAB fermentation. LAB play a key role in food fermentations where they contribute to the development of the desired sensory properties and microbiological safety. The antimicrobial effect of LAB is mainly related to the production of lactic and acetic acids, as well as phenolic and proteinaceous compounds—bacteriocins or bacteriocin-like inhibitory substances (Cizeikiene et al., 2013). Flowcharts of the traditional kvass-making technique using stale sourdough rye bread and a modified technological scheme for kvass production using extruded wholemeal rye flours are presented in Fig. 3.2. Boza

Boza is cereal-based fermented beverage obtained from the whole grains or flour. Different grains such as wheat, millet, rye, maize, barley, and semolina could be used for boza production (Petrova and Petrov, 2017). Boza is widely consumed in Turkey and in Balkan countries such as Bulgaria, Serbia, Romania, Albania, Macedonia, as well as in South Russia. Due to boza’s pleasant flavor and taste and high nutritional value this beverage has become a very popular drink consumed daily by people of all ages. The content of alcohol in boza varies from 0.02% to 0.79%, although the boza produced in Egypt has a higher alcohol content (up to 7% by volume) and is consumed as a “beer” (LeBlank and Todorov, 2011; Petrova and Petrov, 2017). In general, the pH of the boza varies from 3.4 to 3.9, whereas the content of lactic acid varies from 0.02 to 0.3 mmol/g. The content of lactic acid depends on the content of fermentable carbohydrates present in the substrate. The lowest content of lactic acid was found in millet boza (0.3% w/v), whereas the highest content was found in wheat boza (0.6% w/v) (Akpınar-Bayizit et al., 2010).

3.3.2 Nutritional Properties The beneficial effect of boza on human health displays mainly due to: (1) the valuable cereal components such as dietary fibers, especially β-glucans and resistant starch, and (2) direct consumption of probiotic LAB. The taste and odor of boza, and its positive influence on human health mainly depend on factors such as the source of flours, probiotic microbial starters, and fermentation conditions which affect the quality of the final product (Petrova and Petrov, 2017). Boza contains a number of different probiotic LAB such as Lactobacillus plantarum, Lactobacillus acidophilus, Lactobacillus fermentum, Lactobacillus coprophilus, Leuconostoc raffinolactis, L. mesenteroides, and Lactobacillus brevis and could be labeled as a functional-probiotic food (Todorov et al., 2008). Moreover, LAB strains isolated from boza survived the conditions simulating the gastrointestinal tract and were able to produce bacteriocins active against pathogens (Todorov et al., 2008). Probiotics provide benefits for health as they make digestion easy with their lipolytic, proteolytic, and β-galactosidase activities (Songu¨r et al., 2016). S. cerevisiae and their

Figure 3.2 Flowcharts of two kvass-making techniques using different raw material: (A) stale rye bread and (B) extruded wholemeal rye flour. (A) Adapted from Gambu´s, H., Mickowska, B., Barto´n, H., Augustyn, G., Zie˛´c, G., Litwinek, D., et al., 2015. Health benefits of kvass manufactured from rye wholemeal bread. J. Microbiol. Biotechnol. Food Sci. 4 (3), 34
39. (B) Adapted from Basinskiene, L., Juodeikiene, G., Vidmantiene, D., Tenkanen, M., Makaravicius, T., Bartkiene E., 2016. Non-alcoholic beverages from fermented cereals with increased oligosaccharide content. Food Technol. Biotechnol. 54 (1), 36
44.

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Figure 3.2 (Continued)

Cereal-Based Nonalcoholic Beverages 79 metabolites in the intestine commonly available in boza can stimulate the mucosal immune system (Saegusa, 2004). Millet, the grain for boza production, is a source of both omega-3 and omega-6 fatty acids. These fatty acids are able to decrease the risk of cardiovascular diseases, such as myocardial infarction, coronary heart disease, and sudden cardiac death (Lavie et al., 2009). Moreover, omega-3 can reduce blood pressure, prevent arrhythmias, and decreases the risk of several cancers such as those of the kidney, prostate, breast, and colon (Anand et al., 2008). 3.3.2.1 Production Technology The technological processes of boza production may have some differences whereas the cereal grains are always the major component (Petrova and Petrov, 2017). The main production steps entail the preparation of raw materials including boiling, cooling, sugar addition, and fermentation (Arıcı and Da˘glıo˘glu, 2002). A flowchart of the traditional boza-making technique is presented in Fig. 3.3. Boza can be produced from various cereals or their combination of two or more. The grains are milled to obtain flour or semolina, whereas to remove the remaining hull and bran, the grains are sifted. Prepared cereals and cereal products are mixed with water (ratio 1:4
6) after which they are boiled. The boiling continues until a homogeneous mixture is obtained. The duration of boiling depends on the boiling temperature and the type of raw material used, thus taking 1
2 h (Yegin and Fernandez-Lahore, 2012). The boiled-cereals product is left for refrigeration. The duration of refrigeration is from 12 to 24 h. Following the refrigeration procedure, water is added to the rested and cooled mixture. Continuous stirring should be carried out in order to ensure homogeneity during the addition of water. It is further filtrated to eliminate unwanted particles (Songu¨r et al., 2016). Following the filtration procedure, sugar is added in order to improve LAB fermentation. Fermented boza (2%
3%), sourdough or yoghurt as a starter culture is used for fermentation. Two different kinds of fermentation happen simultaneously, namely alcohol fermentation and lactic acid fermentation (Arıcı and Da˘glıo˘glu, 2002; Cosansu, 2009). Microflora of boza mainly consists of LAB and yeasts, with an average LAB/yeasts ratio equal to 2:4 (Gotcheva et al., 2000). Interactions between LAB and yeasts are uncontrolled during the process, which leads to variability in product quality. After the fermentation, partially fermented boza is cooled and bottled, and should be stored at refrigerator temperatures. It should be consumed within 3
5 days of storage (Arıcı and Da˘glıo˘glu, 2002). Tanzanian togwa

Tanzanian togwa is a beverage prepared from fermented sorghum, maize flour, millet, or a mixture of maize and sorghum. It is widely consumed in Tanzania either in the form of porridge as weaning food or in diluted form as beverage. In some parts, rice and cassava flour can be used. Cereal flour is mixed with water and cooked for approximately 20 min to obtain gruel. To prepare malt flour, cereal grains are soaked in water for approximately

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Figure 3.3 Flowchart of traditional boza-making technique. Adapted from Yegin, S., Fernandez-Lahore, M., 2012. ¨ zgu¨l Evranuz, E. (Eds.), Boza: a traditional cereal based, fermented Turkish beverage. In: Hui, Y.H., O Handbook of Fermented Food and Beverage Technology. CRC Press, Boca Raton, FL, pp. 284
305; Tangu¨ler, H., 2014. Traditional Turkish fermented cereal based products: tarhana, boza and chickpea bread. Turk. J. Agric. Food Sci. Technol. 2 (3), 144
149.

Cereal-Based Nonalcoholic Beverages 81 12 h, draining and germinating for 3
6 h. The germinated grains are sun dried and milled to obtain malt flour. Malt flour is mixed with the gruel at a concentration of 5% (w/v), whereas 10% (v/v) of the older togwa is used as inoculum. In the traditional togwa production the natural microflora dominates; therefore the product characteristics vary (Bansal et al., 2016). Due to uncertain product characteristics and unhygienic preparation practices, togwa is associated with poor people (Mugula et al., 2001). Lactobacillus such as L. plantarum, Weissella confusa, and Pediococcus pentosaceus have been isolated from traditional togwa, whereas yeast species were found to be Issatchenkia orientalis, S. cerevisiae, Candida tropicalis, and Candida pelliculosa (Mugula et al., 2001). These isolates can also be used as starter cultures in order to produce togwa at a commercial scale ensuring quality and hygienic conditions. Mahewu

Mahewu is a fermented beverage usually produced from maize and all age groups in South Africa commonly consume it. For mahewu preparation, the maize porridge is diluted and mixed with malting sorghum/millet flour or wheat flour. The mixture is left for approximately 24 h at an ambient temperature for spontaneous fermentation. In traditional fermentation, Lactococcus lactis ssp. lactis was found to be the major microorganism (Steinkraus, 1996). After the fermentation, various fruit flavorings can be added to enhance the flavor (Edwards, 2003). Traditional mahewu is produced industrially using Lactobacillus bulgaricus var. delbrueckii or L. brevis (Bansal et al., 2016). Mahewu is available at supermarkets in South Africa; however, the quality of commercial mahewu beverages was found to be low compared to traditional brews. Therefore, the development of starter cultures capable to impart the quality attributes to the industrial mahewu beverages should be carried out (Bansal et al., 2016; Gadaga et al., 1999).

3.3.3 Nontraditional Cereal-Based Probiotic Beverages Recently many efforts have been made to develop new cereal-based fermented beverages with functional ingredients to stimulate cardiovascular benefits and improve gastrointestinal health (Vijaya Kumar et al., 2015). For example, milk substitutes obtained from cereals can be fermented using probiotic bacteria to produce a yoghurt-type beverage while transforming the raw material into a more acceptable form. Application of probiotics previously isolated from various spontaneously fermented cereal-based foods, for new beverages production increased during the past decade. There are some newly developed cereal-based fermented beverages and foods that are considered as probiotic products (e.g., yosa; Wood, 1997). Other traditional cereal-based fermented foods and drinks have been modified with the purpose to control some diseases. An improved ogi named dogik has been developed using a lactic acid starter with antimicrobial properties

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against some diarrheagenic bacteria (Okagbue, 1995). A few novel cereal-based beverages fermented with probiotic cultures are listed in Table 3.2. In 1994, the first functional food supplemented with probiotic cultures produced from oatmeal gruel and not containing milk or milk constituents, named ProViva, was manufactured in Skane Dairy, Sweden (Prado et al., 2008). Oatmeal gruel was fermented with LAB L. plantarum 299v, while malted barley was added to increase the liquefaction of the product. The final beverage contains probiotics B1012 cfu/L. Fermented oatmeal gruel Table 3.2: List of some cereal-based probiotic beverages developed recently. Beverages Emmer grains and flourbased drinks

Mahewu-based beverage Malt-based drink Mixed cereal beverage

Oat-based drink Oatmeal beverage named ProViva Oat milk fermented derivatives Oat, barley, and maltbased drink

Rice-based yogurt

Whole-grain liquid probiotic beverage based on malt, oats, maize, rice, alfalfa seed, barley, linseed (flax), mung beans, rye, wheat, millet, and buckwheat Yosa (oat bran pudding/yogurt)

Probiotic Microorganisms

Viable Cell Count

References

Lactobacillus plantarum 6E and 10E, Weissella confuse 12E, Lactobacillus brevis 20S, Weissella cibaria WC4, WC3 and WC9, Lactobacillus plantarum PL9, Pediococcus pentosaceus PP1, Lactobacillus rhamnosus SP1 Bifidobacterium lactis DSM 10140 Lactobacillus reuteri 11951 Lactobacillus plantarum NCIMB 8826, Lactobacillus acidophilus NCIMB 8821 Lactobacillus plantarum B28 Lactobacillus plantarum 299v

5 3 10 cfu/mL

Coda et al. (2011)

Lactobacillus reuteri, Streptococcus thermophiles Lactobacillus acidophilus NCIMB 8821, Lactobacillus plantarum NCIMB 8826, Lactobacillus reuteri NCIMB 11951 Lactobacillus acidophilus, Lactobacillus casei subsp. rhamnosus Lactobacillus bacteria

Lactic acid bacteria and bifidobacteria

8

107 cfu/g

McMaste et al. (2005) 109 cfu/g Kedia et al. (2007) 7 3 108
4 3 108 cfu/mL Rathore et al. (2012) 7.5 3 1010 cfu/g 5 3 1010 cfu/L

Angelov et al. (2006) Prado et al. (2008)

107 cfu/g

Bernat et al. (2014)

106
108 cfu/mL

´n et al. Salmero (2014)

7.6 3 107 cfu/g

Wongkhalaung and Boonyaratanakornkit (2000) Nyanzi and Jooste (2012), Soccol et al. (2012)

Blandino et al. (2003)

Cereal-Based Nonalcoholic Beverages 83 was mixed with various fruit drinks like rose, blackcurrant, hip, strawberry, blueberry, or tropical fruit juices at a concentration of 5%. The product ready for consumption contains B5 3 1010 cfu/L of probiotic bacteria L. plantarum 299v. L. plantarum 299v were found to be resistant to the low pH of the fruit drinks (pH , 2.8
3.4) and remained viable for more than 1 month under refrigerated conditions. GoodBelly, a similar product to ProViva based on oatmeal fermented with L. plantarum 299v, was the first cereal-based (without dairy components) probiotic beverage that spread in the US market in 2006 (Bansal et al., 2016). Another example of a commercial product is Wholegrain Probiotic Liquid (Grainfields, Australia), a refreshing, sparkling liquid containing both yeast (S. cerevisiae var. boulardii) and LAB (L. acidophilus and L. delbrueckii) as well as amino acids, vitamins, and enzymes (Nyanzi and Jooste, 2012; Soccol et al., 2012). Wholegrain liquid probiotic beverage is a blend of non-genetically modified organism, organic predigested, fermented, and cultured malt, oats, maize, rice, alfalfa seed, barley, linseed (flax), mung beans, rye grain, wheat, millet, and buckwheat in a base of filtered water which is fermented, filtered, and bottled. 3.3.3.1 Saccharified Rice Yoghurt Wongkhalaung and Boonyaratanakornkit (2000) developed a saccharified rice yoghurt. To produce a yoghurt-like product, saccharified Jasmine rice was fermented with probiotic LAB. Protocols for making saccharified rice yoghurt are presented in Fig. 3.4. The saccharification was carried out at 55 C using amylase enzymes. To enhance the nutritional value and taste the fortification of such saccharified rice was done with 3% soybean oil, 3% casein, and 0.4% calcium lactate. Rice milk obtained from saccharified and fortified rice was fermented with mixed cultures of L. acidophilus and L. casei ssp. rhamnosus. Further, pectin and strawberry could be added to enhance the taste and consistency. In a rice yogurt, the count of probiotic bacteria was found to be 7.6 3 107 cfu/g. The yoghurt can be stored for at least 20 days at 4 C. Sensory analyses revealed that rice-based yoghurt seasoned with strawberry was well accepted when compared with commercially available strawberry yoghurt. 3.3.3.2 Yosa Yosa is mainly consumed in Finland and other Scandinavian countries. It is made from oat bran pudding cooked in water and fermented with LAB or bifidobacteria. After fermentation, it might be flavored with sucrose or fructose, and fruit jam (Blandino et al., 2003). Yosa has a flavor and texture similar to yoghurt. It is lactose free, suitable for vegetarians, low in fat, and contains β-glucans which can lower the cholesterol levels in the consumers’ blood and reduce the risk of heart disease (Bioferme Oy, 1999). Yosa is a healthy meal because it contains oat fiber and probiotic lactobacilli, which can maintain and improve the human intestinal environment (Toufeili et al., 1997).

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Figure 3.4 Flowchart of saccharified rice yoghurt. Adapted from Wongkhalaung, C., Boonyaratanakornkit, M., 2000. Development of a yogurt-type product from saccharified rice. Kasetsart. J. 34, 107
116.

Cereal-Based Nonalcoholic Beverages 85 3.3.3.3 Beverages From Germinated Cereals Recently beverages obtained from germinated cereal grains such as wheat, barley, finger millet, and moth bean (Chavan et al., 2018; Herrera-Ponce et al., 2014; Mridula and Sharma, 2015) have received a lot of attention. Chavan et al. (2018) developed probiotic drinks using germinated and ungerminated grains of barley, ragi, and moth beans seasoned with sugar and cardamom. Previous studies confirmed the mixture of geminated barley, finger millet, and moth bean being suitable for the propagation of probiotic cultures such as L. acidophilus as those mixtures are rich in the required amounts of carbohydrates, starch, and protein necessary for lactobacilli growth (Maselli and Hekmat, 2016). According to Chavan et al. (2018) probiotic beverages using germinated grains mixture contain a higher probiotic count than probiotic drinks having ungerminated grain mixtures. The main technological processes such as washing, soaking, germinating, drying, roasting, and grinding are applied for the production of such kinds of beverages. Chavan et al. (2018) mixed the grains in a ratio of 2.5:1.5:1 (barley:finger millet:moth bean) with sugar, cardamom, and milk of soy, almond, and coconut. L. acidophilus probiotic culture was applied for germinated cereal drink fermentation for 6 h at 37 C. The authors reported that the germinated probiotic drinks had higher values of trolox equivalent antioxidant capacity and total phenolic content. The addition of soymilk and sugar had a positive effect on the probiotic count in sprouted wheat beverages (Mridula and Sharma, 2015). Previous studies also indicated the suitability of soymilk for LAB growth because of the presence of oligosaccharides, amino acids, and peptides, which are growth-promoting constituents (Chou and Hou, 2000). Ma˚rtenson et al. (2002) have proven that oat-based substrates have a positive influence for the growth of Lactobacillus reuteri, L. acidophilus, and Bifidobacterium bifidum. 3.3.3.4 Prebiotic and Symbiotic Cereal-Based Beverages Prebiotics can be defined as “food materials comprehended by fibers of natural origin that are not digested in the upper gastrointestinal tract and improve the health of the host by selectively supporting the development and activity of particular genera of microorganisms in the colon, mostly lactobacilli and bifidobacteria” (Patel et al., 2014; Pandey et al., 2015). The most common prebiotics used are carbohydrates of low digestibility namely xylooligosaccharides, mannooligosaccharides, pectic-oligosaccharides, galactooligosaccharides, transgalactosylated oligosaccharides, arabinoxylanoligosaccharides, and chitooligosaccharides (Aachary et al., 2011; Damen et al., 2011; Duncan and Flint, 2013). The study of cereals and their health-promoting effects has given special attention to the evaluation of whole-grain fiber due to its prebiotic effects (Alminger and Eklund-Jonsson, 2008). The design of beverages formulated with whole grains and their certain fractions will have beneficial effects on human health by modulating the gut microorganisms with bioactive components of dietary fiber. It is proven that wholegrain fibers from oats and barley lower the postprandial blood glucose and insulin responses (Alminger and Eklund-Jonsson, 2008).

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Connolly et al. (2012) reported that oat whole grain lowers the threat of cardiometabolic disorders and blood glucose, which makes it attractive for developing diets with low-glycemic loads. Wheat arabinoxylan and its oligosaccharides improve production of fermentation health metabolites such as short-chain fatty acids (Damen et al., 2011). Xylooligosaccharides from corncobs lower cholesterol levels and have antiinflammatory, antiallergy, antimicrobial, and improved mineral absorption properties (Aachary et al., 2011). β-Glucans from barley can control food intake and it can even reduce energy intake (Alminger and Eklund-Jonsson, 2008; Xu et al., 2016; Zhu et al., 2016). β-Glucans from oats increase solution viscosity and increase total transit time by delaying gastric emptying, which are related with the reduction of blood glucose level, total and LDL cholesterol (Sethi et al., 2016). The application of mild processing conditions such as fermentation could support the development of cereal beverages with high β-glucans values (Alminger and Eklund-Jonsson, 2008; Xu et al., 2016; Zhu et al., 2016). According to Verspreet et al. (2015) wheat fructans selectively fermented by colon microorganisms exert modifications in the gastrointestinal microorganisms conferring health benefits. In this regard, barley and oat-fermented beverages have the highest potential for market success due to their health benefits related to the phytochemicals and dietary fibers such as β-glucan. An important matter in the development of novel drinks containing β-glucans from oat and barley is to outline the right dose that will provide beneficial effects on health such as decreasing blood cholesterol and LDL levels. Synbiotics are “a selective blend of probiotics and prebiotics that have a proven effect of improving the viability of activating the metabolic functions of health-promoting bacteria predominantly lactobacilli and bifidobacteria in the upper and lower gastrointestinal tract” (Pandey et al., 2015). After it was proven that these components were able to improve our health, the importance of using combinations of probiotics and prebiotics increased (Pandey et al., 2015). The evaluation of physicochemical characteristics and sensory properties of novel products is a significant task that requires to be investigated as these properties strongly influence the acceptance of new cereal-based synbiotic drinks by consumers. During the investigation of potential synbiotic beverages made with quinoa, soy, and fructooligosaccharides additives fermented with the probiotic L. casei LC-1 strain it was observed that such beverage could support the growth of probiotic bacteria, possess prebiotic features, and has acceptable sensory attributes (Bianchi et al., 2015).

3.4 Future Trends 3.4.1 New Probiotic Cultures Selection and Application for Beverages Production Newly developed fermented cereal-based drinks should be favourable globally, including developing countries, as those products are highly nutritious, as well as including Western

Cereal-Based Nonalcoholic Beverages 87 countries, due to increasing amount of consumers tend to choose healthy lifestyle (vegan, vegetarian, low-calorie, low-fat, and low-salt). To meet these needs, an appropriate LAB starter culture and cereal-based raw materials must be selected. LAB strains are suitable for the biopreservation of cereal-based beverages. Ideally, selected strains should be highly antibacterial, antifungal, and antimycotoxigenic. Those strains should be able to bind mycotoxins and possess proteolytic activity for toxic peptides neutralization and flavorcontributing amino acid releasing (Waters et al., 2015). Moreover, those strains should have the ability to ferment cereals while synthesizing oligosaccharides, thus presenting a major opportunity for the development of safer cereal-based functional prebiotic beverages. Usually, fermentation mainly includes probiotic cultures belonging to Lactobacillus or Bifidobacterium genera (Bansal et al., 2016; Pandey et al., 2015; Patel et al., 2014). The most common probiotic strains are presented in Table 3.3. Probiotic strains isolated from the health human gut belonging to Lactobacillus and Bifidobacterium genera are favorable for new cereal-based beverage technologies creation. In order to produce new fermented products, the starter cultures, preferred probiotics, must be able to grow and dominate in the cereal’s medium, and produce the desired textured and flavored compounds, as well as having health-beneficial compounds. Bacteria-producing lactic acid have been used for cereal fermentations for centuries and many cereals are known to be able to support their growth, whereas low levels of fermentable carbohydrates in some grains may cause a problem (Zannini et al., 2012). To overcome this, sugars and food-grade yeast extracts can be added to the media. Moreover, germinated raw material can be used to increase the amount of fermentable sugars and amino acids by improving the Table 3.3: Most common probiotic strains (Bansal et al., 2016; Blandino et al., 2003; Fijan, 2014; Pandey et al., 2015; Patel et al., 2014; Peyer et al., 2016). Bacterium Genus

Species

Bacillus spp. Bifidobacterium spp.

B. coagulans, B. subtilis B. adolescentis, B. animalis, B. bifidum, B. breve, B. brevis, B. longum, B. infantis, B. thermophilum, B. lactis L. acidophilus, L. bifidus, L. brevis, L. bulgaricus, L. casei, L. cellobiosus, L. cremoris, L. crispatus, L. delbrueckii subsp. bulgaricus, L. collinoides, L. dextranicum, L. fermentum, L. gallinarum, L. gasseri, L. helveticus, L. johnsonii, L. reuteri, L. rhamnosus, L. ruminis, L. johnsonii, L. lactis, L. paracasei, L. plantarum, L. raffinolactis, L. reuteri, L. rhamnosus, L. salivarius, L. sakei, L. thamnosus, L. vitulinus Lact. lactis subssp. lactis, Lact. cremoris L. mesenteroides, L. paramesenteroides P. acidilactici, P. halophilus, P. pentosaceus S. cremoris, S. diacetylactis, S. equinus, S. faecium, S. lactis, S. salivarius subsp. thermophiles Propionibacterium freudenreichii, Enterococcus faecium, Enterococcus faecalis, Sporolactobacillus inulinus Saccharomyces bayanus, Saccharomyces boulardii, Saccharomyces cerevisiae

Lactobacillus spp.

Lactococcus spp. Leuconostoc spp. Pediococcus spp. Streptococcus spp. Other bacteria Yeasts

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growth of probiotic strains (Charalampopoulos et al., 2002). It was suggested that a minimum of 107 probiotic bacterial cells should be alive at the time of consumption per gram or milliliter of the product (Homayouni et al., 2008). Despite the antimicrobial activity of the LAB from cereal-based fermented foods, the use of these lactobacillus and their fermented products for the production of new probiotic beverages is also in its infancy (Blandino et al., 2003). The term “probiotic” refers to a product containing mono- or mixed-probiotic cultures of alive microorganisms which, when ingested, improve the health status and/or beneficially affect human health by improving its microbial balance (Salovaara, 1996). Cereal grains can be applied as nutrient sources that not only promote several beneficial physiological effects, but can also stimulate the growth of bifidobacteria and lactobacilli (Charalampopoulos et al., 2002; Herrera-Ponce et al., 2014; Patel et al., 2004; Rathore et al., 2012). Much research confirms that cereals such as malt, wheat, barley, and oats are able to support bacteria such as L. fermentum, L. reuteri, L. acidophilus, L. plantarum, and Bifidobacterium spp. growth and increase their acid and bile tolerance (Charalampopoulos et al., 2002, 2003; Michida et al., 2006; Patel et al., 2004; Rozada-Sa´nchez et al., 2008). Kedia et al. (2007, 2008) confirmed that fermentations of different fractions of cereal grains, for example, oat and malt with L. reuteri, L. acidophilus, and L. plantarum produced higher lactobacilli levels than those obtained with the use of the whole grain. Combined culture fermentations in cereal-based media, for example, in malt and barley, produced similar counts of L. acidophilus and L. plantarum cells, but the production of organic acids was significantly different. Therefore the sensory properties are unique for each fermented cereal beverage (Rathore et al., 2012). Herrera-Ponce et al. (2014) reported that different inoculum levels did not display a significant influence on probiotic lactobacilli such as L. rhamnosus, L. casei, and L. acidophilus growth. It was observed that protein-supplemented simple, germinated, and malted oat improved the cell viability of the probiotic strains. The use of probiotics in cereal-based beverage production has attracted great interest (Saavedra, 2007) due to their ability of gut wall translocation, immune system stimulation (Mustafa et al., 2009), and production of substances that affect intestinal pain receptors (Rousseaux et al., 2007; Zocco et al., 2007) and epithelial function modulation (Martins et al., 2007).

3.4.2 Micro- and Nanoencapsulation Techniques for Improved Probiotics Surveillance Probiotics must prevent against several diseases, therefore they must survive in gut pH, reach the small intestine, and colonize the host. To improve the survival of probiotic microorganisms during gastric transit, encapsulation is considered as a promising process (Shori, 2017). Varieties of polymers such as alginate and chitosan are commonly used for

Cereal-Based Nonalcoholic Beverages 89 encapsulation of probiotic bacteria. Moreover, encapsulation of probiotics using plant-based materials such as pea protein isolate and fructooligosaccharides may play a significant role in food applications (Klemmer et al., 2011). There is widespread interest in the improvement of the physical and mechanical stability of polymers used in probiotics encapsulation. Different techniques have been applied to increase the resistance of probiotics against gastric conditions. Factors such as acid resistance properties of probiotic strains, encapsulating materials and their concentrations, encapsulation methods, and types of polymers incorporated in the matrix can affect the protection and survival of encapsulated probiotics during gastric transit (Shori, 2017). Encapsulation of a probiotics layer-by-layer technique is very effective to improve the protection and viability of the probiotic microorganisms in the gastric tract. Examples of microencapsulation on the protection of probiotics able to apply for food and can be adapted to beverages are given in Table 3.4. The development of novel micro- and nanoparticles of inorganic or organic structures are necessary to ensure the pass of probiotics through the unfavorable conditions of the gastrointestinal tract; consequently, a novel trend in food technology includes the creation of nanogels, nanocapsules, or microcapsules (Salmero´n, 2017; Shori, 2017). The incorporation of probiotic cultures in nanogels or nanocapsules can improve the delivery of probiotics or other bioactive compounds. The main important requirement is that the Table 3.4: A few microencapsulation techniques on the protection of probiotics. Probiotic

Type of Encapsulating Material

References

Bifidobacterium adolescentis Bifidobacterium animalis

Gelatin microspheres with alginate Pea protein isolate-alginate with fructooligosaccharide Ca-alginate

Bifidobacterium bifidum Bifidobacterium breve

Alginate
chitosan Alginate
chitosan and fluid-bed drying Poly D,L-lactic-co-glycolic acid containing prebiotic galactooligosaccharides incorporated into an alginate
chitosan matrix Alginate and human-like collagen Alginate-CaCO3Alginate-Ca-ethylenediaminetetraacetate Carrageenan-locust bean gum-coated milk Alginate
chitosanAlginate
chitosan
carboxymethyl chitosan Alginate
chitosan Chitosan-coated alginate capsules with locust bean Ca-alginate

Annan et al. (2008) Klemmer et al. (2011) Guimaraes et al. (2013) Chavarri et al. (2010) Cook et al. (2011) Cook et al. (2014)

Bifidobacterium longum Lactobacillus acidophilus Lactobacillus bulgaricus Lactobacillus casei Lactobacillus gasseri Lactobacillus rhamnosus

Enterococcus faecium Saccharomyces boulardii

Alginate
chitosan Chitosan/dextran sulfate

Su et al. (2011) Cai et al. (2014) Shi et al. (2013) Li et al. (2011) Chavarri et al. (2010) Cheow et al. (2014) Guimaraes et al. (2013) Kanmani et al. (2011) Thomas et al. (2014)

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molecules used to create nanomaterials must be recognized as safe. The most common nanomaterials are biopolymers designed from carbohydrates and proteins. The versatility of polysaccharides is that they have hydrophobic and hydrophilic motifs with flexible extension in the same molecule that generates matrices sensitive to environmental conditions. This is an outstanding feature because the regulation of the nanoparticle surface influences the interaction within the cell surface and can modulate the delivery of the food-grade nanoparticles in the gastrointestinal tract (Santiago and Castro, 2016). Therefore further research is required in polysaccharides isolated from cereal sources that could be used to design nanocapsules with bioactive compounds, which could be applied in the creation of unique cereal-based fermented beverages with health improvement properties.

3.4.3 Nanotechnology Application for Functional Cereal-Based Beverages Nanoscience has developed tools that can be applied in the functional cereal-based beverages production and bioprocessing industries (Neethirajan and Jayas, 2011). The application of food-grade nanoparticles has potential for their incorporation into novel cereal-based beverages; however, it is still necessary to evaluate the ability of nanoparticles to pass through the gastrointestinal tract and to reach the desired target. In vivo studies that evaluate the influence of food-grade nanoparticles to the human gastrointestinal tract are limited. The investigation of the effect of food-grade nanoparticles to the intestinal tract pH, bile acids, and exposure time should be tested to establish the bioactivity of these new nanoparticles and estimate whether they can be incorporated into the creation of novel fermented cereal-based beverages (Salmero´n, 2017). Recently nanoparticles such as zinc oxide particles that pose antidiabetic effects (El-Gharbawy, et al. 2016; Umrani and Paknikar, 2013), silver nanoparticles (Le Ouay and Stellacci, 2015), and nanoinorganic metal oxide (Tang and Lv, 2014), gold nanoparticles have exhibited promising applications in the development of anticancer drugs (Zhu and Liao, 2015) and have good antibacterial properties have attracted great interest. There is great interest to create novel synthesis methods that will improve the incorporation of these nanoparticles into different cereal-based beverages (Kalakotla et al., 2015) due to the certain health attributes and physicochemical properties of nanoparticles (Salmero´n, 2017).

3.4.4 Colloidal Delivery Systems for Food-Grade Nanoparticles In order to improve the incorporation of insoluble particles into functional beverages, the creation of colloidal delivery systems has attracted great interest. Delivery systems can be created using polymers as a base for micro- or nanoparticles, liposomes, or micelles (Salmero´n, 2017). Three types of colloidal dispersions can be applied: liquid-in-liquid, solid-in-liquid, and self-assembled molecules (Ismail et al., 2015). Applying colloidal

Cereal-Based Nonalcoholic Beverages 91 delivery systems, the nanoparticles containing insoluble compounds can be delivered, therefore, molecules that previously were not attractive for application due to their insolubility would, with this technique, be able to reach the target. Thus healthier cereal-based fermented beverages can be created.

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Further Reading Berger, K., Falck, P., Linninge, C., Nilsson, U., Axling, U., Grey, C., et al., 2014. Cereal byproducts have prebiotic potential in mice fed a high-fat diet. J. Agric. Food Chem. 62, 8169
8178. Subrota, H., Shilpa, V., Brij, S., Vandna, K., Surajit, M., 2013. Antioxidative activity and polyphenol content in fermented soy milk supplemented with WPC-70 by probiotic Lactobacilli. Int. Food Res. J. 20, 2125
2131.

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CHAPTER 4

Ready-to-Drink Tea Kriti Kumari Dubey, Madhura Janve, Aratrika Ray and Rekha S. Singhal Food Engineering and Technology Department, Institute of Chemical Technology, Mumbai, India

Chapter Outline 4.1 Introduction 102 4.2 Types of Ready-to-Drink Tea 103 4.2.1 Instant Tea Powder 103 4.2.2 Batch Brewed Tea 104 4.2.3 Brewed Tea Extract 104

4.3 4.4 4.5 4.6 4.7 4.8 4.9 4.10 4.11 4.12 4.13 4.14 4.15 4.16 4.17 4.18 4.19 4.20 4.21 4.22 4.23

Raw Materials for the Manufacture of RTD Tea 105 Green Tea Leaves 108 Black Tea Leaves 111 Additives 112 Prebiotic and Probiotic Components of Different Types of RTD Tea Manufacturing and Processing of RTD Tea Beverages 117 Extraction of Black and Green Tea Extract 117 Taste Enhancement of RTD Tea 117 Color Improvement of RTD Tea 118 Aroma Enhancement of RTD Tea 118 Clarity of RTD Tea 119 Mouthfeel of RTD Tea 119 Prevention of Creaming of RTD Tea 120 Shelf Stability of RTD Tea 121 Packaging of RTD Tea 122 Sensory Evaluation of RTD Tea Beverages 123 Health Benefits of RTD Tea 124 Safety of RTD Tea During Processing and Consumption 125 Bioavailability of RTD Tea Constituents 129 Ready-to-Drink Tea Market 130 Factors Affecting RTD Tea Manufacturing 131 4.23.1 Product Innovation 131 4.23.2 Raw Material Sourcing 131 4.23.3 Process Development 132

Trends in Non-alcoholic Beverages. DOI: https://doi.org/10.1016/B978-0-12-816938-4.00004-5 © 2020 Elsevier Inc. All rights reserved.

101

112

102 Chapter 4 4.23.4 Testing of Quality Parameters 132 4.23.5 Packaging 132 4.23.6 Marketing 132

4.24 Conclusion 133 References 133 Further Reading 139 Websites 139

4.1 Introduction The general public view of modern diet and human health has undergone drastic changes in recent years. Rapid socioeconomic development coupled with improper or unhealthy eating disorders has resulted in the rise of several diseases such as obesity, heart disease, cancer, and diabetes. The high cost associated with healthcare compels modern young consumers to inculcate self-nutrition and preventive healthcare behavior as well as wisely choosing among various options available in the market. Rising healthcare expenditure due to improper food consumption and growing concerns among the ageing population regarding heart health and obesity is also augmenting the demand for nutritious snacks and beverages. Fast-changing lifestyles that encourage “on the go” eating and the growing trend to replace meals with smaller nutritional snacks are encouraging the adoption of the ready-to-eat snacks and drinks. The trend of being proactive to avoid chronic health problems is creating an astounding insist for nonalcoholic, ready-to-drink (RTD) tea as a suitable beverage option as it offers several health benefits due to the presence of antioxidants and other essential ingredients. RTD tea is a good alternative for consumers seeking refreshing products without sacrificing taste. Tea is an infusion prepared by boiling dried plant parts such as leaf, flower, stem, or fruit in water. Depending on the type of leaf (e.g., Camellia sinensis) used, the brewed beverage can be classified as green or black tea. Apart from the common brewing methods, certain teas can be prepared by fermentation of the brew with beneficial microorganisms to develop RTD fermented tea which is better known as Kombucha tea. RTD ice tea is a ready prepared tea, mostly black or green, and generally consumed cold. It can be sweetened, unsweetened, flavored, or unflavored. RTD ice tea can be produced either from tea extract (as powder or concentrate) or as a freshly brewed extract. Thus, it can either be prepared from instant tea powders by the addition of cold water or can be already prepared and available as a bottled drink. By product type, the ice-tea market is segmented as liquid RTD, concentrated sirup, and premix. Among these segments, liquid ice tea is most consumed and also represents a steady growth. Powder premixes are available in different sizes, flavors, and convenient to carry and mix and, hence, is expected to grow. Concentrated sirup includes sugar, flavor, and tea extract; it is easy to dissolve and convenient to use. The ice tea market is also segmented into flavor options such as lemon, peach, passion, mint, ginger, herbal, and others. Different types of

Ready-to-Drink Tea 103 fermented RTD teas are available depending on the type of tea used and the bacterial culture inoculated. These fermented beverages, due to the presence of beneficial bacteria, are probiotic. Apart from RTD teas prepared from C. sinensis, there is another class called herbal teas which are of two types, viz. tropical and temperate herbal teas, depending on the climatic conditions of the plant growth. Lemongrass (Cymbopogon citratus), lemon myrtle (Backhousia citriodora), guava (Psidium guajava), rooibos (Aspalathus linearis), bitter gourd (Momordica charantia), and getto (Alpinia zerumbet) are some of the types of tropical herbal teas. The temperate herbal teas include oregano (Origanum vulgare), mint (Mentha spicata), peppermint (Mentha piperita), rosemary (Rosmarinus officinalis), and chamomile (Matricaria recutita) (Chan et al., 2010). The worldwide popularity of tea prepared from leaves of C. sinensis is greater than other herbal teas. Recent technological advancements in the field of the RTD market has brought convenience and ease during processing, packaging, marketing, and consumption of the finished product for industrial manufacturers and consumers.

4.2 Types of Ready-to-Drink Tea Ice tea is manufactured in two ways such that it can be available as a powder format or as an RTD liquid. Conventional manufacturing provides end products in the form of powder or concentrate. Tea leaves are generally brewed with hot water and dried to produce tea powder or concentrated to produce tea concentrate. This water-soluble extract is then dissolved in water and combined with other food ingredients (sweeteners, flavors, acidity regulators, etc.). The tea leaves are directly extracted to provide a fresh brew which becomes the final RTD product. Selected tea leaves are brewed with hot water and the infusion is filtered to remove residuals and insoluble particles. Other food ingredients (sweeteners, flavors, acidity regulators, etc.) are premixed separately and added to the fresh brew. The emergent awareness of the relationship between diet and health has led to an increase in demand for food products that support health as well as providing basic nutrition. Probiotics and prebiotics are components that are either present in foods or can be incorporated into foods, thus yielding health benefits due to their interactions with the gastrointestinal tract.

4.2.1 Instant Tea Powder Formulation of instant RTD powder was started in the first half of the 20th century to cater the need of RTD ice tea market. Instant tea powder is manufactured by precipitating a soluble tea solid or by spray drying the tea onto a carrier. Spray-drying involves temperatures that flash off valuable volatile flavor components. During spray drying, there are chances of a generation of oxidation reactions leading to the production of unpleasant flavor molecules in the dried powder. As a result, products in which instant tea powder is the principle ingredient often needs additional flavors to impart the characteristic flavor and aroma notes to the dried instant RTD powder. Therefore older methods of instant tea

104 Chapter 4 production involving spray drying is no longer a favored choice for the production of clean, strong tea profiles. The addition of sweeteners plays a major role in improving the sensory profile of instant tea powder. Added sweetener improves the taste of instant RTD, but does not enhance the flavor profile. The physical analysis, bulk density, color, solubility and chemical analysis, moisture content, total polyphenol content, and antioxidant activity are determined to maintain the quality and uniformity of products in different batches. Instant tea produced by the spray drying method has been found to be of good color, pungency, and other liquoring characteristics. Thus there are considerable savings in the economy since the juice and the residue are converted into value-added products.

4.2.2 Batch Brewed Tea In recent times, modern-day consumers are attracted towards real brewed products with authentic, premium, sensory appeal. Therefore high-quality brewed liquid teas are being used as the base for the production of RTD iced tea beverages. The batch-brewing process of liquid tea involves brewing tea at industrial scale in large volumes. The process involves steeping tea leaves in large tanks of heated water to make a single-strength or slightly concentrated brewed tea. The resulting steeped beverage possesses good shortterm clarity and robust flavor and earns the designation of “real-brewed” on the finishedproduct label.

4.2.3 Brewed Tea Extract A brewed tea extract gives processors all the advantages of batch-brewed tea without the costs, hassles, or potential inconsistencies. Brewed tea extracts are of high quality, very clear and are excellent tasting RTD beverages currently produced at commercial scale. The most important step is a selection of high-quality tea leaves for the production at industrial scale. Therefore sourcing of premium quality tea leaves plays an important role. Procured tea is brewed in closed, continuous brewing systems that prevent loss of steam, flavors, and keynote aromatic volatiles during processing and remain integrated with the processed liquid brew. Closed systems during processing makes it more efficient and consistent than batch brewing. After brewing, the brew is separated into multiple components, and undesirable solids (leading to cloudiness) are removed. The finished product or beverage obtained by this method possesses improved clarity, stability, and intact flavor components over a long period. A brewed-tea extract ensures ease of production, finished-product consistency, and feasibility of production at different geographical locations. The finished product can later be customized into different RTD categories like sweetened/unsweetened, flavored/unflavored, and others, to cater for the demand of a different range of customers. The brewed RTD tea components can be adjusted and recombined according to market demand for flavor, color,

Ready-to-Drink Tea 105 sweetness, and other properties while maintaining quality standards. Advancements in the field of the RTD manufacturing process with the advent of new technologies allocate the creation of finished extracts adapted to the manufacturers’, marketers’, and customers’ preferences and needs. Brewed tea products exhibit consistent quality in individually packaged items (glass bottles, plastic bottles, tetra packs, etc.) resulting in enhanced shelf life leading to a positive impact on the growth of RTD industry. Tables 4.1
4.4 documents the types of RTD tea available in the market.

4.3 Raw Materials for the Manufacture of RTD Tea RTD tea is manufactured from a tea infusion, sugar, and additives. Two main varieties of tea are generally used for RTD manufacturing, the smaller leaf China variety (C. sinensis var. sinensis), typically used for green tea manufacture, and the larger leaf Assamica variety (C. sinensis var. assamica) typically used for black tea manufacture. Depending on the different ways of processing, especially the extent of fermentation, tea is usually divided into three basic types, namely green tea (nonfermented), oolong tea (semifermented), and black tea (fully fermented). Apart from this, by combining the ways of processing and the characteristic quality of manufactured tea, tea can be classified into six types: i. ii. iii. iv. v. vi.

Green tea Yellow tea (involves withering) Dark tea (containing brick tea and Pu-erh tea) White tea Oolong tea Black tea

Tea is loaded with polyphenolic constituents which have high antioxidant, antiinflammatory, antimutagenic, and anticarcinogenic properties in various biological systems. The phenolic content in tea is represented by the natural plant phenols and polyphenols components. Polyphenols in tea contain catechins, theaflavins, flavonoids, and tannins which are known to affect the flavor and are speculated to provide probable health benefits. Tea contains large amounts of various flavonoids, which are characterized by the benzopyrane skeleton, with the pyrane ring bearing one or more aromatic ring. Catechins comprise approximately 25% of the dry weight of fresh tea leaves, although total catechin content varies widely depending on species, light variation, season, growing location, clonal variation, and altitude. Catechins are present in nearly all teas made from C. sinensis leaves and include green tea, black tea, white tea, and oolong tea. Catechins include epicatechin (EC), epigallocatechin (EGC), epicatechin-3-gallate (ECG), and epigallocatechin-3-gallate (EGCG). Other catechins, such as catechin gallate, gallocatechin (GC), gallocatechin galllate, EGC-digallate, methyl-EC, and methyl EGC are present in minor quantities. EGCG

106 Chapter 4 Table 4.1: Types of RTD ice tea products available in the market. Brand Name Ice-steeped cold brew (sweetened and unsweetened) Lipton

Variants/Flavors Distinctive Constituents G G G

G G G

Pure leaf (sweetened and unsweetened)

G G G G G G

Nestea

G

G

AriZona

G G

G

Role (no added sugar)

G

G G G

Snapple (containing aspartame) Gold Peak Tea (sweetened and unsweetened)

G G G G G G

Manufacturer References

Orange Raspberry Peppermint

Green tea, organic dried orange/ raspberry/peppermint, natural flavor, and ascorbic acid

ITO EN

www.itoen.com

Citrus Berry Peach

Green or black tea, juice concentrate, natural flavor, malic acid, citric acid, ascorbic acid, sodium polyphosphates, potassium sorbate, ethylenediaminetetraacetic acid (EDTA), and purified stevia leaf extract Brewed green/black tea, natural flavor, pectin citric acid, and sugar

Unilever

www.liptontea. com

Tea extract, natural flavor, citric acid, and steviol glycosides

Nestle´

www.nestea.com

Green/black tea extract, natural flavor, ginseng flavor, honey, ascorbic acid, and citric acid

Arizona Beverages USA

www.drinkarizona. com

Blend of green and black tea, juice concentrate, turmeric extract, ginger flavor, curcumin, and black pepper

Role Tea

www.drinkroletea. com

Lemon Pomegranate Peach Raspberry Mint Honey Black tea in peach and lemon flavors Green tea in lime-mint and raspberry flavors Peach Ginsengplum Honeylemon Turmeric and ginger in apple Lemon Mango Peach Peach Mango Raspberry Lemon Peach Raspberry

Green or black tea, natural flavors, and citric acid

www.pureleaf.com PepsicoUnilever joint venture

Dr Pepper Snapple Group Brewed green/black tea, natural The Coca flavors, caramel color, citric acid, Cola and phosphoric acid Company

www.snapple.com

www. goldpeakbeverages. com (Continued)

Ready-to-Drink Tea 107 Table 4.1: (Continued) Brand Name Brisk Iced Tea

Variants/Flavors Distinctive Constituents G G

G G G G G

G G G

Fuze Iced Tea

G G G G

Honest Tea

Teavana (sweetened and unsweetened)

G

G

G G

G

Long Island Iced Tea (unsweetened and diet)

G G G G G G

Lemon Strawberrymelon Fruit punch Lemonade Peach Blueberry Pineapplepassion fruit Raspberry Watermelon Cherry Watermelon Lemon Berry punch Honeyginseng

Lemon

Pineappleberry Mango Strawberryapple Passion tango Peach Lemon Guava Mango Raspberry Honey

Manufacturer References

Black or green tea, natural flavor, PepsiCo and www.drinkbrisk. citric acid, ascorbic acid, high Unilever Joint com fructose corn sirup, sodium Venture polyphosphates, potassium sorbate, gum arabic, citrus pectin, acesulfame potassium, glycerol ester of rosin, sucralose, calcium disodium EDTA, yellow 5, and yellow 6

Green/black tea powder, natural flavors, citric acid, high fructose corn sirup, sucralose, phosphoric acid, potassium citrate, potassium sorbate, sodium benzoate, calcium disodium EDTA, vitamin B6, and vitamin B12 Brewed black tea, juice from concentrate, organic lemon extract, citric acid, and organic cane sugar Green/black tea infusion, spearmint/lemon verbena/ lemongrass/natural flavor, and citric acid

The Coca Cola Company

www.cocacolaproductfacts. com

The Coca Cola Company

www.cocacolaproductfacts. com

Starbucks and Tata

www.teavana.com

Black/green tea, natural flavor, citric acid, and cane sugar

Long Island Iced Tea

http://www. longislandicedtea. com

due to its potential health effects is being investigated by the scientific community. The catechins content of tea is metabolized into hydoxybezoic acids and its derivatives in humans after consumption. Flavanols, including kaempferol, myricetin, quercetin, and their glycosides are also present in tea leaves. The three main types of theaflavins found in black tea are theaflavin, theaflavin-3-gallate, and theaflavin-3, 3-digallate. Thearubigins are polymeric polyphenols that are formed during the enzymatic oxidation and condensation of

108 Chapter 4 Table 4.2: Types of tea premixes available in the market. Brand Name Society Instant Tea Premix

Variants/Flavors G G G G

TEAki HUT Instant Black Tea Powder Instant Tea Matcha Organic Instant Tea

G

G G

G G G G

Nestea Iced Tea

Premium Instant Tea

G

G

Constituents

Manufacturer References

Elaichi Masala Ginger Lemongrass Unsweetened (no flavors/ preservatives/ colors/fillers) Mango Kiwi

Black tea

Amar Tea Private Limited

Black Tea Instant Tea Jasmine Tea Oolong Tea Lemon flavor

Royal Chai

http://www. societytea.in

100% pure black tea made from TEAki Hut ground tea leaves of any kind added

www.amazon. com

Green tea powder

10th Avenue Tea

100% organic tea

One organic

https:// 10thavenuetea. com http:// oneorganicbrand. com

Sugar, citric acid, maltodextrin, malic acid, tricalcium phosphate (prevents caking), natural lemon flavor, sucralose 100% natural

Nestle

https://www. nestle.in

Royal Chai

http://royalchai. net/sit/

two gallocatechins (EC and ECG) with the participation of polyphenol oxidases during the fermentation reactions in black tea. Thearubigins are responsible for imparting a reddish color to fully oxidized tea.

4.4 Green Tea Leaves Green tea has a complex chemical composition. Carbohydrates including cellulosic fiber and pectic substances form the largest component of tea leaves (up to 33% dry weight) and contribute to about 11% (w/w) of extract solids (Graham, 1992). While xanthic bases such as caffeine and theophylline are the most well-known nitrogenous component of tea, tea proteins and amino acids contribute significantly to the composition of both the leaf (15%
20% dry weight) and extract. In addition to the common amino acids, there is a unique amino acid known as theanine (y-N-ethyl glutamine) which is believed to be the major amino acid present in tea, comprising about 3% (w/w) of extract solids. It is a significant component of green (Sakato et al., 1950) and black tea (Feldheim et al., 1986) and has been associated with improved flavor and modulation of the stimulative effects of caffeine (Kimura and Murata, 1971). Tea leaves also have fatty acids such as linoleic and

Ready-to-Drink Tea 109 Table 4.3: Types of fermented teas available in the market. Brand Name KeVita Master Brew Kombucha

Variants G

G

G G

G

G

Kombucha organic and raw

G G

G

G

G G G G

G G

Kombucha raw and organic Buchi Kombucha

G G G

G G G G G G G

Blueberry Basil Dragonfruit Lemongrass Ginger Grapefruit Lavender Melon Pineapple Peach Raspberry Lemon Roots Beer Tarts Cherry Mojito Cosmic Cranberry Superfruits Raspberry Rush Divine Grape Triology Rose Ginger Chia Raspberry Chia Ginger berry Grape Chia Strawberry Serenity Ginger Lemon Aloe Chilly Air Earth Water Fire Seed Holiday Avonlea

Distinctive Constituents

Manufacturer References

Filtered water, black tea extract, green tea extract, natural flavor, fruit concentrate, cane sugar, fruit and vegetable juice for color, kombucha culture

KeVita

https://www. kevita.com

Polyphenols, glucuronic acid, L(1) lactic GTS acid, acetic acid, probiotics Bacillus coagulans GBI-30 6086, S. Boulardii

https:// gtslivingfoods. com

B-tea Pilsner laden water, organic Japanese bancha green tea, organic lemon balm, organic cane sugar, kombucha (Medusomyces gisevi) live culture Organic raw kombucha, organic roasted Buchi roots tea (dandelion, burdock, chicory), kombucha organic apple juice, organic roasted barley (trace amount), organic malt extract, organic herbal tea (holy basil, stinging nettle, rhodiola rosea), organic spices, organic maple sirup, organic cane sugar and molasses, organic kombucha culture, organic molasses

https:// btkombucha. com/ https://www. drinkbuchi.com

(Continued)

110 Chapter 4 Table 4.3: (Continued) Brand Name

Variants

Suja Organic Kombucha

G

G

G

G

Tonica

G G G

Ginger lemon Peach Ginger Lemon Cayenne Ginger Turmeric Ginger Blueberry Peach Mango

Distinctive Constituents

Manufacturer References

Organic kombucha, organic lemon juice, organic ginger juice, organic ashwagandha, organic cane sugar, and probiotic Lactobacillus rhamnosus

Suja

https://www. sujajuice.com

Fermented organic green and black tea, fine-cut ginger, natural ginger extract, organic cane sugar, kombucha culture (yeast and bacteria cultures)

Tonica Kombucha

http:// tonicakombucha. com

Table 4.4: Types of tea bags available in the market. Brand Name

Variants/Flavors

Manufacturer

References

Lipton (black and green iced tea)

Citrus Berry Peach Unflavored Masala Lemon Ginger Mint Lemon Aloe Vera Masala Elaichi Honey (some variants contain vitamin C and B6) Spicy Ginger Fragrant Cardamom Rich Masala Fresh Lemon Taj Mahal Honey Lemon Green Chamomile Earl gray Peppermint Sencha green Tart blood orange Ginger green

Unilever

www.liptontea.com

Amar Tea Private Limited

http://www.societytea. in

Tetley

https://www.tetley.in

The Brook Bond Taj Mahal Tea House

https://www. tajmahalteahouse.com

Paisley Tea

https://twoleavestea. com

G G G

Society—Tea Bags

G G G

Tetley Tea (green/ black tea)

G G G G G G

Taj Mahal Tea

G G G G G

Paisley Tea Bags

G G G G G G

Ready-to-Drink Tea 111 α-linolenic acids in the lipid fraction; sterols as stigmasterol; vitamins (B, C, E); pigments as chlorophyll and carotenoids; volatile compounds as aldehydes, alcohols, esters, lactones, hydrocarbons, and others; organic acids as oxalic acid, malic acid; and minerals and trace elements (5% dry weight) such as Ca, Mg, Cr, Mn, Fe, and others. Chlorophyll, carotenoids, lipids, and volatile compounds are present as minor constituents in tea infusions, but they also play a significant role in the development of aroma (Hara et al., 1995). Polyphenols, particularly flavonoids, constitute an important part of green tea components. The main flavonoids commonly present in green tea include catechins (flavan-3-ols). EGCG represent 59% of the total catechins, EGC (19% approximately), ECG (13.6% approximately), and EC (6.4% approximately) (Vinson et al., 1995). Green tea also contains gallic acid (GA) and other phenolic acids such as chlorogenic acid and caffeic acid, flavonols such as kaempferol, myricetin, and quercetin, and their glycosides.

4.5 Black Tea Leaves Polyphenols are produced from the controlled enzymatic reactions involved in the fermentation of green leaves during tea production. The fermentation of green tea leaves also results in the development of characteristic aroma components, a darkening of the color of the leaf and extracts, and decreasing astringency with increased fermentation time. The catechins (present majorly in green tea) form the building blocks of black tea polyphenols and form theaflavins, theaflavinic acids, and theurubigins or theasinensis, which are mainly responsible for briskness, brightness, color, and strength (Lee et al., 2008). Theaflavins, formed by the oxidation of quinones in EC, provide a bright, red-orange appearance to the tea beverage and is correlated with the market value of tea (Roberts, 1958). They are present to the extent of 1%
2% in dry black tea and are substantially water extractable (Millin, 1987). Thearubigins are the largely unidentified, highly colored, flavanol oxidation products constituting about 10%
20% in dry black tea (Ullah et al., 1984). Depending on the degree of fermentation, some green tea polyphenols remain unconverted into black tea. Majorly, all the flavonols (free as well as glycosides) present in the initial fresh green leaf remain unoxidized and are likewise present in black tea in similar quantities. Amino acid degradation is involved in the generation of the tea’s aroma (Balentine et al., 1997). Black tea has low tea catechin content [3%
10% (w/w)], with theaflavins and thearubigins accounting for about 2%
6% (w/w) and 10%
20% (w/w) of the dry weight of the leaves, respectively. Theaflavins account for 2%
6% of the dry weight of solids in brewed black tea, is orange or orange-red, and possess a benzotropolone skeleton that is formed from cooxidation of appropriate pairs of catechins, one with a vic-trihydroxy moiety and the other with an ortho-dihydroxystructure (Geissman, 1962). They are produced by the oxidative dimerization of a simple (dihydroxy) catechin and a gallo (trihydroxy) catechin, catalyzed by polyphenol oxidase (Owuor et al., 2006). During the fermentation process of

112 Chapter 4 green tea leaves, wherein black and oolong tea are developed, certain chemical changes occur in the polyphenol content of tea leaves. The polyphenol oxidase converts the monomeric catechins to quinones which further undergo polymerization to bisflavans and more complex structures of theaflavins, thearubigens, and higher molecular mass compounds (Bailey et al., 1993). Bitterness and astringency of steeped black tea are contributed by theaflavins while color is imparted by thearubigins. The presence of theaflavins and their gallates are maximum in black tea because of the oxidative condensation between EC and ECG (Tanaka et al., 2011). However, the lipid oxidation levels of these polymerized components are lower than those of EGCG, ECG, and EGC. Lin et al. (2003) reported and analyzed catechins in the same tea variety by various manufacturers involving different fermentation processes. The levels of EGCG and total catechins in teas were found to be most abundant in the old green tea leaves followed by oolong tea and Pu-erh tea. Liang et al. (2004) reported more intensive oxidation of tea polyphenols by the combined action of microorganisms and environmental oxygen during the black tea fermentation process, resulting in low concentrations of tea polyphenols and tea catechins during fermentation of partially dried leaves piled up in humid conditions (moisture content 40% at 25 C
60 C) for a few weeks.

4.6 Additives Food additives are auxiliary materials of natural or synthetic origin which are added for enhancing the quality of products. The food additives not only help in extending the shelf life of packaged products, but also improve their appearance, color, aroma, texture, and taste. Every food additive performs a specific function. The additives are roughly grouped as color additives, aroma enhancers, sweeteners, solubilizers, preservatives, and texture improvers. Table 4.5 lists the types of additives used in the manufacturing of RTD tea.

4.7 Prebiotic and Probiotic Components of Different Types of RTD Tea Probiotics are the helpful components obtained by incorporating microorganisms that provide probable health benefits to the host or the consumer. Generally, RTD teas are enriched with probiotics with cultures like Bifidobacterium bifidum, Bifidobacterium breve, Bifidobacterium infantis, Bifidobacterium longum, Bifidobacterium lactis, and Bifidobacterium animali. Prebiotics are nondigestible carbohydrates that beneficially affect the host after ingestion as they are available as a selective energy source for probiotic Lactobacilli and Bifidobacteria, stimulating their growth and activity in the colon. The effects of carbohydratetype prebiotics may not always be beneficial, as they can also encourage the growth of nonprobiotic bacteria (Ziemer and Gibson, 1998). Green tea polyphenols like EGCG, EGC, ECG, and EC are effective prebiotics providing active support to the probiotic gut microflora, thereby increasing gut health. A few genera of microflora that are essentially isolated from

Ready-to-Drink Tea 113 Table 4.5: Additives used in ready-to-drink tea. Parameter

Additive

References

Color

E133 E129 E102

Kirksey et al. (1998) [US5780086A]

Aroma

Cinnamic acid Cinnamic acid salts Cinnamic acid esters and their mixtures Recovered tea aroma Sucrose Isomaltulose Aspartame Acesulfame potassium Sodium cyclamate Saccharin Powdered honey Jams, preserves Fresh fruit (cut or ground) Sugar cane pieces Sugars (fructose, glucose, maltose), corn sirups (high fructose corn sirups and high maltose corn sirups), invert sugar (maltodextrins, polydextrose, and cyclodextrins) Polyols (glycerol, propylene glycol, sorbitol, mannitol, maltol, and xylitol) Polyglycerols (triglycerol, hexaglycerol, and decaglycerol) Natamycin (pimaricin) Potassium sorbate Sodium benzoate Parabens Cinnamic acid Acidulant (citric, malic, acetic, succinic, fumaric, lactic, tartaric, ascorbic, hydrochloric, phosphoric, and sulfuric acid) Cellulose microfibrils

Cirigliano et al. (2000a,b) [US6036986A] Mutuku and Sharp (2016) [US20160278398A1]

Sweetener

Solubilizer

Preservative

Mouthfeel improver

¨rr et al. (2009) [US7553509B2] Do Syfert et al. (1988) [US4748033A] Cooper (1999) [US5895672A]

Syfert et al. (1988) [US4748033A]

Cirigliano et al. (1998) [US5773062A] Cirigliano et al. (1999) [US5895681A] Lehmberg et al. (2002) [US6413570B1] Cirigliano et al. (2000a,b) [US6022576A] Anslow and Stratford (2000) [US6042861A]

Koppert and Velikov (2018) [EP2934162A1]

black tea kombucha are Acetobacter (Chen and Liu, 2000), but a species of Gluconacetobacter are also reported (Marsh et al., 2014). Glucooligosaccharides (GOS) and fructooligosaccharides (FOS) are also useful prebiotics added to RTD tea to induce the growth of probiotic microflora which, in return, provide essential health benefits to humans. Tea catechins have potent antibacterial activity (Hara et al., 1995; Diker et al., 1991). They are bactericidal against food-borne pathogenic bacteria, such as Staphylococcus aureus, Clostridium perfringens, Bacillus cereus, and Vibrio parahaemolyticus, but not against Bifidobacteria and Lactobacilli. The effect of tea polyphenols on the fecal flora and

114 Chapter 4 metabolites of pigs was examined by Hara et al. (1995). This study involved feeding eight 30-day old pigs a diet supplemented with 0.2% tea polyphenols for two weeks which resulted in a significant increase in the numbers of Lactobacilli and a significant decrease in total bacteria and bacteroidaceae counts. Goto et al. (1999) administered 300 mg of tea catechins per day to 15 people for three weeks which revealed a statistically significant improvement of the intestinal flora and fecal odorous metabolites. Ishihara et al. (2001) reported that feed containing green tea extracts maintained high fecal counts of Bifidobacterium species and Lactobacillus species in calves. Green tea extract creates a more favorable anaerobic environment for probiotic bacteria due to its oxygen scavenging, antioxidant, and antiradical properties (Shah et al., 2010). It has been established that only 5%
10% of the total polyphenol intake is absorbed in the small intestine. The remaining 90%
95% of total polyphenol may accumulate in the large intestine where, along with the bile conjugates, they are excreted into the intestinal lumen and further subjected to the enzymatic activities of the gut microbial flora. Probiotic bacteria possess certain enzymatic activities such as deglycosylation, ring-fission, dehydroxylation, demethylation, or decarboxylation which can convert polyphenols into more bioavailable or bioactive forms than the original phenolic compounds. The fermentation of flavonol glycosides with some probiotic microorganisms with glucosidase activity such as β-glucosidase, β-galactosidase, or rhamnosidase could improve their bioavailability. This bioavailability is increased since the bacteria transform the flavonol glycoside into its aglycone, which is more absorbable (Uskova et al., 2010; Donkor and Shah, 2008). The colonic microbiota present in the human gut is responsible for the extensive breakdown of the original polyphenols into a series of low-molecular weight phenolic metabolites that, being absorbable, may be responsible for the health effects derived from polyphenol-rich food consumption. The effects of different types of prebiotic and probiotic components are listed in Table 4.6. Jayabalan et al. (2008) studied kombucha fermentation using green tea, black tea, and fermented tea waste and analyzed the transformation in tea polyphenols. In comparison to black tea kombucha and tea waste kombucha, much less degradation of EGCG (18%) and ECG (23%) was observed in green tea kombucha. Theaflavin and thearubigin were found to be relatively stable when compared to EC isomers. The amount of theophylline was found to be significantly increased in black tea fermentation by yeast Dabaryomyces hansenii for ten days. Due to the reduction of caffeine and excess tannins in significant amounts for consumption, fermented black tea was reported as a modified beverage with higher nutritive values (Pasha and Reddy, 2005). Kim et al. (2013) studied the changes in green tea fermentation using A. oryzae fungus strain and reported that the major flavonoid compounds of GC, EGCG, and ECG decreased significantly during fermentation, whereas the levels of phenolic compounds, such as GA, 3-p-coumaroylquinic acid, and other flavonoid metabolites like GC, EC, and ECG increased significantly during fermentation. The

Ready-to-Drink Tea 115 Table 4.6: Prebiotic and probiotic components of different types of tea. Prebiotic/Probiotic Type of RTD Tea Components

Brief Summary

References

Prebiotic Components Green Tea

EC, EGCG, ECG, and EGC

Green tea extracts were reported Vodnar and Socaciu (2012) to protect the viability and stability of B. infantis and B. breves microencapsulated in chitosan coated with alginate microcapsules which improved gastrointestinal conditions

Kombucha Tea

Gluconic acid,glucose, and fructose

Antimicrobial, antioxidant, hepatoprotective, and anticancer properties of kombucha tea were reported

Jayabalan et al. (2014)

Herbal Tea with Raw dandelion greens

Phenylpropanoids, triterpenoid, and saponins

Dandelion leaves containing phenylpropanoids, triterpenoid, and saponins attributed to their prebiotic activity

Yarnell and Abascal (2009)

Black Tea

Black tea polyphenols (BTP)(theaflavins and thearubigens), galacto-oligosaccharides (GOS), inulin, and fructooligosaccharides (FOS)

BTP was reported to possess potential antimicrobial activity. BTP showed different level of resistance to varied bacterial strains. Synergistic and beneficial effect on the initial micorbial composition was also reported

Duynhoven et al. (2013) Tewari et al. (2018)

Black Tea

Inulin

Inulin can be used in milk Chowdhury fortification developing antibiotic (2016) resistance through the presence of L. casei

Black Tea

1-Kestose, nystose, FOS, GOS, xylo-oligosaccharides (XOS), isomalto-oligosaccharides, raffinose, and lactosucrose

Lactobacillus paracasei strains reported to metabolize all oligosaccharides, but when cultured with FOS, sucrose was found to be remaining in the extract

Black Tea

GOS, FOS, inulin, lactulose, maltodextrin, GOS-inulin mixture, and FOS
inulin mixture

Growth characteristics of Watson et al. Bifidobacteria and Lactobacilli are (2013) shown best results in GOS and lactulose in comparison to inulin, maltodextrin. GOS/Inulin, FOS/ Inulin mixtures

Endo et al. (2016)

(Continued)

116 Chapter 4 Table 4.6: (Continued) Prebiotic/Probiotic Type of RTD Tea Components

Brief Summary

References

Probiotic Components Black Tea

Lactobacilli and Bifidobacteria

Tea phenolics were reported as metabolic prebiotics and matrix for probiotic strains resulting in considerable effects on the intestinal environment by alteration of the intestinal bacterial population

Lacey et al. (2014)

Green Tea Kombucha

Saccharomyces cerevisiae, Gluconacetobacter sp.

The kombucha was found to stimulate the immune system, aid in digestion, protection against cancer and cardiovascular diseases, prevention of microbial infections; hypoglycaemic effect and antilipidemic properties, freeradical scavenging activities

Malbasa et al. (2011) Aloulou et al. (2012) Ilicic et al. (2012)

Mushroom Black Tea Kombucha

Yeast and acetic acid bacteria

The developed ganoderma hot water extracted kombucha showed antioxidant activity antibacterial activity against Staphylococcus epidermidis and Rhodococcus equi, and a minimum bactericidal concentration (0.16 mg/mL) against Bacillus spizizenii, B. cereus, and R. equi

Sknepnek et al. (2018)

Green Tea Premix Lactobacillus acidophilus

Spray drying of the prebiotic ice tea resulted in a premix which was sensorially and functionally acceptable after reconstitution

Tewari et al. (2018)

Black Tea Kombucha

The fermented beverage Marsh et al. contained Gluconoacetobacter (2014) (.85%) in greater concentration than Acetobacter (,2%) Among the bacteria the Lactobacillus population was up to 30% whereas the yeast population was dominated by Zygosaccharomyces at .95% in the black tea kombucha

Zygosaccharomyces, Gluconacetobacter, and Lactobacillus

Ready-to-Drink Tea 117 biochemistry of kombucha fermentation and polyphenol transformation were analyzed using green and black teas by Kallel et al. (2012). In the kombucha medium during the two-week fermentation, slight changes were observed in total phenolics and the main tea flavanols. At the end of the 2-week fermentation process, theaflavins moderately increased (more than 50%) and the thearubigins were found to be markedly decreased (more than 200%).

4.8 Manufacturing and Processing of RTD Tea Beverages The presence of polyphenols in RTD products depends on various factors. Astill et al. (2001) reported that the variety of tea leaves, growing environment, manufacturing conditions, and particle size of the tea leaves influence the tea leaf and final infusion compositions. The composition of the tea infusion is affected by the preparation method (including the amounts of tea and water used), infusion time, agitation time, and type of teabag (the size and material of construction of the bag) was shown to be significant determinanst of the component concentrations various polyphenols of tea beverages consumed.

4.9 Extraction of Black and Green Tea Extract Extraction is a separation process in which tea constituents are separated from the matrix. Water is used for the extraction of tea constituents. The method used for making the tea infusion is as important as the quality of the tea leaves. Superior quality tea infusions can be obtained by carefully optimizing the proportion of water and tea leaves for an appropriate time and temperature. Tea infusions must have a definite character and a delicate aroma. The quality of water used in the extraction process determines the efficiency of extraction, and hence, soft water is of paramount importance for this process. The initial step in the preparation of a tea infusion is heating the water to boiling point. Pale colored, harsh, flat, and brackish infusions are obtained if the water has been boiled for a more extended period before the addition of tea leaves. The tea concentrates of superior quality can be manufactured by using cell wall lysis enzymes such as carbohydrases, cellulose, tannase, and mascerase during the extraction process. The tea concentrate can also be stabilized by xanthan gum to prevent the sedimentation of tea solids (Lehmberg and Ma, 2000).

4.10 Taste Enhancement of RTD Tea Both unsweetened and sweetened variants of RTD teas are available. Usually, sucrose is used in the sweetened option. Health-conscious consumers prefer anticariogenic, low calorie, and low-glycemic index beverages. Sucrose can be replaced by natural or synthetic low-calorie sugar substitutes. Isomaltose, a naturally occurring reducing disaccharide

118 Chapter 4 ketose, is acariogenic as is degraded in the small bowel by glucosidases. It has a lower sweetening power compared to sucrose and, hence, it is used in combination with other high intensity sweeteners. Sugar addition to beverages contribute to the mouthfeel of the product and, therefore, artificially sweetened beverages can also be supplemented with edible gums such as guar, xanthan, locust bean, and cellulose gums.

4.11 Color Improvement of RTD Tea A color additive is a substance, dye, or pigment capable of imparting color to food. The color of a beverage plays a significant role in determining its consumer acceptance. It is essential to select the right color additive as a natural-looking beverage is considered to be of superior quality. Since the color additives are usually stable at a lower pH, acids such as erythorbic, ascorbic, and citric acid are also added to the beverage. The stability of 10
40 ppm colorant can be obtained by 300
1500 ppm erythorbic or ascorbic acid, or 0.5%
8.0% citric acid. The color of tea concentrate can be enhanced by a caramelized solution of a reducing sugar or mixture of reducing sugars. Sugars are heated with a food-compatible acid in the caramelization step followed by the addition of tea solids. The proteins and amino acids in tea solids react with sugars to give Malliard reaction products, which further intensify the brownish-red color of the tea concentrate (Tse, 1985).

4.12 Aroma Enhancement of RTD Tea The distinct aroma of a beverage is responsible for its reminiscence as well as identification. Tea aroma is unique because of its numerous volatile compounds. A tea’s aroma depends on the quality of the tea leaves and the extent of their fermentation. During the manufacturing of RTD tea, substantial amounts of these volatiles are lost during various processing stages, namely, concentration and drying of the extract. The extent of the loss of aroma depends on the processing conditions such as extraction temperature, extraction method, and percentage of the solids in the extract. The tea aroma can be recovered by condensing the exhaust gases released during the processing of tea leaves. The recovered aroma can later be added to the processed beverage just before packing. Alternatively, flavor-enhancing agents such as linalool and linalool oxide can be added to the final tea beverage. Cinnamic acid is used as an antimicrobial agent at a concentration of 50
600 ppm in RTD tea and contributes a pleasant flavor resulting in an organoleptically acceptable and microbiologically safe beverage. The natural tea’s aroma, obtained by condensing the volatiles released during the manufacturing of the tea, comprises mainly of terpene alcohols such as linalool, nerol, and geraniol. This recovered tea aroma is added back to the tea before packing. The terpene

Ready-to-Drink Tea 119 alcohols degrade under acidic conditions and release off-flavors. Hence the loss of aroma or flavor is observed in RTD tea beverages manufactured by this conventional method. Although the natural aroma of tea can be conserved by the addition of preservatives in RTD tea beverages, consumers prefer beverages with fewer additives. The tea aroma can be conserved by pasteurizing the acidic and nonacidic components of tea separately. The components are then cooled and filled into the container (can or bottle) simultaneously or sequentially (Narayanan and Sinkar, 2009). The RTD tea beverages develop off-flavors and precipitates over a period. These malodorous compounds are formed due to the reaction of certain tea components with acids. The sugars react with acids to form furfurals, whereas limonene from lemons added to the tea is degraded to form terpenes.

4.13 Clarity of RTD Tea The consumers’ perception of the product quality significantly depends on its appearance. The RTD tea beverages are anticipated to be clear and free of precipitates. The majority of RTD tea beverages do not contain milk, but a few variants with milk are available in the market. The RTD tea with milk faces stability problems. The product appeal is affected by sedimentation and creaming of the milk in the tea. Additives such as cellulose microfibrils are used to stabilize the milk component of the beverage. The solubilizers are incorporated during the manufacturing of the RTD tea to improve the cold-water solubility of tea solids and to prevent the formation of cream and other precipitates. Invert sugar, maltodextrin, and glycerol are preferred as solubilizers and their concentration in the beverage depends on the quantity of tea solids. The addition of a milk solution to an acidified tea extract results in denaturation and precipitation of milk proteins. Addition of a pH buffer reduces or eliminates precipitation of milk protein when the milk solids are mixed with acidic tea components. The pH buffer selected to give a stable milk-tea beverage is a lactate salt such as potassium lactate and carbonate salt such as sodium bicarbonate, sodium carbonate, potassium bicarbonate, or potassium carbonate (Rosevear, 2011).

4.14 Mouthfeel of RTD Tea The RTD tea with enhanced mouthfeel, creaminess, and thickness at a lower dosage of solids is desirable whereas the attributes such as ‘sliminess’ or ‘stringiness’ is undesirable. Mouthfeel is a sensory perception and is different from texture, which is a physical property. Hence increasing the viscosity/thickness of a beverage by addition of hydrocolloids gums does not guarantee improved mouthfeel. The excessive use of hydrocolloids in hot beverages also contributes to negative textural effects such as sliminess, stringiness, or gel formation upon cooling. The addition of water-soluble starches

120 Chapter 4 also increases the viscosity of the RTD tea with a limited effect on the mouthfeel. However, the amount of water-soluble starch that delivers these attributes is usually so high that a number of spoonfuls of the product are required to make the beverage. Hence the balanced use of additives while processing is essential for the RTD tea to be acceptable (Villagran et al., 2001).

4.15 Prevention of Creaming of RTD Tea The phenomenon resulting in the cloudy and hazy appearance of RTD beverages is called ‘creaming’ or ‘creaming down reaction’ (Ishizu et al., 2014). The formation of tea cream in RTD tea beverages adversely affects its consumer acceptability. Tea cream is a brown-white turbidity and the precipitation observed when a hot tea infusion cools down. Tea cream is also observed in refrigerated RTD tea. Tea cream formation affects the physical, organoleptic, and biological activities of the beverage (Kim and Talcott, 2012). The tea cream consists of around 30% tea solids. The main constituents of black tea cream are thearubigins, theaflavins, and caffeine. Theflavins and thearubigins are formed from the condensation of polyphenols during fermentation of tea and, hence, tea cream formation has been widely reported in black and oolong tea. Poorly soluble complexes are a result of interaction between hydroxyl groups of polyphenols, peptide groups of proteins, and the keto-amide group of caffeine. The variation observed in the formation of tea cream varies as it depends particularly strongly on the tea solid concentration and presence of low solubility polyphenols and theaflavins resulting in phase separation into two immiscible phases. The semifermented tea cream consists predominantly of catechins (30%), caffeine (20%), and protein (16%). Major catechins that precipitate are EGCG (19%) and ECG (5%) (Yin et al., 2009). Caffeine forms a 1:1 complex and a 2:4 complex with nongallated and gallated catechins, respectively (Ishizu et al., 2014). The size of green tea cream particles is roughly one order of magnitude larger than those of black tea (Lin et al., 2015). Decaffeinated tea is also capable of forming creams indicating that caffeine is involved, but is not critical for the reaction. The calcium in tea infusion also accelerates the creaming process (Jo¨bstl et al., 2005). Physical filtration techniques such as the use of membranes of different molecular weight cut-offs and materials (fluoropolymer, polysulfone, and regenerated cellulose) can remove the haze from RTD tea beverages (Evans et al., 2008). The disadvantage of the filtration methods is that they lower the concentration of bioactive and organoleptic components. Chemical methods such as the use of tannase to hydrolyze gallated polyphenolics involved in cream formation results in loss of astringency and overall quality of RTD tea. The use of enzymes has further limitations such as noncontinuous operating conditions (i.e., batch processing) and difficulty in the recovery of enzymes. Although tea-cream formation

Ready-to-Drink Tea 121 decreases under low pH, the addition of food-compatible acids such as citric acid affects the flavor profile of the RTD tea (Argyle and Bird, 2015). Addition of metal ions in the green tea contributes greater turbidity in comparison to phenolics and caffeine (tea-creaming activators). Chelating agents such as ethylenediaminetetraacetic acid (EDTA), polyphosphates, and potassium citrates bind cream-promoting divalent cations. The tea extract is further processed to remove these molecules by using ion exchange chromatography, reverse osmosis, or filtration techniques. Food grade cation exchange resin such as sulfonated copolymers of styrene and divinylbenzene, sulfite-modified cross-linked phenol-formaldehyde resins, sulfonated tetrapolymers of styrene, divinylbenzene, acrylonitrile, and methyl acrylate effectively remove metal cations present in the extract (Ekanayake et al., 1999; Gosselin and Gonley, 2006). Additives such as honey and lemon are frequently used to improve the sensorial appeal of the product. The presence of both honey and lemon changes the flavonoid content and acidity of the tea infusion, respectively, resulting in the formation of cream. The reduction in the creaming of honey-lemon tea can be carried out by pretreatment of the honey to remove the polyphenols and interacting minerals (Hategekimana et al., 2011).

4.16 Shelf Stability of RTD Tea The shelf-stable and natural tea concentrates are highly desirable as a raw material for the manufacture of RTD tea beverages. The water activity of tea concentrate containing 55% solids at 24 C is from about 0.75 to about 0.85. Tea concentrates are preferred over tea powder as it consumes less power during manufacturing due to the requirement of fewer processing steps. Tea solids can be more easily transported in a concentrated form than as a diluted extract. The shelf-stable RTD tea beverages can be prepared by acidification, heating, and clarification (removing the volatiles and the precipitates formed) of the tea extract followed by blending it with sweeteners and flavors. The tea product manufactured by this method is shelf-stable and does not require any preservatives (Hing, 1985). Preservatives help in extending the shelf-life of food by retarding microbial growth and preventing changes in product color, flavor, and texture. The RTD beverages packaged in glass and plastic are more susceptible to spoilage by yeast and molds than canned beverages. The growth of pathogenic bacteria along with spoilage organisms has been reported in beverages when the native pH of beverages is between 2.5
6.5 in the absence of preservatives. Natamycin is used to prevent the growth of yeast and molds. Natamycin is stable in the dry state and can be added to dry diluents. It is also sensitive to ultraviolet light, oxygen, and extreme pH and, hence, is used in combination with sorbates, benzoates, and parabens. This combination has been proven to improve the stability as well as efficacy of natamycin in beverages packaged in glass and polyethylene terapthalate (PET) bottles. Cinnamic acid along with acidulants

122 Chapter 4 such as citric, maleic, phosphoric, and tartaric acid help in improving the shelf-stability by maintaining the beverage below pH 4.5.

4.17 Packaging of RTD Tea Packaging remains a critical aspect of any food product. It requires precise technological interventions as packaging controls the shelf life of a product to a large extent. Aromatic commodities like tea are more prone to deterioration and storage loss. Hence the use of proper packaging materials remains very much relevant for RTD tea products as well. The packaging requirements for RTD teas are: • • • • • •

Leak-proof and contamination prevention Protection of the contents against chemical deterioration Elimination of external flavors Hygienic and safe Economical, easy to use and dispose Good aesthetic appearance

Depending on the RTD tea formula, the packaging pattern varies. However, before using packaging material for RTD teas, general consideration for packaging materials should be considered like the nonreactivity of the material as well as the water
vapor transmission rate. The most used packaging material is paperboard carton with a liner or an overwrap of poly(propylene) or regenerated cellulosic film. Other materials are plastic jars, bottles, pouches, strips, and envelopes. Plastic pouches have captured 12% of the tea market. Different RTD companies have launched innovative packaging systems like single-use plastic cups with lids and drinking apertures. Apart from these, retort pouches are beneficial specially for iced teas as they are found to provide both protection from ultraviolet rays and oxidative degradation. Glass bottles are also used for packaging of iced teas as the richness of colored RTD ice teas makes the product more attractive to the consumer. Recently a new, two-side coated, biodegradable cellulosic-based film has been developed which is sealable with heat and offers an intermediate moisture barrier for tea products as they are prone to loss of aroma due to improper packaging (www.greenerpackage.com). This package is capable of reducing waste as composting of this package can be done at home, with the degradation period being a few weeks. Conveniently, the biodegradable primary package can be combined with a paper box that also offers a wide range of recycling options for consumers. Aseptic packaging is also a common packaging method for RTD tea. Products are packed in cartons which are hermetically sealed and have a shelf life of 6 months at ambient temperature. The standard carton is made up of six layers: polyethylene (moisture barrier), paperboard (strength), polyethylene again, aluminum (light, air, and odor barrier), a third polyethylene layer, and a fourth polyethylene layer.

Ready-to-Drink Tea 123 Printing is applied to the paper layer, and then all layers are laminated and flame threated together one after another to create the cardboard mixture. The most common plastic for thermoforming packaging designs is made up of PET. This is because of the high-strength barrier that can resist outside tampering and other elements. PET bottles are cost effective and easy for transport because of their low weight and before filling, and they are not blown into their full shape. Therefore they do not require excessive space for storage.

4.18 Sensory Evaluation of RTD Tea Beverages Sensory evaluation is a scientific discipline which measures and statistically analyses the sensory responses of food commodities as perceived by the senses of sight, smell, taste, touch, and hearing. Sensory evaluation entails the understanding of the acceptability of a product based on appearance, color, aroma, taste, mouthfeel, and visual texture of the food or drink. The sensory analysis of a product helps in determining its quality, market potential, batch-to-batch variation if any, and pricing. It also reduces the chances of product failure. A range of tests such as the descriptive, discrimination, and affective tests can be carried out to evaluate the product. The descriptive test helps in determining the sensory profile of the product, whereas the discrimination test is used to evaluate the similarity or differences between the products. The affective tests can determine the preference or liking of the product. The sensory laboratory must be equipped with individual tasting booths, controlled ventilation, appropriate lighting, and a water filtration system. Tea tasting is carried out by a highly trained sensory panel comprised of individuals with exceptional sensory sensitivity. A semitrained or untrained sensory panel can also be used depending on the requirement of the technique. The linear partial least square-artificial neural networks hybrid model can be used to predict the compositions of RTD tea beverages which would potentially be liked by the consumers, based on its coefficient of determination and root-mean-square error. Such hybrid models can be prepared by sensory evaluation of some green tea model systems containing tea flavors specific for the green tea aroma and taste. Sensory evaluation yields hedonic liking scores which can be further analyzed by regression models such as linear partial least squares to describe the effects of the important flavor keys on consumer liking (Yu et al., 2018). The sensory quality and health benefits of tea are associated with its chemical composition. It is, thus, important to know these chemical markers for assessment of the quality of the manufactured RTD tea. Gas chromatography/ Gas chromatography -mass spectrometry (GC/GC
MS) has been used to determine the chemical markers of black tea volatiles. A group of 123 components, comprising of key odorants, technological, and botanical tracers from black tea have been mapped. The pattern recognition tools can recognize the 2D fingerprints of such volatiles and, thus, help in quality assessment (Magagna et al., 2017).

124 Chapter 4

4.19 Health Benefits of RTD Tea Since primordial times, green tea has been considered in traditional Chinese medicine as a healthy beverage. Tea as a drink is enriched with several polyphenols that have health healing properties like antiosteoporotic, antioxidant, antiatherosclerotic, antiallergic, antifibrotic, hypolipidemic, hypocholesterolemia, antiobesity, antiviral, antimutagenic, antimicrobial, anticarcinogenic, antidiabetic, and neuroprotective effects (Nash and Ward, 2017; Lorenzo and Munekata, 2016; Williamson, 2017). Green tea leaves contain three main components which affect human health: i. polyphenolic compounds; ii. xanthic bases (caffeine and theophylline); iii. essential oils. The major components of tea polyphenols that are available in green tea leaves include catechins. These catechin compounds are present in different forms in tea and, depending on their structural modification, several subcomponents or derivatives of the catechin are also abundant. These catechins are majorly responsible for the series of oxidations and condensations which occur during the production of black tea. Catechins have been widely used as food antioxidants. They can retard rancidity in fats and oils by quenching free-radical peroxide activity brought about by aerobic oxidation. Tea leaf catechins show a similar inhibitory effect on aerobic oxidation of linoleic acid as shown by butylated hydroxyl anisole. The catechin concentration of tea leaves also changes with its aging. On a comparative basis, the green tea polyphenol fractions show superior scavenging effects on some active oxygen radicals than ascorbic acid (vitamin C) and tocopherol (vitamin E). EC possesses strong antioxidant activity and also exhibits anticancer properties by reportedly promoting apoptosis (Okabe at al., 1999), arresting metastasis by inhibiting metalloproteinases (Demeule et al., 2000), impairing angiogenesis (Jung et al., 2001), and reversing multidrug resistance (Jodoin et al., 2002). The next important and abundant catechin among green tea polyphenols is the EGCG. Though present abundantly in green tea, this component is absent in black tea and scant in oolong tea. The beneficial impacts of EGCG lies in its potential antioxidant effect, chemoprevention, resisting cardiovascular diseases, efficiency in weight loss, and protection of skin from harmful UV radiation among others. This component is also known to control different disease-specific molecular targets that are affected by EGCG concentration. The required concentration necessary for such molecular targets is much higher and cannot, however, be fully achieved by consumption of green tea directly or dietary supplements containing green tea extracts (Nagle et al., 2006). It is this component which cumulatively provides the health benefits of drinking green tea. EGCG consists of about 50% of the catechin content of green tea. Some other catechins present in green tea at lower concentrations include ECG and EGC. EGC and ECG have a comparable antioxidant activity. ECG and EGC are also

Ready-to-Drink Tea 125 known to possess antiradical activity against alkyl peroxyl radical (Grzesik et al., 2018). Caffeine acts on the central nervous system resulting in stimulation of wakefulness and decreasing the sensation of fatigue (Varnam and Sutherland, 1994). Theophylline induces psychoactive activity, has a slightly inotrope and vasodilator effect, diuretic effect, and nonspecific relaxation on the bronchial smooth muscle. The content of essential oils is higher in green tea and is known to facilitate digestion. However, the most interesting is the group of polyphenols which have strong antioxidant and biological properties. The aqueous extract of tea possesses antimutagenic, antidiabetic, antibacterial, antiinflammatory, and hypocholesterolemic properties (Pan et al., 2003; Feng et al., 2001) and protection against dental caries, periodontal disease, and tooth loss. In case of black tea, theaflavins and thearubigins have antioxidant activities and also act as antioxidants in vitro by sequestering metal ions and by scavenging reactive oxygen and nitrogen species (Gardner et al., 2007). The polyphenol quality as well as quantity changes with the stage of processing of the tea. Green tea is enriched with major polyphenols which may be degraded or altered during the processing steps of fermentation, curing, and drying to develop black and oolong tea. Table 4.7 lists the health benefits of the different tea components.

4.20 Safety of RTD Tea During Processing and Consumption Tea processing requires certain rules and regulations to be abided to maintain the safety and quality of the product. Regulatory authorities across the globe have set regulations for food safety concerning the hygiene of foodstuffs that are important and obvious for food business operators to safeguard at all stages of production, processing, and distribution of food which are under their control and satisfy the relevant hygiene requirements laid down in the HACCP guidelines and regulation. The potential hazards in case of tea processing include physical and chemical contamination, foreign particulates, and microbiological contamination. Chemical contaminants pose a danger of acute level as they have a multivariate source of occurrence. Chemical contamination can originate from environmental pollution, absurd use of agrochemicals, adulteration, sabotage, lubricants used in tea processing machinery, or fumigant residues originating from the fumigation of containers and contamination during transport or storage. Apart from these, chemical contamination is generated from inappropriate handling behavior, for example, smoking when handling harvested tea leafs and tea (packaged or unpackaged). Pesticides in tea processing can also pose a problem in the further steps for product development. Hence the maximum residue level for pesticides is a major safety step for the quality maintenance of products. But most of the time the levels are under control and as a result, the food safety risk from agrochemicals are considered to be low. Some hazards are generated due to chemical components generated from the processing of tea like brewing where polycyclic aromatic hydrocarbon (PAH) is generated which are regarded unsafe for consumption, but mostly these components are below measurable analytical level. These components are

126 Chapter 4 Table 4.7: Health benefits of different tea components. Type of Tea Properties

Highlights

References

Catechin (C) Green Tea

Antimicrobial properties

Black Tea

Antioxidant property

G

Oolong Tea

Antioxidant activity

G

G

The major bioactive components of green tea, the catechin was found to possess antimicrobial activity helpful in treatment of topical and oral infections as well as maintaining gastrointestinal flora Black tea exhibited potent antioxidant properties by its ability to scavenge free radicals, inhibit lipid peroxidation, and chelate metal ions due to presence of catechin

Oolong tea possesses an antioxidative activity and a high lipoxygenase inhibitory activity, as compared to black tea

Taylor et al. (2005) Xu et al. (2017), Song et al. (2005) Oh et al. (2013) Sharma and Goyal (2015) Grzesik et al. (2018) Tiwari et al. (2005) Chan et al. (2011)

Epicatechin (EC) Green Tea

Antioxidant activity

G

Black Tea

Anticancer activity

G

Oolong Tea

Antioxidant activity

G

(
)-Epicatechin (EC) was found to have strong antioxidant and antiangiogenic activity as well as their inhibitory impact on carcinogenic cell proliferation and modulatory nature of carcinogenic cell metabolism Epicatechins present in have shown apparent activity against human cancer, reportedly helping in cell apoptosis, arrest metastasis by inhibiting metallo-proteinases, impair angiogenesis, and reverse multidrug resistance Tea polyphenols are potent antioxidant agents and their activity involves removal of superoxide, peroxyl, and hydroxyl radicals. Various pharmacological activities such as antioxidant activity by reducing oxidative stress of Oolong tea was reported

Yang et al. (2001) Henning et al. (2003) Filomeni et al. (2015) Strzelczyk and Wiczkowski (2012)

Green tea polyphenols as direct antioxidants by scavenging reactive oxygen species or chelating transition metals as has been demonstrated in vitro. Green tea was found to contain 12% of ECG Black tea extract and oolong tea have a preventive effect against hepato-carcinogenesis due to the presence of catechins like epicatechin gallate (ECG)

Gramza et al. (2005) Forester and Lambert (2011)

Josic et al. (2010)

Epicatechin gallate (ECG) Green Tea

Antioxidant property

G

Black Tea

Inhibitory effect

G

Kawai et al. (2003)

(Continued)

Ready-to-Drink Tea 127 Table 4.7: (Continued) Type of Tea Properties Oolong tea

Antioxidant property

Highlights G

References

ECG present in oolong tea was reported as freeradical scavengers which in return were reported to be effective in protection against cancer and cardiovascular and metabolic diseases

Nakanishi et al. (2010)

The most effective antioxidant in green tea is EGCG. Among the most investigated antiproliferative effects green tea polyphenols, EGCG showed the most potent antiproliferative effects when tested in animal cell lines Black tea showcases the properties of free radical scavenging activities due to the presence of the three adjacent hydroxyl groups on the B-ring of EGCG which helps to inhibit lipid peroxidation and chelate metal ions Oolong tea extracts work wonder by reducing the mutagenic effects of carcinogens such as heterocyclic amines. In Salmonella reverse mutation assay (Ames test), the greater antimutagenic effect was found in oolong tea than in green tea and black tea and some antimutagenic substances

Forester and Lambert (2011)

The chemo-preventive effect of EGC (2) Epigallocatechin, a polyphenolic compound having great potential to protect DNA from damage by superoxide mutase and peroxide radicals are found abundantly in green tea, and they inhibit protein kinase C (PKC), a major inducer of carcinogenicity EGC protect low density lipoproteins LDL fraction against oxidation by activating the synthesis of the prostaglandins and possess antiplatelet and metal chelating proprieties EGC present in Oolong induces chemo-protective activity by preventing the proliferation of superoxide dismustase ions

Stammler and Volm (1997)

Catechins are present from 15% to 20% by weight in green tea. Green tea catechins have a hypocholesterolemic effect and suppress the intestinal absorption of cholesterol

Ikeda et al. (1992)

Epigallocatechin gallate (EGCG) Green Tea

Antiproliferative effects

Black tea

Antioxidant activity

G

Oolong tea

Anticancer activity

G

G

Nihal et al. (2005) Noda et al. (2007) Ji et al. (1996) Chen and Liu (2000) Carriere et al. (2001)

Epigallocatechin (EGC) Green Tea

Chemo-preventive effect

Black Tea

Antioxidant activity

Oolong Tea

Chemo-protective activity

G

G

G

Gramza et al. (2005)

Miura et al. (1997)

Caffeine Green Tea

Hypocholesterolemic effect

G

(Continued)

128 Chapter 4 Table 4.7: (Continued) Type of Tea Properties Black Tea

Anticarcinogenic effect

Inhibition of lung tumorigenesis

Oolong Tea

Antiobesity

Highlights G

G

G

Caffeine might contribute to the anticarcinogenic effect of tea, as shown in several animal models. Studies in animal cell line culture have revealed that tea flavanols have antiproliferative, antiangiogenic, and anticarcinogenic activities Investigators demonstrated the inhibition of lung tumorigenesis by black tea and caffeine in F344 rats during a lifetime 2-year bioassay. The results show that 2% black tea significantly reduced the incidence of lung cancer and liver cancer Caffeine decreased food intake and increased thermogenesis and resulting in body weight reduction. Thermogenesis by caffeine was found to synergistically enhance with catechins in rat adipose tissues

References Yang et al. (2001); Lambert et al. (2003) Chung et al. (1998)

Rumpler et al. (2001)

insoluble in water, hence RTDs prepared from brewed tea infusions have lower residual levels of PAH. However, no naturally occurring constituents of tea are identified as a safety risk requiring control measures. Foreign extraneous particles may be considered as elements which are naturally associated with tea, for example, parts of other plants growing nearby or extraneous material introduced during the process, such as metallic parts, stones, scale, glass, insects, fragments, jewelry, packaging materials, and others. Lastly, microbiological hazards are easier to control. Tea contains natural plant associated microorganisms, but as dried tea leaves have lower moisture content and water activity, these do not pose any hazard if the tea is stored in dry conditions. According to the European Union’s Scientific Committee on Food, moisture levels up to 10% appear to give an acceptable safety margin for the storage of tea. Adulteration can be controlled by a trained panelist for tea by testing various parameeters of the leaves before and after infusion and the appearance, odor and taste of the liquor, rather than by reference to its chemical composition. For green tea infusion, the brewing technique affects the EGCG content. The maximum consumption of green tea infusions should be such that it does not exceed the EGCG intake beyond 734 mg per person per day. Green tea extract
based beverages are considered to be safe when the EGCG concentration delivered by it is identical to those delivered by traditional green tea infusions. The humans can tolerate EGCG at a maximum concentration of 338 mg from the dried tea extract (Dekant et al., 2017; Hu et al., 2018). Excessive fluoride intake results in fluorosis of the teeth and skeleton. The fluoride content of green tea infusions is greater when mature leaves are used in the manufacture of tea. An increase in the fluoride bioavailability has been observed on the consumption of tea during fasting which may have a deleterious effect on health (Chan et al., 2013).

Ready-to-Drink Tea 129

4.21 Bioavailability of RTD Tea Constituents The term bioavailability is defined as the fraction of an ingested nutrient that reaches the systemic circulation and the specific sites where it can exert its biological action in animal models (D’Archivio et al., 2010). In the human body, green tea flavan-3-ols undergo complex catabolism resulting in several metabolites which are difficult to identify and quantify in urine and blood. The gut microbiota also tranforms (1)-catechin to (1)-EC resulting in further variations in pharmacokinetic data. The manufacture of RTD tea involves canning and bottling at high temperature, which may also result in epimerization of green tea polyphenols. Earlier analytical methods and synthesized pure standards to quantify flavan-3-ols and its metabolites were not available. However, newer sophisticated techniques such as high-performance liquid chromatography with tandem mass spectrometry (HPLC
MS/MS) can now be used to investigate the catabolism, pharmacokinetics and urinary excretion of flavan-3-ols. This technique can also detect the unknown catabolites of green tea occurring from their interaction with the gastrointestinal tract and its host microflora. The analysis of human biological fluids had revealed the presence of 39 tea catabolites revealing the presence of highest content of EGCG (unmetabolized form) in comparison with ECG and EC conjugates. The calculated bioavailability of catechins was 39% considering the variations in the urinary excretion of colonic metabolites among the subjects (Del Rio et al., 2010). Studies have indicated a large variation among the subjects in the absorption of green tea catechins through the intestine. Green tea catechins have greater bioavailability from supplements compared to brewed tea (Bansal et al., 2012). Catechins cannot be completely extracted from the fresh tea leaves and, hence, their concentration differs from the absolute values determined through complete extraction of leaves. Catechins are unstable and their concentration in the extract may change considerably. Thus a comparison of catechin content of the initial dose administered to the model animals during in vivo experiments is very difficult (Chacko et al., 2010). Studies in Sprague Dawley rats have shown the absorption of EGC and EGCG from green tea to be significantly improved in the presence of both sucrose and ascorbic acid as compared to the green tea control (Peters et al., 2010). The digestive stability and intestinal uptake of catechins in RTD green tea in the presence of xylitol and citric/ascorbic acid were studied in an in vitro digestion model coupled with Caco-2 cells. Total catechins, EGC, and EGCG have shown a poor digestive recovery from green tea without additives. However, the presence of citric acid or vitamin C increased their concentration in gastrointestinal fluids and Caco-2 human intestinal cell significantly. The presence of xylitol along with citric/ascorbic acid in green tea reportedly improves the recovery of total catechins by 1.7
2.5 times and 3 times, respectively (Shim et al., 2012). The absorption of catechins is significantly affected by the presence of food. Black tea is popularly consumed with milk. The addition of semiskimmed milk (3 g solids) to black tea

130 Chapter 4 (100 mL in 600 mL) does not hamper the bioavailability of tea catechins (Van het Hof et al., 1998). The combination of quercetin and green tea can enhance the chemo-preventive properties of green tea which are affected by excessive methylation occurring in vivo. Quercetin, a natural inhibitor of catechol-O-methyltransferase and multidrug resistance proteins, decreases the methylation from 63% to 19% in lung cancer A549 cells, and 97% to 56% in kidney 786-O cells. Quercetin also increases the absorption of EGCG 4-fold in lung cancer A549 cells and 2-fold in kidney 786-O cells (Wang et al., 2012). The manufacturing processes do not have a significant effect on the antioxidant activity and bioavailability of green tea polyphenols (Xu et al., 2004).

4.22 Ready-to-Drink Tea Market The whole world including India has seen an upsurge of the ready-to-drink tea market, which depends on the raw material (black, green, white, herbal, and oolong teas and other drinks), method of packaging (loose packets, plastic container, tin cans, and dip tea bags), mode of application (household and commercial), as well as distribution channels (convenience store, supermarket/hypermarket, specialty centres, online retail sales). Methods of differentiation for analysis of RTD marketability data has been beneficial to judge the growth scenario of RTD market. The RTD tea market statistics deal with different aspects including technology, supplies, capacity, production, profit, price, and competition. RTD tea can be categorized as a subgroup of soft drinks, but they differ in their function. Though is ambiguity regarding the exact figures for the market value of RTD, certain market news analysis agencies like Zion Market Research reports have cumulatively stated that in 2017 the tea maket globally reached nearly US$50 million markets with an upcoming expectation to increase by 2024 having a compound annual growth rate (CAGR) of around 4.5% (http://www.digitaljournal.com). The worldwide market for RTD green tea is expected to grow at a CAGR of roughly 62% over the next 5 years, according to a new study. The front runners in the RTD industry include The Coca-Cola Company, PepsiCo Inc., Pokka Corporation, Nestle´ S.A., Lucozade Ribena Suntory, Arizona Beverage Company, Danone SA, Monster Beverage Corporation, Starbucks Corporation, and Unilever. RTD green tea is becoming increasingly popular among European consumers and sales are expected to rise. However, there are drawbacks for the RTD green tea industry to penetrate the soft drink market as there are with a high market share for other beverages which leads to intense competition dominated by well-established brand names (www.alliedmarketresearch.com). The Asia-Pacific market is recognized as a potential market for RTD tea, citing fastgrowing economies and enormous urbanizationin the region. In 2017, Tata Global Beverages, the world’s second-largest tea company, launched its first tea cafe´ “Tata

Ready-to-Drink Tea 131 Cha” in Bengaluru, India. The wide flavor range in the cold RTD section include cucumber green tea, sugar-free tangy tamarind, dilliwali kanji, masala shikanji, meetha paan and rasmalai milk shake, peach iced tea, and chili guava ice slush. Some of the important key players profiled in the global herbal tea market are Associated British Foods Plc. (United Kingdom), Dilmah Ceylon Tea Company Plc. (Sri Lanka), ITO EN (North America) Inc. (United States), Tata Global Beverages Ltd. (India), The Unilever Group (United Kingdom), Barry’s Tea Ltd. (Ireland), R.C. Bigelow, Inc. (Unites States), Celestial Seasonings, Inc. (United States), Harney & Sons Tea Corp. (United States), and Mighty Leaf Tea Company (United States). In the upcoming era, importance of RTD is growing to increase at fast rate globally, which is an encouraging sign to foster self-nutrition and preventive healthcare behavior.

4.23 Factors Affecting RTD Tea Manufacturing 4.23.1 Product Innovation Tea is a popular beverage in Asia but in order to increase its popularity in Europe, the flavour profile of tea needs a substantial development. Manufacturers must discover new tea varieties and infusions. Consumers also appreciate total transparency concerning the source of tea leaves. RTD tea in exotic flavors must be invented. Sugary drinks are not likely to be accepted because people are becoming increasingly health conscious. Hence, RTD tea containing stevia or a low-calorie sweetener would be well received by the consumers. RTD tea beverages that are slightly sweetened, but provide health benefits such as higher antioxidants, polyphenols, and prebiotic content are likely to be favored by health-conscious consumers. An extensive sensory evaluation of the prepared recipes must be carried out by a trained sensory panel before launching the product.

4.23.2 Raw Material Sourcing The quality of RTD tea reflects the nature of the raw materials used for its production. Premium quality RTD tea beverages can only be manufactured when the manufacturer has a thorough knowledge of the raw materials regarding their chemical composition. The raw materials required for RTD tea manufacture must have certain characteristics, including: • • • •

consistent quality cost effective readily available throughout the production period safe and legal to use

132 Chapter 4

4.23.3 Process Development The manufacturer must be familiar with the optimization processes, bottling facilities, and distribution and supply chains. The tea manufacturers must periodically invest in the latest production machinery for greater output. The optimized RTD tea manufacturing process must be meticulously implemented to get a consistent quality product with minimum batchto-batch variation and the desired shelf life. The RTD tea beverages can be manufactured from freshly brewed tea leaves, procured tea concentrates, or powdered tea. The type of raw material used depends on the product and process specifications, and the production facilities.

4.23.4 Testing of Quality Parameters The product variation can be controlled if the chemical composition of the product, as well as the raw material, is identified. Theaflavins, thearubigins, highly polymerized substances, total liquor color, and total soluble solids are the major quality parameters tested in black tea, whereas that for green tea include EGCG content. The caffeine content of tea is another important factor that must be quantified. Analytical instruments such as high performance liquid chromatography (HPLC), gas-chromatography (GC), alcohol analyzers, refractometers, spectrophotometers, colorimeters, and moisture analyzers are routinely used for this purpose. Analytical instruments must be purchased from a reliable supplier. The instruments must be routinely calibrated for dependable analytical results.

4.23.5 Packaging RTD tea beverages are packaged in PET bottles, glass, or cans. RTD beverages in PET bottles are more common because of the ease of conveyance. Recently glass bottles have become popular as consumers are increasingly environment conscious. The packaging of RTDs play an important role in attracting the consumers and hence, the brands such as Teavana have started packaging their iced teas in sleek glass bottles to stand out. The packaging of RTD tea is crucial for advertising as well as communicating with the consumers. Colors of the package must be chosen while taking into consideration the target demographic.

4.23.6 Marketing The brands are built by marketing the products. The marketing not only helps in selling the products, but also forms a relation with the audience. The product marketing includes advertising, promotion, sales, and public relations. There are many big players in the

Ready-to-Drink Tea 133 RTD tea industry market and, hence, along with innovation, marketing the product becomes equally challenging. The manufacturers must promote their product on dedicated websites and other retail platforms for maximum visibility. The unique characteristics of the beverage should be emphasized during the promotion for the greater impression.

4.24 Conclusion Ready-to-drink tea is one of the most popular beverages worldwide, and its consumption has been claimed to be associated with beneficial health effects such as anticarcinogenicity, anti-mutagenicity, and cardioprotective effects. RTD tea is a ready prepared tea, mostly black or green, and generally consumed as hot or cold depending on a consumer’s preference. It is a healthy alternative to alcoholic drink and other soft drinks available in the market. Market development of RTD from their country of origin to other parts of the world has also led to novel technological advancements, not only to optimize their production, but also to satisfy consumers, particularly regarding health benefits, convenience, flavor, and taste. Market growth is expected to rise progressively over the next few years and new RTD tea products will give marketing shelves around the world a new makeover, increased interest, curiosity, and a wide variety of nonalcoholic beverage options with unique flavors, eco-friendly packaging, and nutritional benefits.

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138 Chapter 4 Tanaka, K., Miyak, Y., Fukushima, W., Sasaki, S., Kiyohara, C., Tsuboi, Y., et al., 2011. Intake of Japanese and Chinese teas reduces risk of Parkinson’s disease. Parkinsonism Relat. Disord. 17, 446
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Ready-to-Drink Tea 139

Further Reading Bindes, M.M.M., Cardoso, V.L., Reis, M.H.M., Boffito, D.C., 2019. Maximisation of the polyphenols extraction yield from green tea leaves and sequential clarification. J. Food Eng. 241, 97
104. Chen, S.Q., Wang, Z.S., Ma, Y.X., Zhang, W., Lu, J.L., Liang, Y.R., et al., 2018. Neuroprotective effects and mechanisms of tea bioactive components in neurodegenerative diseases. Molecules 23, 5
12. Dekant, W., Fujii, K., Shibata, E., Morita, O., Shimotoyodome, A., 2017. Safety assessment of green tea based beverages and dried green tea extracts as nutritional supplements. Toxicol. Lett. 277, 104
108. Hara, Y., 1994. Prophylactic functions of tea polyphenols, American Chemical Society Symposium Series (USA), vol. 2. American Chemical Society, Washington, pp. 34
50. Hara, Y., Yang, C.S., Isemura, M., Tomita, I. (Eds.), 2017. Health Benefits of Green Tea: An Evidence-Based Approach. CABI, Wallingford. Harbowy, M.E., Balentine, D.A., Davies, A.P., Cai, Y., 1997. Tea chemistry. Crit. Rev. Plant Sci. 16 (5), 415
480. Lambert, J.D., Elias, R.,J., 2010. The antioxidant and pro-oxidant activities of green tea polyphenols: a role in cancer prevention. Arch. Biochem. Biophys. 501, 65
72. Manach, C., Scalbert, A., Morand, C., Remesy, C., Jimenez, L., 2004. Polyphenols: food sources and bioavailability. Am. J. Clin. Nutr. 79, 727
747. Matsumoto, Natsuki, Kohri, Toshiyuki, Okushio, kazuo, Yukihiko, Hara, 1996. Inhibitory effects of tea catechin, black tea extract and oolong tea extract on hepato-carcinogenesis in rats. Jpn. J. Cancer Res. 87, 1034
1038. Sakanaka, S., Jumneja, L.R., Taniguchi, M., 2000. Antimicrobial effects of green tea polyphenols on thermophilic sore forming bacteria. J. Biosci. Bioeng. 90 (1), 81
85. Sano, H., Kawahito, Y., Wilder, R., Hashiramoto, A., Mukai, S., Asai, K., et al., 1995. Expression of cyclooxygenase-1 and -2 in human colorectal cancer. Cancer Res. 55 (37), 85
89. Xu, Y., Ho, C.T., Amin, S.G., Han, C., Chung, F.L., 1992. Inhibition of tobacco-specific nitrosamine-induced lung tumorigenesis in A/J mice by green tea and its major polyphenol as antioxidants. Cancer Res. 52 (38), 75
79. Zhang, H., Zhang, Y.W., Chen, Y., Huang, X., Zhou, F., Wang, W., et al., 2012. Appoptosin is a novel proapoptotic protein and mediates cell death in neurodegeneration. J. Neurosci. 32, 15565
15576. Zuo, Y., Chen, H., Deng, Y., 2002. Simultaneous determination of catechins, caffeine and gallic acids in green, Oolong, black and pu-erh teas using HPLC with a photodiode array detector. Talanta 57 (2), 307
316.

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140 Chapter 4 ,https://www.10thavenuetea.com/. (accessed 17.10.18.). ,http://www.oneorganicbrand.com/. (accessed 17.10.18.). ,https://www.nestle.in/. (accessed 17.10.18.). ,http://www.royalchai.net/sit/. (accessed 17.10.18.). ,https://www.kevita.com/. (accessed 17.10.18.). ,https://www.gtslivingfoods.com/. (accessed 17.10.18.). ,https://www.btkombucha.com/. (accessed 17.10.18.). ,https://www.drinkbuchi.com/. (accessed 17.10.18.). ,https://www.sujajuice.com/. (accessed 17.10.18.). ,http://www.tonicakombucha.com/. (accessed 17.10.18.). ,https://www.tetley.in/. (accessed 18.10.18.). , https://www.tajmahalteahouse.com/. (accessed 18.10.18.). ,https://www.twoleavestea.com/. (accessed 18.10.18.). ,http://www.digitaljournal.com/. (accessed 13.11.18.). ,https:// www.greenerpackage.com/. (accessed 06.01.19.). ,https://www.lipton.com/us/en/home.html/. (accessed 16.10.18.).

CHAPTER 5

Membrane Technologies for the Production of Nonalcoholic Drinks ˜oz1,2,3,4 Roberto Castro-Mun 1

University of Chemistry and Technology Prague, Prague 6, Czech Republic 2Institute on Membrane Technology, ITM-CNR, Rende, Italy 3Nanoscience Institute of Aragon (INA), Universidad de Zaragoza, Zaragoza, Spain 4Tecnolo´gico de Monterrey, Campus Toluca. Avenida Eduardo Monroy Ca´rdenas 2000 San Antonio Buenavista, 50110 Toluca de Lerdo, Mexico

Chapter Outline 5.1 Introduction 141 5.2 Nutritional Value of Alcoholic Beverages 143 5.3 Nonalcoholic Beer Production Through Membrane Processes 145 5.4 Nonalcoholic Wine Production Through Membrane Processes 151 5.5 Production of Other Nonalcoholic Beverages by Membrane Processes 5.6 Conclusion 158 Abbreviations 159 References 159

157

5.1 Introduction Today, the adult per capita consumption of alcoholic beverages has increased enormously according to the World Health Organization (WHO) (2011). It has been reported that the consumption in 2018 of alcoholic beverages worldwide was around 54.2 billion liters per year (www.statista.com), and this consumption is expected to increase (Solov, 2018). At this point, several types of drinks can be found in the category of alcoholic beverages, such as beer, spirits, wines (e.g., fortified wines, rice wine, or fermented beverages made of sorghum, millet, and maize), and some other traditional high-alcoholic content beverages (Cleophas, 1999). Among all these products, beer and wine have the highest consumption. However, over the past few decades the market of nonalcoholic beverages, especially for beer and wine, has increased in demand due to regulations concerning health issues. It is well-known that high and excessive consumption of alcoholic beverages may cause

Trends in Non-alcoholic Beverages. DOI: https://doi.org/10.1016/B978-0-12-816938-4.00005-7 © 2020 Elsevier Inc. All rights reserved.

141

142 Chapter 5 pancreas cancer, pancreatitis, hepatitis, fatty degradation of liver, cirrhosis, peptic ulcers, allergenic induction, increase of uric acid in plasma, obesity, and some other derivative harmful effects. In particular, pancreatitis and cirrhosis in their acute forms are frequently caused by high consumption of alcoholic beverages (Costanzo et al., 2010; Partanen et al., 1997; Sohrabvandi et al., 2012). Of course, these diseases are directly attributed to the alcohol content of such beverages. On the other hand, there are several favorable benefits of these products for human health, such as nutritional benefits and hypolipidemic, antimutagenic, and anticarcinogenic effects, reduction of cardiovascular disease (e.g., cardioprotective effect), immune system stimulation, antiosteoporosis effect, and reducing the risk of dementia (Sohrabvandi et al., 2012). In theory, nonalcoholic beverages can be manufactured by interrupting the fermentation process (Purwasasmita et al., 2015), or by using special and immobilized yeasts (Strejc et al., 2013). Unfortunately, changing this process may restrict the production of some of the desirable compounds of such products because in the brewery industry fermentation plays an important role during flavor formation and quality control of beers (Olaniran et al., 2017). In this way, this practice is not the most recommendable way for the production of non-alcoholic beverages. Herein, the post-alcohol removal (once the beverage fermentation is done) is the better approach. The dealcoholization of beverages is a potential alternative for the production of nonalcoholic drinks and can preserve most of the organoleptic and nutritional values of the original beverages. The dealcoholization process mainly involves physical processes, such as thermal (e.g., evaporation or distillation) (Andre´s-Iglesias et al., 2016; Belisario-Sa´nchez et al., 2012), or membrane-based processes [e.g., pervaporation (PV), nanofiltration (NF), reverse osmosis (RO), dialysis, membrane distillation (MD), diafiltration, osmotic distillation (OD), and membrane contactors (MCs)] being the latest and most sought-after technology for food technicians according to the features of each membrane process (Lipnizki, 2014; Mangindaan et al., 2018). Indeed, membrane-based processes are emerging alternatives for the treatment and processing of food systems (Cassano et al., 2018;Castro-Mun˜oz et al., 2017, 2018a; Galanakis, 2013; Galanakis et al., 2015), as well as the recovery of high-added value compounds from natural food products (Castro-Mun˜oz et al., 2016, 2018a; Galanakis, 2013, 2015; Galanakis et al., 2015). The aim of this chapter is to provide an overview of the literature findings for the dealcoholization of alcoholic beverages (beer, wines, and some others) by membranebased technologies for the production of nonalcoholic drinks. In addition, a brief overview of the nutritional value of original alcoholic beverages is also addressed, providing an outlook of the importance of selecting techniques (e.g. membrane processes) for the dealcoholization. The most relevant results from recently published studies are addressed and discussed.

Membrane Technologies for the Production of Nonalcoholic Drinks 143

5.2 Nutritional Value of Alcoholic Beverages An alcoholic beverage is typically defined as a drink which contains alcohol (i.e., ethanol) in its composition. Typically, alcoholic beverages can be classified into two categories. First, those that are commonly produced by fermentation, such as beer, cider, wine, mead, and pulque (Blas-Yan˜ez et al., 2018; Guichard et al., 2019; Sroka and Satora, 2017). These beverages contain less than 15% ethanol content. Second, are alcoholic drinks produced by distillation, such as vodka, gin, tequila, whiskey, mezcal, brandy, and soju to mention just a few (Arrizon et al., 2011; Jakubı´kova´ et al., 2018; Prentice and Handsjuk, 2016; Trejo et al., 2018). These beverages (so-called spirits) contain at least 20% ethanol, but they can contain up to 40% (well called as liquors). They are typically elaborated by means of fermenting grain, fruit, or vegetables. Afterward, the drink is concentrated by distilling. Beer, as a complex brewed beverage produced from the fermentation of malted barley in the presence of water and hops, is widely consumed around the world. It is likely that this product could the most consumed alcoholic drink because is more economical and typically easily accessible to customers (Bamforth, 2002). Beers generally contain between 2.5% and 13% (v/v) ethanol and, thus, their classification is commonly based on the alcohol content, for example, beers are usually classified as low-strength (having about 2%
3% alcohol), medium/ average strength (containing about 5% alcohol), and high-strength/strong (.5%
6% alcohol) beers (Bamforth, 2002; Sohrabvandi et al., 2012). Most beers worldwide have alcohol contents in the range of 3%
6% (v/v). When dealing with the benefits of beer in terms of nutrimental value, many studies have denoted that a light-to-moderate consumption of beer may provide multiple advantages to human health due to the presence of bioactive compounds such as protein, phenolics (antioxidants), certain minerals, anthocyanins, dietary fibers, some prebiotic compounds, and B vitamins (Sohrabvandi et al., 2010a, 2012). Table 5.1 shows the most common nutrients that can be found in beer. Table 5.1: Nutrients contained in normal beer. Vitamins Biotin Vitamins B12, B6 Vitamins A, C, D, E, K Niacin Folate Thiamine Riboflavin

Minerals Calcium Phosphorus Magnesium Potassium Sodium Iron Zinc Selenium

Source: Adapted from Sohrabvandi, S., Mortazavian, A.M., Rezaei, K., 2012. Health-related aspects of beer: a review. Int. J. Food Prop. 15 (2), 350
373. https://doi.org/10.1080/10942912.2010.487627.

144 Chapter 5 Definitely, beer is positively well-recognized as a good nutrient and energy source which contains multiple, desirable organoleptic compounds (e.g., alcohols, esters, carbonyl compounds, and vicinal ketones) (Olaniran et al., 2017) and also offers some medicinal health advantages. Finally, beer contains more protein and B vitamins than wine (Sohrabvandi et al., 2012); however, wine tends to present higher bioactive compound (e.g., polyphenols and anthocyanins) content than beer, for example, red wines contain about 1720 mg polyphenols/L (Lugasi and Ho´va´ri, 2003). Such compounds are well-known for their associated antioxidant capacity (Cartron et al., 2003; Paixa˜o et al., 2007). Indeed, minimal content of phenolic compounds have been quantified in beers compared to wines (Bartolome´ et al., 2000); although more than 35 phenolic compounds (e.g., tyrosol, ferulic acid, HMF, and tryptophol) can be found in beers (about 80%
90% from malt and 10%
20% from hops) (Sohrabvandi et al., 2010b), a huge range of phenolic compounds are contained in wines, such as catechin, epicatechin, p-coumaric acid, caffeic acid, gallic acid, and fertaric acid, to mention just a few (Paixa˜o et al., 2007). Table 5.2 displays the phenolic compounds that have been quantified in wine. The variety of phenolic compounds depends on the type of wine (e.g., red, white, sparkling, sherry, port, fruit, and brandy). Red wine is a complex mixture of flavonoids (such as anthocyanins and flavan-3-ols) and nonflavonoids (such as resveratrol, cinnamates, and gallic acid), while flavan-3-ols are the most abundant, with polymeric procyanidins composing up to 50% of the total phenolic constituents (Guilford and Pezzuto, 2011). It has been reported that phenolic compounds provided by beer and wine are absorbed and extensively metabolized by the human body (Nardini et al., 2006, 2009). Moreover, some beneficial effects have been attributed to the consumption of beer and wine, such as Table 5.2: Phenolic content in red wine. Phenolic Compound

Concentration (mg/L)

Catechin Epicatechin Dimer B1 Dimer B2 Dimer B3 Dimer B4 Trimer C1 Trimer C2 Gallic acid Protocatechuic acid Caftaric acid Gentisic acid Caffeic acid

89 94 69 54 79 96 41 74 43 12 55 54 8

Source: Adapted from Cartron, E., Fouret, G., Carbonneau, M.A., Lauret, C., Michel, F., Monnier, L., et al., 2003. Red-wine beneficial long-term effect on lipids but not on antioxidant characteristics in plasma in a study comparing three types of wine—description of two O-methylated derivatives of gallic acid in humans. Free Radic. Res. 37 (9), 1021
1035. https://doi.org/10.1080/10715760310001598097.

Membrane Technologies for the Production of Nonalcoholic Drinks 145 antimutagenic and anticarcinogenic effects, cardioprotective effect, immunomodulation, and antiosteoporosis effect (Sohrabvandi et al., 2012). Finally, the balance between alcohol and phenolic compounds in wine and beer may be critical in determining their antioxidant potential due to alcohol displaying prooxidant effects (van Golde et al., 1999).

5.3 Nonalcoholic Beer Production Through Membrane Processes Typically, dealcoholization implies the removal of ethanol from alcoholic beverages (Lipnizki, 2014) without altering the sensory and nutritional properties of the original products. However, unfortunately some of the valuable compounds can be lost considerably. Table 5.3 shows a comparison of the polyphenols profiles and related substances in alcohol-free and standard beers. Importantly, nonalcoholic beers are currently produced by means of different approaches in order to suppress the alcohol production in the beer (Lehnert et al., 2009; Sohrabvandi et al., 2010a; Strejc et al., 2013), including: • • • • • • • •

the use of special strains of fermenting yeasts; reducing fermentable fractions to nonfermentable fractions; reducing glucose content in the wort; heating of fermenting wort; high-temperature mashing; pressurization during fermentation; cold contact procedure; periodic aeration of fermenting wort; Table 5.3: Comparison of the polyphenols content and its derivatives in alcohol-free and standard commercial beers. Compound HMF p-Hydroxybenzoic acid Tyrosol Catechin 2,3-Dihydroxy-1-guaiacylpropan-1-one Vanillic acid Caffeic acid Vanillin p-Coumaric acid Ferulic acid Sinapic acid Tryptophol

Alcohol-Free Beer

Standard Beer

1.65 0.073 2.78 0.641 0.025 0.347 0.045 0.048 0.576 0.718 0.073 0.242

2.57 0.092 11.83 0.463 0.034 0.477 0.074 0.028 0.773 1.305 0.090 0.368

Source: Adapted from Bartolome´, B., Pen˜a-Neira, A., Go´mez-Cordove´s, C., 2000. Phenolics and related substances in alcohol-free beers. Eur. Food Res. Technol. 210 (6), 419
423. https://doi.org/10.1007/s002170050574.

146 Chapter 5 All these ways produce changes in the nutrimental value as well as the sensorial characteristics of beer (Bra´nyiket al., 2012). This is the main reason that the industry is looking for selective techniques to carry out the dealcoholization. According to Sohrabvandi et al. (2010a), several techniques are currently being investigated to be commercially employed for the dealcoholization of beers, such as vacuum distillation, water vapor or gas-stripping under vacuum, adsorptive alcohol removal, dialysis, RO, and OD. Some of membrane processes like dialysis, and RO are already industrial methods for beer dealcoholization (Blanco et al., 2016). Using membrane processes, it is quite possible that the first successful attempt of ethanol removal from beer was proposed by Leskosek and Mitrovic (1994). They used a dialysis technique which does not use transmembrane pressure as a driving force, but is governed by the concentration gradient to produce a low-alcohol content beer using cuprophane (regenerated cellulose) membranes. This dialysis process was efficiently able to remove up to 40% of the alcohol content from beer. The researchers optimized the process allowing up to 80% ethanol removal (Leskoˇsek et al., 1995; Petkovska et al., 1997). In this method, dealcoholization using dialysis is performed in the water, beer ingredients tend to move from the side of the high concentration (beer side), to the side of the low concentration (water), while some water could diffuse and thus pass from dialysate into beer (Bra´nyik et al., 2012). At this point, the beer risks becoming diluted which changes its composition; moreover, during the removal of alcohol by this technique, some other compounds (e.g., esters) can be removed as well. However, the advantage of this membrane technology is that there is no thermal stress on the product. Even though dialysis is a pressureless process, a certain overpressure [at least carbon dioxide (CO2) saturation pressure] should be applied to the side of the beer as well as the permeate side since CO2 release may disturb the diffusion (Leskosek and Mitrovic, 1994). In dialysis, the degree of dealcoholization, which implies dealcoholized products from 0.39 to 0.79 vol.%, is regulated by varying the dialysate flow rates in the ratios of 1:6.5
1:0.4 (beer:dialysate) (Leskosek and Mitrovic, 1994; Zufall and Wackerbauer, 2000). The higher the flow rate of the dialysate, the higher the dealcoholization degree. Furthermore, depending on the flow rate conditions, 4%
11% of the total alcohols of the original beer can be found in the alcohol-reduced beer (Zufall and Wackerbauer, 2000), whereas the total of aromatic esters decreases below the detection limit. Importantly, a reduction of the ethanol content by more than 90% (i.e., ,0.5 vol.%) is hardly possible using dialysis. In this way, bitter units and pH decrease slightly, while the color, total nitrogen, coagulable nitrogen, and polyphenol content remain unchanged (Zufall and Wackerbauer, 2000). The use of another membrane technology toward beer dealcoholization was proposed by Leskoˆsek et al. (1997). They also used a diffusive and convective process, like diafiltration, employing polysulfone, and cellulose-based membranes. Such membranes displayed an alcohol removal tendency of about 50% (Leskoˆsek et al., 1997). Finally, the alcoholreduced beers are clearly noticeable by their lack of body, which can be countered with higher dialysate flow rates during the diafiltration process. There are no changes produced

Membrane Technologies for the Production of Nonalcoholic Drinks 147 by heat variations, as mentioned previously, such as caramel or bread-like notes, but a clear acid impression is noticed (Zufall and Wackerbauer, 2000). However, the concentration of diacetyl at a specific threshold value (diacetyl 5 0.15 mg/L) is responsible for the typical aroma aberrations in beer. RO has also been also employed for beer dealcoholization. In this process, the flow is fed tangentially to the membrane surface, where ethanol (and water) tends to permeate across the membrane when a transmembrane pressure is applied, which substantially exceeds the beer osmotic pressure. The taste and nutritive components of beer are retained in the product (Mangindaan et al., 2018). The RO can be performed in batch, continuous, and diafiltration modes, as illustrated in Fig. 5.1. For RO and its role in the removal of alcohol, membranes with an asymmetric structure, having active layers made from several materials such as cellulose acetate, polyamide, or polyimide on polyester, polysulfone, or fiber glass support structures, are needed (Bra´nyik et al., 2012). For instance, a cellulose acetate (200 g mol MWCO) membrane can reach an alcohol concentration in permeate of up to 3.84% (Catarino et al., 2007), and final alcohol content in the beer being about 0.5% (Catarino et al., 2006). Furthermore, Catarino et al. (2007) reported that higher transmembrane pressures resulted in higher permeate flux and higher rejection of ethanol, while lower temperatures commonly obtained low-permeate flux, but an increase in the rejection of aroma compounds. It seems like cellulose acetate membranes are suitable for producing high fluxes with lower ethanol rejection, while the

Figure 5.1 Graphical depiction of RO processes for beer dealcoholization. RO, reverse osmosis.

148 Chapter 5 highest rejection can be obtained by polyamide (hydrophobic) membranes. Moreover, a 77% retention of ethyl acetate and 68% for isoamyl acetate for RO cellulose acetate membranes at 20 bar and 51 C can be obtained. However, such retention rates decrease notably when increasing the pressure (Catarino et al., 2007). Falkenberg (2014) tested a commercial RO90 polyamide-based membrane for the dealcoholization of beer, and the author observed relatively high retention being lowest at 0.45% while the highest permeability calculated was 85%. Generally, the level of permeability of approximately 50% was observed. This was in agreement with the data provided by the supplier (Alfa Laval), in which an ethanol permeability level of 49% at 20 C and 25 bar was reported. On the other hand, higher ethanol removal together with the rejection of desirable aroma compounds can be obtained via a diafiltration mode rather than a batch-operating mode (Mangindaan et al., 2018). Nevertheless, Bra´nyik et al. (2012) have presented a comparison of the physicochemical properties of original beers and the effect on their composition after alcohol removal by dialysis and RO (see Table 5.4). It can be seen that some high-added value compounds together with the alcohol can be removed from the beer, for example, significant losses of volatile compounds of around 70%
80% of higher alcohols and 80%
90% of esters have been reported. Finally, Alcantara et al. (2016) also evaluated beer dealcoholization by means of RO. Their process allowed to preserve the phenolic compounds, antioxidant activity, and some other quality parameters (e.g., color, bitterness, and pH), whereas the alcohol content was almost totally removed after 7 h operating time. Table 5.4: Comparison of original input beer and alcohol-free beers processed by dialysis and reverse osmosis. Dialysis Property/Compound Original gravity (wt.%) Ethanol (% ABV) 1-Propanol (mg/L) 2-Methylpropanol (mg/L) 2-Methyl-1-butanol (mg/L) 3-Methyl-1-butanol (mg/L) Ethyl acetate (mg/L) Isoamyl acetate (mg/L) 2-Phenyl ethyl acetate (mg/L) Isovaleric acid (mg/L) Caproic acid (mg/L) Capric acid (mg/L)

Reverse Osmosis

Original

Dealcoholized

Original

Dealcoholized

11.16 4.80 9.4 7.0 9.9 43.6 12.1 2.2 , 0.1 1.22 1.88 0.35

4.53 0.47 0.5 0.3 0.4 1.5 , 0.1 , 0.1 , 0.1 0.49 1.02 0.21

10.83 4.92 12.0 17.0 4.3 3.0 15.0 1.5 0.63 0.76 2.0 0.95

2.48 0.40 2.0 5.1 2.8 10 1.8 0.16 0.04 0.18 0.22 0.11

Source: Adapted from Bra´nyik, T., Silva, D.P., Baszczyˇnski, M., Lehnert, R., Almeida e Silva, J.B., 2012. A review of methods of low alcohol and alcohol-free beer production. J Food Eng. 108 (4), 493
506. https://doi.org/10.1016/j.jfoodeng.2011.09.020.

Membrane Technologies for the Production of Nonalcoholic Drinks 149 PV is considered an emerging technology to produce nonalcoholic beer (Blanco et al., 2016). This membrane process is efficient in separating different types of water
organic, organic
organic, and organic
water mixtures (Castro-Mun˜oz et al., 2018b,d) where the beer dealcoholization implies an organic
water separation (i.e., ethanol removal from a complex aqueous solution). PV is able to separate the components by a solution-diffusion mechanism together with the driving forces (temperature and vacuum pressure) (Castro-Mun˜oz et al., 2018c). In particular, the membrane material plays an important role for the separation by PV, as illustrated in Fig. 5.2. Crucially, the removal of alcohol comprises the use of nonporous hydrophobic membranes which are able to remove organics, such as alcohols (e.g., ethanol, propanol, isobutanol, and isoamyl alcohol), aldehydes (e.g., acetaldehyde), and esters (e.g., ethyl acetate and isoamyl acetate). Indeed, PV may find its main application in food and cosmetic industries for the extraction of aroma compounds (Lipnizki et al., 2002; Raisi et al., 2009; Saffarionpour and Ottens, 2018). For example, Catarino et al. (2009) developed a process to extract aromas from beer through a polyoctylmethylsiloxane membrane. Several compounds were identified in beer, such as alcohols (e.g., ethanol, propanol, isobutanol, and isoamyl alcohol), esters (e.g., ethyl acetate isoamyl acetate), and aldehydes (e.g., acetaldehyde). Moreover, the authors demonstrated that different groups of substances (higher alcohols or esters) are enriched in the permeate stream depending on the parameters flow rate, feed temperature, and permeate pressure (Catarino et al., 2009). Similarly, Olmo et al. (2014) demonstrated that PV meets the requirements for the recovery of aroma compounds from beer, for example, isobutyl alcohol increased up to 16% in the alcohol-free beer, while ethyl acetate in low-alcohol beer increased up to 35.72%. In this context, the extraction of beer aromas could be useful to match the aroma profile of the dealcoholized beers, which can, unfortunately, be lost during the processing.

Figure 5.2 General drawing of hydrophilic and hydrophobic membranes for PV applications. PV, pervaporation.

150 Chapter 5 Regarding beer dealcoholization, Catarino and Mendes (2011b) investigated the production of low-alcohol beer by means of an industrial plant. Basically, the plant involved a hybrid process, which included a PV set-up and distillation unit. The aroma compounds (e.g., amyl alcohol, ethyl acetate, isoamyl acetate, and acetaldehyde) were recovered using a PV polyoctylmethylsiloxane membrane. Such aroma compounds were then incorporated into the dealcoholized beer (produced by conventional distillation). At this point, this industrial methodology allowed to obtain a nonalcoholic beer (less than 0.5 vol.%) with a good flavor profile. It is important to note that PV technology does not, in principle, require temperature to carry out the separation, nonetheless, the use of temperature may help to improve the permeate fluxes with a possible effect on component selectivity. MD, which is a similar membrane process to PV but uses temperature in the feed, was proposed for beer dealcoholization (Purwasasmita et al., 2015). The dealcoholization process was performed by using a nonporous, spiral-wound membrane (polyamide-based, thin-film composite). This process reduced the ethanol content up to 2.45% alcohol by volume (ABV) (from 5% ABV) within 6 h. Moreover, the authors reported that minimal loss in nutriment components was observed. Unlike MD, OD uses porous membranes to carry out beer dealcoholization. Typically, an ethanol is placed onto the membrane surface at atmospheric pressure and temperature, while on the other membrane side is contacted to a stripping solution which is flowed in a back-current mode, as Fig. 5.3 shows. Basically, ethanol is permeating through the membrane and, thus, the stripping solution is tasked to capture the ethanol. De Francesco et al. (2015) developed an OD pilot plant for the production of low-alcohol beer. This set-up was able to reduce the alcohol concentration up to 0.5
0.8 vol.% (from an initial content of 4.5
5 vol.%). Unfortunately, the percentage of volatile

Figure 5.3 General drawing for beer dealcoholization using osmotic distillation.

Membrane Technologies for the Production of Nonalcoholic Drinks 151 compounds loss was significantly high (80%
85%) after treatment, conducting many volatile compounds to be under the sensory threshold. In the same way, several studies producing low-alcohol beers have been reported using this membrane technology, for example, the nonalcoholic beers contained ethanol between 0.47 and 1.0 vol.% (De Francesco et al., 2014; Liguori et al., 2015; Russo et al., 2013). Indeed, OD has demonstrated to be able to remove the ethanol by over 80%, which can be achieved by polypropylene hollow fiber membranes (De Francesco et al., 2014; Liguori et al., 2015).

5.4 Nonalcoholic Wine Production Through Membrane Processes Similar to nonalcoholic beer, low-alcoholic wine production is carried out using similar approaches. Generally, prefermentation technologies are used to restrict the alcohol production. Typically, low concentration of fermentable sugars in juice during early grape harvest, juice dilution, or arresting fermentation produce the limitation of ethanol production. At this point, significant levels of unfermented sugars remain. In another strategy, the early grape harvest could result in wines that are organoleptically undeveloped due to the reduction of flavor precursor development in the grapes prior to harvest, coupled to high-acidity level, and lack of yeast-contributed flavor compounds. In this regard, adjusting the vine-leaf area to crop ratio is another interesting viticultural intervention for controlling the concentration of fermentable carbohydrates in harvested wine grapes (Schmidtke et al., 2012). Finally, the use of biotechnological tools, like enzyme technology (e.g., glucose oxidase, and catalase), for lowering the concentration of fermentable sugars in the grape juice is also applied to restrict the alcohol production prior to fermentation. Concurrent with fermentation, the use of novel yeast strains is also highlighted. According to the literature, different types of genetically modified strains have been used such as Saccharomyces cerevisiae, Pichia, and Williopsis. All these strains have proven to limit the alcohol production in wines which displayed acceptable organoleptic properties; however, there are further drawbacks implied in gene technology for yeast-strain manipulations, which have not allowed the consolidation of this approach (Schmidtke et al., 2012). On the other hand, there are some other techniques which are used as postfermentation technologies for removing ethanol, such as vacuum evaporation and vacuum distillation (Andre´s-Iglesias et al., 2015; Blanco et al., 2016; Lipnizki, 2014). For instance, well-established techniques used in postfermentation steps, such as low-temperature distillation, have been applied during alcoholic fermentation for the removal of about 2% v/v of alcohol without significantly changing the concentration of other wine constituents (Aguera et al., 2010). However, these approaches still change the sensorial properties of the products. As introduced previously, the wine has been also processed by membrane-based technologies, to produce nonalcoholic wine. Since wine contains more nutritional compounds than beer, the

152 Chapter 5 postfermentation removal of ethanol has to be carefully performed, promoting the degradation of bioactive compounds (e.g., polyphenols, antioxidants, etc.) as little as possible (Go´mez-Plaza et al., 1999); however, wine also contains a higher ethanol content compared to beer. To date, different types of wines have been dealcoholized, for instance, Taka´cs et al. (2007) reported dealcoholization of semi-sweet Tokaji Harslevelu-type wines (alcohol content 13.11% ABV) using pervaporation (PERVAP) membranes. Such commercial membranes are well-recognized by their organophilic nature. The authors reported that temperature influences in PV performance in terms of flux and separation ability, for example, higher permeate fluxes, were commonly obtained at higher temperatures, whereas the ethanol selectivity of the membranes tended to decrease. No details about the physicochemical properties of the dealcoholized wines were provided. It is important to note that in PV technology the ethanol removal takes place at the membrane interface where the ethanol is absorbed by partial vaporization and then diffused across the membrane, followed by a condensation into the stripping phase (Baker et al., 2010; Castro-Mun˜oz et al., 2018b). On the other hand, Catarino and Mendes (2011a) used another PV organophilic (polyoctylmethylsiloxane supported in polyetherimide) membrane to recover the aroma compounds from wine. Afterward, the aroma compounds were added back to the dealcoholized wine, which was partially dealcoholized by means of NF. The authors tested four different NF membranes (with the same molecular weight cut-off of 200 Da), which were manufactured by different membrane materials. In general, the integrated membrane processes were able to provide a high-quality, low-alcohol wine (c. 7
8 vol.%) from a standard alcoholic wine (c. 12 vol.% of ethanol). In a different approach, Salgado et al. (2017) applied PV and NF steps for the preparation of flavored white wines with lowalcohol content. Basically, the overall production processes, NF process is involved in sugar reduction of must, while PV was used for aroma recovery. The obtained wine contained a final alcohol degree between 10.2 and 10.5 vol.%. The conventional production commonly produces white wine containing c. 12 vol.% ethanol concentration, which means a small reduction in alcohol degree with a concentration of the aroma compounds. Particularly, the harvest of grapes also plays an important role in wine production. It is well-documented that early ripening of grapes promotes, among others, a higher fermentable sugar (glucose and fructose) content. This practically leads to wines with an alcoholic degree higher than desired. In this context, NF is mainly considered as an easy tool for the sugar reduction in must (Salgado et al., 2015a,b). As can be seen, NF technology has also been applied in the production of nonalcoholic wine. NF, well-defined as a pressure-driven membrane process, uses asymmetric porous membranes (Cassano et al., 2018; Galanakis, 2015) and displays features between RO and UF technologies. However, NF can also comprise with the concentration of the wine (Banvolgyi et al., 2006; Taka´cs et al., 2010). For example, Banvolgyi et al. (2006) analyzed the performance of NF (XN45 from Trisep) for concentrating red wine in the retentate,

Membrane Technologies for the Production of Nonalcoholic Drinks 153 while the water and ethanol permeated through the commercial membrane resulting in permeate with a similar alcoholic content (10.75% ABV) as the original wine. The use of NF technology could be an strategic way for the production of wine with a low-alcohol content due to it being possible to produce low alcohol
content wine by reducing sugar levels in the must before fermentation (Garcı´a-Martı´n et al., 2010, 2011; Salgado et al., 2015b). In this way, a clarified white wine containing 5
7.3 vol.% of ethanol could be obtained, where the control and the normal process usually presents 12.0 vol.% (Garcı´a-Martı´n et al., 2011). Similarly, Garcı´a-Martı´n et al. (2010) also performed sugar reduction (glucose and fructose) by using two sequential NF steps. This allowed to produce a red wine with an alcohol content between 5.6 and 8.4 vol.%, which was directly collected from permeate streams. However, the wine did not meet the sensory quality, which was attributed to the high rejection values that NF membranes offer toward high-added valuable compounds, such as resveratrol and anthocyanins (Banvolgyi et al., 2016). The authors suggested that low-alcohol wine could be improved by being combined with normal wine produced by standard procedures (Garcı´a-Martı´n et al., 2010). The partial dealcoholization using NF membranes has been studied by other authors who demonstrated that such technology may produce wines with very low alcoholic content, for example, 1.2
1.4 vol.% (Salgado et al., 2015a,b) and 4
6 vol.% (Banvolgyi et al., 2016). RO displays similar characteristics as NF; however, RO has been studied in more detail. RO needs low-energy input, can be operated at ambient temperatures, allows reproducible control over separations. Moreover, it does not require disposable filtration media or other devices, and RO can be easily automated for continuous operation. RO, such as some other membrane technologies, operates under the same principle of tangential flow, in which the liquid flows parallel or tangential to the membrane surface at high velocity under pressure. The fluid passes through the membrane, but compounds with molecular weight higher than the nominal molecular weight cut-off of the membrane will be swept along in the stream of feed across the membrane (Echavarrı´a et al., 2012; Gil et al., 2013; Pilipovik and Riverol, 2005). Importantly, the recycling configuration may ensure that more permeate will pass through the membrane during each cycle until the desired concentration of the feed can be reached. In order to effectively do this, several module configurations have been developed, such as e flat sheet (better known as plate and frame), tubular, hollow fiber, and spiral-wound configurations. The first patent for the application of RO in alcoholic beverages was obtained by the West German brewing company Lowenbrau in 1975 for the dealcoholization of beer and wine (Meier, 1992; Schmidtke et al., 2012). However, other applications of RO in wine production imply the removal of flavors and colors, must concentration (as an alternative to chaptalization), development of new products such as aperitifs, and wine stabilization against tartrate precipitation and deacidification (i.e., removal of volatile acids) of grape juices (Baldwin, 1998; Smith, 2002).

154 Chapter 5 Currently, RO has been mainly applied for wine dealcoholization, which mainly seeks to control the alcohol content of wines (Labanda et al., 2009; Massot et al., 2008). RO is used for the postfermentation removal of ethanol, which can considerably reduce the alcohol content up to 2 vol.% (Bogianchini et al., 2011), while minimal changes on physicochemical properties can take place. Table 5.5 shows a comparison of an original wine before and after dealcoholization by RO. Practically, the ethanol content of wine was reduced from the original content of 12.70
1.77 vol.%. Moreover, some components were slightly concentrated, for example, anthocyanins and tannins. This produced an increase in antioxidant activity as well (Bogianchini et al., 2011). Gil et al. (2013) partially dealcoholized red wine by means of RO, and unlike the previous study, the RO process was not efficient to remove high quantities of ethanol as only 1
2 vol.% content was reduced. But minimal changes were found in pH, color intensity, total phenolic index, proanthocyanidin concentration, and Table 5.5: Comparison of original wine and alcohol-free wine processed by reverse osmosis. Parameter Ethanol (%, v/v) Glucose (g/L) Fructose (g/L) Total sugar (g/L) Glycerol (g/L) Volatile acidity (g/L) Citric acid (g/L) Tartaric acid (g/L) Lactic acid (g/L) Succinic acid (g/L) Total acidity (g/L) Gelatin index (%) pH Total phenols index (a.u.) Total anthocyanins (mg/L malvidin-3-O-glucoside) Free anthocyanins (mg/L malvidin-3-O-glucoside) Total tannins (g/L) Abs 420 Abs 520 Abs 620 Modified color intensity (MCI) Tonality (tint) Cielab L* Cielab a* Cielab b*

Original Wine

Dealcoholized Wine (Retentate)

12.70 3.36 0.60 3.97 8.18 0.32 0.17 2.50 1.40 3.09 4.50 57.80 3.46 46.18 286.00 227.00 1.54 2.67 3.80 0.78 7.25 0.70 21.30 52.6 34.4

1.77 3.17 0.54 3.72 7.50 0.40 0.16 2.38 1.31 2.81 4.30 50.50 3.60 42.30 289.00 239.00 1.65 3.00 4.77 1.01 8.77 0.63 15.40 45.40 25.70

Source: Adapted from Bogianchini, M., Cerezo, A.B., Gomis, A., Lo´pez, F., Garcı´a-Parrilla, M.C., 2011. Stability, antioxidant activity and phenolic composition of commercial and reverse osmosis obtained dealcoholised wines. LWT Food Sci. Technol. 44 (6), 1369
1375. https://doi.org/10.1016/j.lwt.2011.01.030.

Membrane Technologies for the Production of Nonalcoholic Drinks 155 their mean degree of polymerization between control wines. To date, the studies have provided inputs about the good performance of RO for the wine dealcoholization; however, since wine is a really complex mixture of several compounds (phenolic compounds, anthocyanins, carbohydrates, and so on). Pilipovik and Riverol (2005) stated that operating issues such as concentration polarization and fouling phenomena could compromise the economic feasibility of this process. More recently, Longo et al. (2018) reported a comparative study of the partial dealcoholization of wines versus the earlyharvest process. In principle, the alcohol concentration of early-harvest and late-harvest wines were respectively 9% and 13.5% v/v for Verdelho, and 10.5% and 13% v/v for Petit Verdot. Afterwards, late-harvest wines were dealcoholized to equal the same alcohol level of early-harvest samples using a combined RO-evaporative perstraction process. In dealcoholized wines, there was a decrease in volatile compounds (esters particularly) compared to late-harvest treatments. Moreover, the authors stated that for both varieties, the sensory attribute ratings for overall aroma intensity and alcohol mouthfeel also decreased using dealcoholization. Finally, they concluded that when a dealcoholization treatment is considered for high-alcohol wines, it is important to take into account that membrane effects can significantly change depending on the wine’s nonvolatile matrix composition and the level of alcohol reduction required (Longo et al., 2018). With the use of suitable membrane support and enough pressure, RO can reduce the alcohol content in wines to almost any degree desired. Additional advantages may include the reductive environment that can be maintained during processing, and good energy efficiencies. However, as water and some other organic compounds are removed along with ethanol, it must be added back to the concentrated wine or added to the wine before the use of RO. In this way, this may create legal issues in countries where the addition of water to wine is banned (Pickering, 2000). Interestingly, Bui et al. (1986) avoided the problem of water addition by using a double RO process that was able to produce low-alcohol and alcohol-enriched wines simultaneously. In such time, some other processing approaches based on RO were also reported (Chinaud et al., 1991; Cuenat et al., 1985; Weiss, 1987). Unlike RO, which uses hydrostatic pressure as the driving force, dialysis uses differences in concentrations for compound transport. In dialysis, water is particularly used to provide the concentration gradient, allowing the transport of ethanol and compounds with low-molecular weight out of the wine to the water. The advantages of dialysis include operating without pressure, no need for increases in concentration or dilution, and no need of cooling in the system. These are beneficial to have minimal loss of CO2 (Schobinger, 1986). For instance, Wucherpfenning et al. (1986) reported a procedure in which wine was dialyzed against wine dealcoholized by vacuum distillation rather than against water, especially as the concentration gradient exists only or ethanol, they stated that a slight change was noticed in the concentration of the other compounds.

156 Chapter 5 As mentioned previously, in OD, ethanol (from wine) commonly permeates across the membrane, in which, on the other side of the membrane, the ethanol is captured by the stripping solution (see Fig. 5.3). In general, OD is able to partially dealcoholize wine up to a final concentration of ethanol of about 8%
11% ABV, this reduces the alcohol content by around 2% ABV (Mangindaan et al., 2018). In this process, the performance depends on the temperature and types of stripping agent; however, amazing findings have been reported regarding the removal of ethanol from wine. Varavuth et al. (2009) studied the dealcoholization process by means of microporous PVDF hollow fiber membranes. The ethanol concentration in wine was reduced to roughly 34% of the initial concentration during 360 min operation (at 35 C), which means that the original wine (containing 13.2 vol.% of ethanol) was dealcoholized up to 8.7 vol.%. This was achieved by using water as a stripping solution. Regarding the aroma compounds, ethyl acetate and isoamyl alcohol were lost by approximately 70% and 44%, respectively, after 360 min of operation. While, the ethanol removal from wine in the long-term test of OD was performed over 360 min operating time. Higher dealcoholization efficiency was reported by Liguori et al. (2013a), who reached to reduce up to 2 vol% the ethanol content in wines. The low-alcohol wine conserved the original physicochemical properties of the original wine. More efficiently than the previous study, Liguori et al. (2013b) were able to produce a red wine with very low ethanol concentration (0.19 vol.%) from a normal wine (13 vol.%). However, the volatile compounds (such as isoamyl alcohols, 2-phenylethanol, 3-ethoxy-1-propanol, 2-propanol, 2,3-butanediol, 3-methyl-2-hexanol, 2-hexanol, 1-propanol, isobutyl alcohol, and benzyl alcohol) were also decreased by 98%. This probably may not provide so good organoleptic properties compared to an original wine, even when there were no significant changes in oenological parameters, such as pH, total acidity. Indeed, most of the organic acids were maintained, whereas some others (citric and oxalic acids) were slightly concentrated (Liguori et al., 2013b). In addition, there are some other processes which follow the same principle of OD, for example, MC. This membrane-based technology has also been useful for wine dealcoholization. Table 5.6 provides a summary of some wines that have been processed by means of MC. It can be noticed that MC can reach an almost complete ethanol removal (0.42 vol.%) in wines. Generally, polypropylene-based MCs have been tested and are promising candidates to reduce the ethanol in these beverages (Ferrarini et al., 2016; Gambuti et al., 2011; Liguori et al., 2010; Motta et al., 2017). Moreover, the final dealcoholized products have shown similar chemical compositions to the original wines in terms of reducing sugars and acidity, while in specific cases the dealcoholized wines were enriched in phenolic substances; however, the dealcoholized wines were lacking in aroma compounds, which were probably removed out with the ethanol from the original product. Finally, as with the membranes used for OD technology, the membrane performance in contactors depends on

Membrane Technologies for the Production of Nonalcoholic Drinks 157 Table 5.6: Comparison of original wines and their dealcoholization by means of membrane contactors.

Type of Wine Aglianico wine Langhe Rose` Aglianico red wine Verduno Pelaverga red wine Barbera red wine Piedirosso red wine Red wine Merlot red wine Aglianico red wine

Original Wine (Ethanol Concentration, vol.%)

Dealcoholized Wine (Ethanol Concentration, vol.%)

References

12.8 13.20 15.46 15.2

0.42 5.0 1.84 5.0

Liguori et al. (2010) Motta et al. (2017) Gambuti et al. (2011) Motta et al. (2017)

14.6 13.67 13.99 13.88 15.46

5.0 8.41 6.94 8.99 10.84

Motta et al. (2017) Gambuti et al. (2011) Ferrarini et al. (2016) Gambuti et al. (2011) Lisanti et al. (2013)

temperature, feed composition, types of stripping agent, stripping flow rates, as well as the features of the membrane material (Diban et al., 2008). Such parameters tend to influence the individual resistances for ethanol that are the major contributors to the transport resistance across any membrane.

5.5 Production of Other Nonalcoholic Beverages by Membrane Processes To date, beer and wine are the main alcoholic beverages subjected to dealcoholization. This is probably due to the fact that they are the most consumed alcoholic products worldwide. Nonetheless, some other alcoholic beverages are also popular, such as cider. This product includes a wide range of fermented apple juices obtained by various processes and with different organoleptic characteristics (Villie`re et al., 2015). Cider is a low-alcohol beverage, which represents an important segment of the apple industry, and it is popular in different countries in North America, Europe, and Australia (Lorenzini et al., 2019). A common cider contains 6 mL ethanol/100 mL, 0.5 g/L sugars (e.g., glucose and fructose), 2.9 g/L malic acid, 2.2 g/L sorbitol, and 0.1 g/L acetic acid. While different types of volatile compounds have been identified, such as alcohols (e.g., 1-butanol, 2-butanol, 3-methyl-1butanol, 2-phenylethyl alcohol, cis-3-hexen-1-ol, trans-3-hexen-1-ol, 1-pentanol, benzyl alcohol, and vanillic alcohol), esters (e.g. ethyl butyrate, ethyl isovalerate, ethyl hexanoate, ethyl lactate, ethyl cinnamate, and isoamyl acetate), fatty acids (e.g., octanoic acid, isovaleric acid, and hexanoic acid), and some other traces of organic acids (Lorenzini et al., 2019; Xu et al., 2007; Ye et al., 2014). To date, the success of ciders regards to their great diversity in both composition and sensory characteristics, in which ciders are commonly affected by the process conditions. The probable losses of compounds responsible for odor and aroma could be an important

158 Chapter 5 issue that has limited the dealcoholization procedures (Renard et al., 2011). Since the 1960s, microfiltration technology has been mainly used for the clarification and sterilization of ciders, as well as beer, brandy, and wine (Fane et al., 2010; Palacios and Caro, 2002). In fact, some scopes of research are still currently investigating the role of this membrane technology on cider quality during removal of haze materials (Zhao et al., 2015), pectins (Zhao et al., 2017), and some microorganisms (e.g., Salmonella sp., Escherichia coli, and Cryptosporidium parvum) (Valappil et al., 2009). Similarly, Puskas et al. (2013) evaluated the influence of cold stabilization treatment and membrane filtration on apricot brandy’s stability and volatile compounds. When dealing with dealcoholization, Lo´pez et al. (2002) attempted to produce low-alcohol apple cider by RO. In this study, different aromatic polyamide and cellulose acetate membranes were tested. From the analysis, it was noticed that 90% retention of ethyl acetate for RO polyamide membranes ( . 97% NaCl retention) at 25 bar, 15 C can be reached (Lo´pez et al., 2002). While lower retention at 60% for RO CA membranes ( . 95% NaCl retention) at 25 bar and 15 C was observed. Therefore the authors defined the commercial AFC 99 tubular membrane (based on polyimide) as the most suitable for the dealcoholization process by higher retention rates of desirable compounds (e.g., ethyl acetate, acetaldehyde, propanol, isobutanol, isoamyl alcohol, 1-hexanol, and acetic acid), which was attributed to its hydrophobicity. After that, this membrane was then tested in batch and diafiltration modes for dealcoholization (see Fig. 5.1). It was reported that the diafiltration mode was more efficient for ethanol removal compared to the batch mode; ethanol removals of about 75% and 50% were obtained, respectively. Finally, this approach has proven that membrane-based technologies are an efficient tool for alcohol removal for other types of alcoholic beverages, like ciders. It is quite possible that in the coming years such membrane techniques will be further investigated for the dealcoholization of these highly consumed beverages.

5.6 Conclusion This chapter has provided considerable proof of the dealcoholization of alcoholic beverages postfermentation by means of membrane-based technologies which deal with the production of nonalcoholic drinks. Moreover, the dealcoholization procedure seems to be a simple process; however, alcoholic beverages (e.g., beer, wine, and cider) having complex multicomponent colloidal structures of their numerous interactions, makes the removal of alcohol complicated. In fact, any change in terms of beer/wine/cider composition may cause changes in membrane performance (removal efficiency and rate) and subsequently affect the quality of the dealcoholized beverage. Typically, beer and wine can be dealcoholized by conventional distillation, but definitely, other membrane-based technologies, like RO and dialysis, have established themselves for beer dealcoholization by 8
10 times (Frank Lipnizki, 2014). Clearly, the key advantage of

Membrane Technologies for the Production of Nonalcoholic Drinks 159 such membrane technologies over distillation deals with the operating temperature, for example, beer can be dealcoholized at low temperatures (e.g., 78 C), minimizing the effect of temperature on the beer quality. Moreover, using PV, if the removal of ethanol is attempted to be as efficient as possible, the use or hydrophobic membranes is crucial, which can selectively remove the alcohol from the drinks. However, PV has been mainly involved for aroma recovery. PV may help to match the organoleptic characteristics of the dealcoholized beverages, which definitely loose organic compounds as a result of dealcoholization. It is likely that the membrane-based processes will also be the preferred methods in the future for the removal of alcohol, together with supercritical fluid extraction, despite its high-pressure requirement, due to their promising properties of high selectivity to ethanol, mild-operation temperature, and low-energy consumption, combined with high productivity (in terms of permeate fluxes). Moreover, these technologies will be preferred when the quantity of ethanol is low (,15%) (i.e., wine, cider, and beer). On the other hand, when the ethanol concentration is higher than such percentages, the ethanol selectivity of these technologies are compromised. Finally, there is still a lot of effort to be done on the research for the development of the suitable separation process that may produce brews that are healthy (i.e., dealcoholized), delicious, and with acceptable sensory and organoleptic properties.

Abbreviations PV NF OD MC RO MD

Pervaporation Nanofiltration Osmotic distillation Membrane contactor Reverse osmosis Membrane distillation

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60. Alcantara, B.M., Marques, D.R., Chinellato, M.M., Marchi, L.B., da Costa, S.C., et al., 2016. Assessment of quality and production process of a non-alcoholic stout beer using reverse osmosis. J. Inst. Brew. 122 (4), 714
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412. Available from: https://doi.org/10.1556/AAlim.2010.0001. Trejo, L., Limones, V., Pen˜a, G., Scheinvar, E., Vargas-ponce, O., Zizumbo-villarreal, D., et al., 2018. Genetic variation and relationships among agaves related to the production of Tequila and Mezcal in Jalisco. Ind. Crops Prod. 125 (January), 140
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105. Available from: https://doi.org/10.1002/jib.197. Wedel Falkenberg, A., 2014. Removal of Alcohol From Beer Using Membrane Processes. University of Copenhagen, Copenhagen. Weiss, M., 1987. Verfahren zum herabsetzen des alkoholgehalts alkoholhaltiger getra¨nke, insbesondere wein und schaumwein. German Federal Republic Patent DE, 34, 13 085 C2. WHO, 2011. Global Status Report on Alcohol and Health. WHO, Geneva. Wucherpfenning, K., Von, K., Millies, K.D., Christmann, M., 1986. Hestellung entalko- hololisierter weine unter besonderer beru¨cksichtigung des dialyseverfahrens. Die Weinwirtsch. Tech. 122, 346
354. Xu, Y., Fan, W., Qian, M.C., 2007. Characterization of aroma compounds in apple cider using solvent-assisted flavor evaporation and headspace solid-phase microextraction. J. Agric. Food Chem. 55, 3051
3057. Available from: https://doi.org/10.1021/jf0631732. Ye, M., Yue, T., Yuan, Y., 2014. Changes in the profile of volatile compounds and amino acids during cider fermentation using dessert variety of apples. Eur Food Res. Technol. 239, 67
77. Available from: https:// doi.org/10.1007/s00217-014-2204-1. Zhao, D., Lau, E., Huang, S., Moraru, C.I., 2015. The effect of apple cider characteristics and membrane pore size on membrane fouling. LWT Food Sci. Technol. 64 (2), 974
979. Available from: https://doi.org/ 10.1016/j.lwt.2015.07.001. Zhao, D., Lau, E., Padilla-zakour, O.I., Moraru, C.I., 2017. Role of pectin and haze particles in membrane fouling during cold micro fi ltration of apple cider. J. Food Eng. 200, 47
58. Available from: https://doi. org/10.1016/j.jfoodeng.2016.12.020. Zufall, C., Wackerbauer, K., 2000. Verfahrenstechnische Parameter bei derEntalkoholisierung von Bier mittels Fallstrom-verdampfung und ihr Einfluß auf die Bierqualita¨t. Monatsschr. Brauwiss. 10, 163.

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CHAPTER 6

Nonalcoholic Beer ¨zel, Mustafa Gu ¨zel and K. Sava¸s Bahc¸eci Nihal Gu Department of Food Engineering, Hitit University, C ¸ orum, Turkey

Chapter Outline 6.1 Introduction 167 6.2 Chemical and Sensorial Properties 171 6.3 Production of Nonalcoholic Beer 174 6.3.1 Biological Methods 175 6.3.2 Physical Methods 181 6.3.3 Other Methods 191

6.4 Conclusion 192 References 193 Further Reading 200

6.1 Introduction Beer is one of the oldest beverages. Recent archeological evidence found in Raqefet Cave, Israel has revealed that beer was known as early as 11,000 BCE (Liu et al., 2018). Similar studies have indicated that beer was known in China for 9000 years (Bai et al., 2011). Apart from the historical importance of being the oldest biotechnological product, beer was very important for civilization because it is nutritious and nonperishable. Considering the climate of the Middle East, for example, beer offered a safe beverage, not only because of ethanol, but also because of the organic acids it produces spontaneously (Renneberg et al., 2016). In addition, the antimicrobial compounds from hop, its low pH value, and competitive microflora made beer safe. Beer is also one of the most popular alcoholic beverages in the world, with a production of nearly 2 billion hectoliters per year (Mertens et al., 2015). As a group, beer is the second-most consumed alcoholic beverage in the world after spirits, and the most consumed in the

Trends in Non-alcoholic Beverages. DOI: https://doi.org/10.1016/B978-0-12-816938-4.00006-9 © 2020 Elsevier Inc. All rights reserved.

167

168 Chapter 6 Americas and Europe (World Health Organization, 2014). Studies show that beer consumption has increased steadily in the past 50 years, even though a decrease in consumption has been observed in traditionally beer-producing countries. The primary reason for the overall increase may be associated with the increased consumption in traditionally spirit-drinking countries such as China and Russia (Colen and Swinnen, 2016). Traditionally, beer has four basic ingredients: barley, yeast, hop, and water. The German Purity Law, dating back to 1516, stated that beer can only be made from barley, water, and hop (Stewart, 2016). Although the purpose of the law was to protect bakers by prohibiting wheat and other premium grains being used in beers production, a tradition started. Today, various kinds of adjuncts of more than 30% of the total recipe can be added for sensory characteristics and cost reduction (Pires and Bra´nyik, 2015). Despite the short recipe list, choosing the right ingredients for beer requires craftsmanship. For example, the quality of the end product is affected by calcium ions in the water used (Narziss et al., 1992). Similar considerations are also true for other ingredients. Although other grains (e.g., wheat, rye) are also used in different kinds of beer, traditionally barley is the main sugar source for yeast. Generally, two-row barleys are preferred by brewers because a higher level of malt can be extracted (Schwarz and Horsley, 1996). For a good quality beer, the germination capacity and the protein and moisture content are essential, and need to be analyzed before malting. Hops, although not a main portion of beer by weight, contributes the aroma, specifically the distinct bitterness (Wunderlich and Back, 2009; Scho¨nberger and Kostelecky, 2011). There are two main types of hops: bitter hops and aroma hops. The difference comes from the α-acid and essential oil content; while bitter hops have higher α-acid, aroma hops have richer essential oil contents (Pires and Bra´nyik, 2015). Different yeast types are used for different kinds of beers. Traditionally, yeasts from Saccharomyces genus are used in beer production. Understanding the yeast behavior is essential in brewing. More emphasis is given to yeasts in the “special yeast” section. In brief, yeast should be in good condition, and should have a high viability and vitality (Wunderlich and Back, 2009). In addition to the ingredients, all of the production steps directly impact on the quality. A significant number of different beers are available commercially. The variation among the different types is due to process, yeast, ingredients, and flavor. Today, lager beers account for more than 90% of total beer production (Pavsler and Buiatti, 2009). There are a lot of subtypes of lager beer, while pilsner is the most popular. Ales, although having a very small market share compared to lagers, are still highly common in several regions such as Britain and Belgium. The main difference between ales and lagers is related to the fermentation. While ales are top fermented beers, lagers are bottom fermented. The beer making process involves a number of operations (Fig. 6.1). Production starts with the malting of grain. Barley in grain form is not suitable for brewing. Malting, which involves several steps, is basically the controlled/artificial germination of barley. After germination, the moisture content is reduced and enzymes are deactivated by a high-temperature step,

Nonalcoholic Beer 169 Barley Malting -Steeping -Germination -Kilning

Malting

Milling

Mashing

Lautering

Boiling

Hop

Yeast Brewing

Whirlpooling

Cooling/fermentation

Maturation

Filtaring/stabilizing

Packaging

Prefermentative

Fermentative

Postfermentative

Figure 6.1 Flow chart of the malting and brewing process of beer production. Adapted from Wunderlich, S., Back, W., 2009. Overview of manufacturing beer: ingredients, processes, and quality criteria. In: Beer in Health and Disease Prevention. Academic Press, pp. 3
16; Riu-Aumatell, M., Miro´, P., Serra-Cayuela, A., Buxaderas, S., Lo´pez-Tamames, E., 2014. Assessment of the aroma profiles of low-alcohol beers using HS-SPME
GC-MS. Food Res. Int. 57, 196
202.

that is, kilning. The kilning step not only stabilizes the malt until brewing, but also determines the color of the final product (Wunderlich and Back, 2009). The malt is then milled and taken into mashing tanks. Mashing is the process through which malt turns into “wort.” In the mashing process, malt is mixed with other grains, adjuncts (if necessary), and water under a high temperature. This operation turns the starch in malt into fermentable sugars due to amylase (i.e., α-amylase and β-amylase) activity. Then the slurry is filtered and boiled with hops (Pires and Bra´nyik, 2015). A yeast culture is then inoculated into wort and starts the fermentation process. The duration and temperature of the fermentation are determined by the type of beer. In lager beers, there are two fermentation steps; primary fermentation (8 C
15 C) and secondary fermentation/ maturation (
1 C to 4 C) (Pavsler and Buiatti, 2009). Finally, the beer is pasteurized or filtered, thus stabilizing the product and increasing its shelf-life. The relationship between beer and health is complex and multidimensional, thus it is very hard to depict comprehensively. Until recently there was a consensus that light or moderate

170 Chapter 6 consumption of beer did not cause health problems. Furthermore, light consumption of beer had health benefits against cardiovascular disease (De Gaetano et al., 2016). For example, in a study performed in Germany, it was found that beer shows a protective effect against coronary heart disease (Brenner et al., 2001). Volpe et al. (2016) stated that consuming alcohol has a protective effect on health, compared to not consuming alcohol at all. McCullough and Volpe (2017) argued that as long as it was consumed by adults in moderate amounts, beer might be a part of a healthy diet. However, a comprehensive report by the Global Burden of Disease showed that even low to moderate consumption of alcohol causes health problems (Griswold et al., 2018). Alcohol consumption was the seventh leading cause of death and disability-adjusted-life-years (DALYs) in all age groups. An even more striking finding was that the use of alcohol was the leading cause of death and DALYs for the population aged 15
49 years. The minimization of health risks for all age groups can be achieved by not consuming alcoholic drinks at all (Griswold et al., 2018). Craft beers and specialty beers have been gaining popularity over the past few decades (Yeo and Liu, 2014; Donadini and Porretta, 2017). These types of beers have emerged in microbreweries, and are produced by various brewing methods (Madsen, 2017). Nonalcoholic (NA) beer can also be classified as a specialty beer along with low-calorie beer, low-alcohol beer, gluten-free beer, and novel flavored beer (Yeo and Liu, 2014). NA beer is defined differently by the European Union (EU) and the United States (Table 6.1). In the EU, beer can generally be called alcohol-free beer if it contains less than 0.5% alcohol by volume (ABV), whereas in the United States, there must be zero alcohol in a beer for it to be called an alcohol-free beer (Liguori et al., 2015a). There are a few exceptions in the EU; two of them are Spain and the United Kingdom where alcohol-free beer is defined as having 1% and 0.05% ABV, respectively (Montanari et al., 2009). Table 6.1: Selected exceptional data relating to alcohol content in beer for different countries. Country Austria Denmark Finland France The Netherlands Norway Spain Sweden The United Kingdom The United States

Light Beer (ABV, %)

Low-Alcohol Beer (ABV, %)

# 3.7

0.1
1.9

Nonalcoholic Beer (ABV, %) , 0.1

2.8 0.1
1.2 1
3 2.2 # 1.2 2.5

# 1.2 # 0.1 # 0.7 ,1 # 0.05 No alcohol

Source: Montanari, L., Marconi, O., Mayer, H., Fantozzi, P., 2009. Production of alcohol-free beer. In: Beer in Health and Disease Prevention. Academic Press, pp. 61
75; Mu¨ller, M., Bellut, K., Tippmann, J., Becker, T., 2017. Physical methods for dealcoholization of beverage matrices and their impact on quality attributes. ChemBioEng Rev. 4 (5), 310
326; Liguori, L., Russo, P., Albanese, D., Di Matteo, M., 2018. Production of low-alcohol beverages: current status and perspectives. In: Food Processing for Increased Quality and Consumption, pp. 347
382.

Nonalcoholic Beer 171 Similarly, the Netherlands and Denmark define alcohol-free beer as containing less than 0.1% ABV. In Islamic countries, alcohol-free beer refers to beer containing zero alcohol (Liguori et al., 2018). In this chapter, NA beer refers to alcohol-free beer. Based on a study conducted in three European countries, consumers prefer specialty beers due to their innovative, authentic, and creative nature, even though this kind of beer is pricier than industrial lager beer (Donadini et al., 2016). As a specialty beer, NA beer has also had a steadily increasing market share in recent years (Jiang et al., 2017). The antioxidant, antiinflammatory, antibacterial, and anticarcinogenic properties of beer have been well studied (Imhof et al., 2004; Chen et al., 2014; Sohrabvandi et al., 2011). All of these properties can be associated with NA beer as they are not ethanol related. While the increasing health awareness is the main reason for this increased market share, other healthrelated issues such as pregnancy and weight issues also responsible for the increasing consumption (Liguori et al., 2018). NA beer has a lower calorie content than regular beer. Since there are no adverse effects of alcohol, NA beer is safe to consume before driving or operating machines (Thierauf et al., 2010). Besides, NA beer is an alternative beverage in countries where the use of alcohol is very low due to religious reasons (Bra´nyik et al., 2012). Indeed, NA beer production has improved significantly, and has reached 2.2 billion liters, which is more than 80% of the amount produced 5 years ago (Liguori et al., 2018). However, even though the production of NA beer has been increasing, it is still hard to tell whether NA beer has been fully accepted by consumers. There is a negative consumer perception toward low-alcohol content and NA beer because of the flavor difference compared to regular beer (del Olmo et al., 2014). Ethanol is one of the key aroma constituents of beer. The absence of ethanol solely changes the sensorial characteristics. Furthermore, depending on the production method, other off-flavors may be created. For instance, caramelization, loss of volatile compounds, and color change might be observed in temperature-based dealcoholization methods (Montanari et al., 2009). Beer has a long and rich history. Although it can be made from only four ingredients with a simple process, making a satisfactory beer requires a good understanding of the components and operations. Although there are a number of studies that favor the beneficial health effects of moderate beer consumption, consumers increasingly prefer NA beer due to health awareness. Therefore there is constant effort to produce good quality NA beer. With the rapid advancements in technology, there are new possibilities in NA beer production. In this chapter, trends in the production of NA beer are discussed.

6.2 Chemical and Sensorial Properties The sensorial quality of a beer depends on the ingredients used (e.g., barley, hop), and these are developed throughout the brewing process. Beer is a complex mixture of volatile and

172 Chapter 6 nonvolatile compounds, all of which together create the unique sensorial characteristics of beer. Hundreds of compounds are formed during fermentation. Volatile compounds in beer include, but are not limited to, alcohols, aldehydes, acids, esters, phenols, alicyclic and heterocyclic compounds, and ethers (da Silva et al., 2015). Most of these compounds affect the aroma, either individually or in combination with other compounds. While some compounds contribute to the aroma majorly, others can be assessed as background flora (RiuAumatell et al., 2014). For instance, amyl alcohols (3 and 2-methyl-1-butanol) contribute to alcoholic, banana, sweet, malty, or vinous flavors in beer and NA beer. Also, 2-phenyl ethanol is responsible for alcoholic, flowery, honey-like, rose, and sweet flavors (Verstrepen et al., 2003). The total ester concentration is an important factor associated with sweet and fruity flavors in beer. Aldehydes are responsible for fresh and grassy flavors (Sampranpiboon et al., 2000). The importance of the different flavor components in beer is determined by their organoleptic threshold values, defined as the minimum amount of a compound added to beer to change the flavor of the beer significantly. Different flavor compounds and their threshold values for regular beer are expressed in Table 6.2. The concentrations of valuable aroma components generally decrease to below their threshold values during dealcoholization, so NA beers are widely described as low aromatic in flavor (Mu¨ller et al., 2017). The sensory characteristics of NA beer clearly differ from those regular beer. First and foremost, one of the main aroma compounds, ethanol is absent in NA beer. The changes in selected volatile compounds of commercial low- and alcohol-free beers as compared with regular beer (as percentage amount) are shown in Table 6.3. Alcoholic compounds (isobutanol, isoamyl alcohol, 2-phenylethanol, decanol, 1-heptanol) and esters (isoamyl acetate, ethyl hexanoate, ethyl acetate, ethyl octanoate) were found in regular beers in higher quantities, while furfural, linalool oxide, benzaldehyde, phenylethyl isobutyrate, and 2-acetylpyrrole were quantified as higher in NA beer. In addition to losing major aroma components, off-flavor compounds might be formed depending on the production. For instance, beer production using biological methods may result in a sweet off-flavor, whereas thermal processes may result in a caramel-like taste caused by heat, and membrane-based dealcoholization may result in a lack of aroma and body (Montanari et al., 2009; Bra´nyik et al., 2012). The body of beer and mount feeling properties relate closely to production methods. For instance, the body of beer produced by thermal processes is described as “empty” or as “lacking body” due to the lack of ethanol or residual sugar content. Also, higher thermal stress can cause undesirable flavor changes such as a “honey-like” or “caramel-like” flavor (Mu¨ller et al., 2017). Unlike the caramel aroma that occurs when a thermal process is used, beers can be gently dealcoholized by thermal and membrane process combinations without any off-flavor occurring (Montanari et al., 2009). Therefore today most studies are focused on the effects of the production method on the aroma profile of beer. The sensory quality of NA beer can be enriched by pre- and posttreatments. For instance, a flavor concentrate can be used for reblending for additional aroma. The addition of aroma concentrates captured during pervaporation and rectification might also increase the

Table 6.2: Different flavor compounds in regular beer and flavor threshold levels. Flavor Threshold (mg/L)

References

Alcoholic, strong Alcoholic, solvent Alcoholic Alcoholic Alcoholic, banana, medicinal, solvent, fruity Alcoholic, banana, sweetish, aromatic Roses, sweetish, perfumed Fresh cut grass, perfumed Coconut, aniseed Sweetish, viscous Bitter, chemical

14,000 2 20,000 10,000 800 200 65

Cortacero 2 Ramirez et al. (2003) Cortacero 2 Ramirez et al. (2003) Kobayashi et al. (2008) Kobayashi et al. (2008) Kobayashi et al. (2008)

70

Kobayashi et al. (2008)

125 0.2 0.015 2 200

Kobayashi et al. (2008) Cortacero 2 Ramirez et al. (2003) Cortacero 2 Ramirez et al. (2003) Cortacero 2 Ramirez et al. (2003) Cortacero 2 Ramirez et al. (2003)

Solvent, sweetish, fruity

21 2 30

Solvent, banana, apple, pear, esterlike Roses, sweetish, apple, honey

0.6 2 1.2

Kobayashi et al. (2008); Verstrepen et al. (2003) Verstrepen et al. (2003)

Ethyl caproate

Sour apple

0.17 2 0.21

Ethyl caprylate

Sour apple

0.3 2 0.9

Grassy, green leaves, fruity

25

Kobayashi et al. (2008)

Butter Honey, toffee-like

0.15 1.0

Kobayashi et al. (2008) Willaert and Nedovic (2006)

Goaty Goaty Waxy, rancid

14 8 10

Verbelen and Delvaux (2009) Verbelen and Delvaux (2009) Verbelen and Delvaux (2009)

Compounds

Flavor Description

Alcohols Ethanol Methanol n-Propanol Isobutyl alcohol (2-methyl propanol) Amyl alcohol (2-methylbutanol 1 3
methylbutanol) Isoamyl alcohol (3-methyl butanol) 2-Phenyl ethanol 1-octen-3-ol 2-Decanol Glycerol Tyrosol Esters Ethyl acetate Isoamyl acetate 2-Phenyl acetate

3.8

Kobayashi et al. (2008), Verstrepen et al. (2003) Kobayashi et al. (2008), Verstrepen et al. (2003) Kobayashi et al. (2008), Verstrepen et al. (2003)

Aldehydes Acetaldehyde Ketones 2,3-Butanedione (diacetyl) 2,3-Pentanedione Organic and fatty acids Caprylic Caproic Capric

174 Chapter 6 Table 6.3: Selected aroma profile of commercial low alcohol and nonalcoholic beer as compared to regular beer. Compoundsa Ethyl acetate Hexanal Isobutanol Isoamyl acetate Heptanal Isoamyl alcohol Ethyl hexanoate 2-Methylpyrazine 1-Octanal 2-Octanol Ethyl octanoate 1-Heptanol Decanol Phenylethyl butyrate Phenylethyl isobutyrate 2-Phenylethanol 2-Acetylpyrrole 5-Methylfurfural Benzaldehyde Decanal Linalool oxide Furfural

Low-Alcohol Beer ,3 (% ABV)

Nonalcoholic Beer ,1 (% ABV)


52 12
74
81 1 0.02
68
88 Nq 1 0.08 1 0.15
97
5
94 Nq 38
98 Nq 1 0.24 1 63 Nq Nq 1 57


84 12
92
80 1 0.03
82
88 1 0.14 1 0.05 1 0.08
95
68 Nq 12 46
99 1 0.09 1 0.13 1 84 1 0.01 1 0.09 1 75

Nq, Not quantified. a Presented as a percentage change of selected properties. Source: Riu-Aumatell, M., Miro´, P., Serra-Cayuela, A., Buxaderas, S., Lo´pez-Tamames, E., 2014. Assessment of the aroma profiles of lowalcohol beers using HS-SPME
GC-MS. Food Res. Int. 57, 196
202.

sensorial quality (Mu¨ller et al., 2017). The addition of regular beer or krausen might increase the sensorial quality. Blending NA beer with krausen (6% ABV) increases the level of ethanol and ethanol-related volatiles, and thus results in a better flavor (Narziss et al., 1992). However, this correction may increase the ethanol content over the legal limits in the final product. In some cases, the use of additives including lactic acid, ascorbic acid, saccharin, and citric acid for various purposes has also been reported (Bra´nyik et al., 2012). Factors other than chemical composition such as foam stability, CO2 and O2 content, and turbidity also affect consumer acceptance, and thus they should not be overlooked in the production of NA beer (Liguori et al., 2015a). In addition, the color of NA beer may be affected by the dealcoholization process.

6.3 Production of Nonalcoholic Beer The production of NA beer is not distinct from regular beer. It is produced from the same materials, that is, malt, water, yeast, and hop. The quality of the ingredients directly affects the final product. The processes of NA and regular beer are almost identical.

Nonalcoholic Beer 175 Limited fermentation Biological

Special yeast

NA beer production methods

Altered mashing Rectification Thermal Evaporation Dialysis Physical

Reverse osmosis Nanofiltartion Membrane based Membrane distillation Osmotic distillation Pervaporation

Figure 6.2 Production methods of NA beer.

The production of NA beer can be fundamentally divided into two; biological (fermentation) and physical (postfermentation) methods (Fig. 6.2). The effect of these methods on the chemical composition of the final product varies significantly (Table 6.4). While biological methods rely on special yeasts or modifications in operational parameters (e.g., time and temperature), physical methods add an extra “dealcoholization” step to the process (Bra´nyik et al., 2012).

6.3.1 Biological Methods Biological NA beer production is a broad term and simply refers to controlled fermentation. Several methods are covered in biological production including the use of special yeasts, mash alteration, and limiting the fermentation capacity of the yeast. The biggest advantage of these methods is probably that they can be carried out in traditional breweries without special equipment. Thus biological methods do not require an extra investment. Furthermore, Roman et al. (2017) stated that consumers’ perceptions are influenced by the naturalness of food. From this point of view, one less process might create a positive consumer perception. 6.3.1.1 Limited Fermentation Limited fermentation, in principle, refers to controlling the yeast’s ability to utilize wort by changing the process conditions. Based on the alteration made in the fermentation process,

Table 6.4: Selected quality parameters for different dealcoholization methods of beer.

Color (EBC)

Turbidity (IBC)

Original Gravity (wt.%)

pH

Ethanol (% ABV)

Higher Alcohol (mg/L)

Aldehydes (mg/L)

Esters (mg/L)

31.2

7.00

0.3

11.57

4.52

5.04

100 2 300

30 2 40

25 2 40

Buiatti (2008); Montanari et al. (2009)

Falling film

28.7

7.75

2

4.54

4.7

0.51

3.8

1.6

, 0.1

9.5

2.3
1.2

5.16

4.71

30.0

8.97

0.73

6.21

4.4 2 4.63

0.02

6.5

2.17

2.7

Montanari et al. (2009) Montanari et al. (2009); Bra´nyik et al. (2012); Andres-Iglesias et al. (2015a)) Catarino (2010); Catarino and Mendes ¨ller et al. (2011a); Mu (2017)

Rectification

25.5

SCC

Dialysis

29.7

7.5

2

4.53

4.68

0.47

2.7

3.7

, 0.1

OD

13 (BU)

8.4

4.41

4.16

0.46

19.12

0.91

0.20

Pervaporation

32.0

10.8

1.7 (EBC) 2

6.70

4.7

0.45

10.82

2.37

2.07

RO

12.3

175.7
227.6

2

2.48

4.2 2 4.4

0.40

0 2 60.2

2

0.6 2 8.0

NF

2

2

2

2

2

0.4

27.9

2

2

Catarino (2010); Mu ¨ller et al. (2017) Kavanagh et al. (1991); Alcantara et al. (2016); Paz et al. (2017) Kavanagh et al. (1991)

Limited fermentation Special yeast

17.4 2 25.4

5.6 2 8.4

2

2.2 2 15.8

2

0.55 2 0.90

Narziss et al. (1992)

2

7.20

67.60

43.31

4.7

14.91

De Francesco et al. (2015b)

Regular beer

Bitterness (EBC)

Reference

Dealcoholization methods Thermal methods

Membranebased methods

Biological methods

0.02 2 0.03 65.37 2 97.8 0.53 2 2.81

7.4 2 11.4 4.87 2 5.01 0.27 2 0.42 12.01 (kg/hL)

5.57

0.51

EBC, European Brewery Convention; IBC, International Bitterness Unit; wt.%, percent in weight; %ABV, alcohol by volume.

0.04

Montanari et al. (2009); Bra´nyik et al. (2012) Liguori et al. (2015a)

Nonalcoholic Beer 177 limited fermentation can be further subcategorized into two groups, namely limited and stopped fermentation methods. For both, the main methods are based on controlling the fermentation process by altering the process temperatures or by removing yeast. In limited fermentation, the activity of the yeast is reduced, whereas in stopped fermentation, the yeast is removed before attenuation (Montanari et al., 2009). In either case, accurate control throughout the fermentation process is needed (Bra´nyik et al., 2012). The attenuation of yeast is interrupted by the removal of the yeast in stopped fermentation (Montanari et al., 2009). The process can be stopped by either reducing the temperature to 0 C, through pasteurization, or by removing the yeast via filtration or centrifugation. However, high temperatures, above pasteurization level, may damage the flavor by causing the loss or degradation of volatile compounds; therefore, decreasing the temperature might be better in terms of quality (Sohrabvandi et al., 2011). To produce NA beer with arrested fermentation, the formation of a “worty” flavor must be taken into account. If wort with 9 P
13 P gravity is used, a strong off-flavor associated with the nonreduced aldehydes is formed (Bra´nyik et al., 2012). In limited/arrested fermentation, achieving low-alcohol levels, facilitating the formation of flavor-active compounds, and the removal of undesirable substances are not easy. Concerning the formation of volatile compounds, cachaca strain 101.8 has the advantage of a higher total ester content as compared traditional lager from strain 2 (Puerari et al., 2016). In a study, the effect of several fermentation parameters on the quality of NA beer was determined (Mortazavian et al., 2014). Saccharomyces species was tested under different inoculum levels, fermentation temperatures, and aeration conditions. A sensory panel with six trained panelist showed that fermentation at 4 C and partial aeration of Saccharomyces cerevisiae with 107 cfu/mL inoculation had the best result in terms of sensory profile (Mortazavian et al., 2014). An alternative method to limited fermentation, “cold contact process” (CCP) is carried out under reduced temperatures and long fermentation times. In CCP, hardly any ethanol is produced, while other chemicals such as esters and high alcohols are formed moderately. In this process, a high concentration of yeast is used ( . 108 cells/mL), resulting in a thick yeast slurry (Montanari et al., 2009). 6.3.1.2 Special Yeast The history of beer is almost as old as agriculture. Beer has been produced intentionally or unintentionally (i.e., spontaneously) through the fermentation of grains since then. As a main component of beer, yeast determines the characteristics of the end product (Pires et al., 2014). S. cerevisiae, a predominant species in ale production, has been utilized for millennia. Saccharomyces pastorinaus, a hybrid yeast that is an interspecies of S. uvarum and S. cerevisiae, has been used for lager beer for centuries (Nakao et al., 2009). Today,

178 Chapter 6 due to advances in molecular methods, the evolution and lineage of the yeasts used in brewing are known (Walther et al., 2014; Baker et al., 2015). The utilization of nonconventional or “special” yeasts shows promising advancements, and might be considered as a trending topic in NA beer. Special strains can produce byproducts that develop aroma, while using the wort sugars partially, thus resulting in low amounts of ethanol in the final product (Basso et al., 2016). The production of NA beer using special strains includes two distinct approaches: (1) the use of genetic modifications to the yeast such as deletion/silencing of certain genes; and (2) considering special strains that cannot ferment maltose. Torulaspora delbrueckii, an abundant yeast in the environment, is found in the spontaneous fermentations of beer and wine, and has been known and used for millennia (van Breda et al., 2013; Albertin et al., 2014). T. delbrueckii has emerged because of its ability to enhance flavor and produce low-alcoholic beer (Canonico et al., 2016). This yeast shows invertase activity, meaning that it can utilize sucrose by hydrolyzing it into glucose and fructose. However, the ability of maltose utilization depends on the strain (Michel et al., 2016a). The yeast is able to tolerate ethanol, and hop-related antimicrobial activity, both of which are desirable traits (Varela, 2016). Saccharomycodes ludwigii is a special species that causes spoilage in the winemaking process (Vejarano, 2018). However, S. ludwigii lacks the enzymes invertase and maltase, and hence, cannot ferment maltose, the main sugar in wort. In fact, S. ludwigii has been utilized commercially for a long time (Capece et al., 2018). In a similar fashion, Zygosaccharomyces rouxii lacks the mentioned enzymes, and can only partially ferment maltose. The utilization of this yeast has been proposed, and studied in a number of studies (Narziss et al., 1992; Sohrabvandi et al., 2009; Liu et al., 2011; De Francesco et al., 2015b). Narziss et al. (1992) used an S. ludwigii strain to produce NA beer. After 120 h of fermentation at 20 C, the resulting product had a 0.68% ABV content. In a more recent study, Liu et al. (2011) utilized S. ludwigii and achieved 0.47% ABV, which is in the NA limit, and thus can be considered as an NA beer. S. ludwigii is a slowly attenuated yeast, which results in a longer fermentation time without the special need for continuous monitoring. De Francesco et al. (2015a) tested several strains of Z. rouxii and S. ludwigii in the production of NA beer. The final product with Z. rouxii had a 0.93% or more ethanol by volume content, and higher levels of off-flavor-causing compounds such as diacetyl. On the other hand, a 10 day fermentation at 20 C with S. ludwigii resulted in 0.5%
0.7% ethanol by volume levels. In addition, the final products had higher levels of esters and lower levels of diacetyl with S. ludwigii compared to Z. rouxii (De Francesco et al., 2015a). The Mrakia genus has several species that are able to ferment glucose and produce ethanol (De Francesco et al., 2018). Thomas-Hall explored the possibility of utilizing the Mrakia species in beer production (Thomas-Hall et al., 2010). Similar to other non-Saccharomyces

Nonalcoholic Beer 179 species, Mrakia gelida strain partially ferments wort, resulting in low-alcohol beer. A psychrophilic strain of M. gelida has been used to produce beer at pilot scale, and the results were compared with the beer produced by S. ludwigii. The beers had similar alcohol levels (1.40% and 1.32%) and diacetyl contents (5.04 and 5.20 μg/L) for M. gelida and S. ludwigii, respectively. The authors stated that the M. gelida beer showed a better sensory profile than that of S. ludwigii (De Francesco et al., 2018). With some modifications (e.g., limited fermentation) Mkrakia species might be utilized in NA beer production. There are also trials on the utilization of strains from Brettanomyces, Scheffersomyces shehatae (Candida shehatae), Pichia kluyveri, and Wickerhamomyces anomalus (Michel et al., 2016b; Saerens and Swiegers, 2017; Capece et al., 2018). For example, Estela-Escalante et al. (2016) used Candida zemplinina to produce craft beer. The ethanol production of C. zemplinina was lower than that of S. cerevisiae, which indicates the potential utilization of this yeast in NA beer production. Besides, C. zemplinina was able to maintain a higher viable cell count, and grew better than S. cerevisiae did in the test medium (Estela-Escalante et al., 2016). In addition to nonconventional yeasts, the utilization of fungi has also been proposed. Lin et al. (2005) used a strain from the Monascus genus and produced a drink that resembles NA beer. Although the drink was refreshing and had high levels of antioxidant capacity, it is questionable to call it beer (Bra´nyik et al., 2012). Saccharomyces boulardii, a probiotic strain of S. cerevisiae, has potential in the production of NA beer as an alternative yeast (Senkarcinova et al., 2019). The yeast is able to grow at very low temperatures (2 C), and is resistant to ethanol at regular beer levels. However, the yeast is also able to utilize wort sugars at 2 C, meaning that the yeast continues to ferment after the brewing process, and ultimately, the ethanol level exceeds the allowed level for NA beer. To overcome this obstacle, mash would have to be altered by the inactivation of β-amylase at high temperatures, or the yeast metabolism would have to be inactivated. A promising method might be using high hydrostatic pressure (HHP) as a pasteurization method. HHP not only inactivates yeast, but also causes limited changes in the constituents of beer, compared to heat pasteurization. Furthermore, even dead cells show probiotic effects. As a result, from a marketing point of view, one of the biggest advantages of NA beer would be that the health benefits would be further enhanced by probiotics (Senkarcinova et al., 2019). Non-Saccharomyces yeasts have also been increasingly tested in specialty beers. For most species, the fermentation efficiency and ethanol tolerance are lower than in conventional yeasts (Basso et al., 2016). For example, many different yeast species and lactic acid bacteria are used in the production of sour beer including but not limited to Lachancea fermentati, Hansenia spora, Schizosaccharomyces japonicus, and W. anomalus (Osburn et al., 2018). The flavor enhancing capabilities of nonconventional yeast strains have been

180 Chapter 6 tested (Holt et al., 2018). They might be used in NA and low-alcohol beers due to their pleasant flavors. Liu and Quek (2016) used Williopsis saturnus var. mrakii to produce low-alcohol beer with an extra fruity aroma. The end product had a higher acetate ester concentration compared to beer produced using S. cerevisiae. Considering the fact that craft beers and microbreweries are widely popular, efforts toward the utilization of nonconventional yeasts as flavor enhancers in NA beers will be continued (Liu and Quek, 2016). Genetically modified (GM) yeast suffers from a negative consumer perception, and thus has not been commercially tested. In general, GM studies involve specific mutants that lack a gene or genes in the ethanol production pathway. For instance, the last step of fermentation is the conversion of acetaldehyde to ethanol by the alcohol dehydrogenase (ADH) enzyme. A mutant strain that lacks ADH genes was able to produce NA beer successfully, but the acetaldehyde content of the end product caused an unpleasant off-flavor (Dziondziak and Holsten-Brauerei, 1989). In a study, the use of GM strains resulted in high amounts of diacetyl and acetoin, both of which cause off-flavors (Nevoigt et al., 2002). In another approach, several strains with deficiencies were used in the production of NA beer. FUM1, KGD1, and KGD2 lacking mutants were able to produce alcohol-free beer with 0.48%, 0.42%, and 0.48% ethanol contents, respectively. These mutants produced more lactic acid, which reduced the contamination risk and worty off-flavors. However, the diacetyl content was increased, which is an undesirable trait (Selecky´ et al., 2008). There is great potential in this field, and with time GM yeasts will most probably be used for the production of NA beer commercially. With new metagenomics studies like population dynamics, a much better understanding of microbial ecology during fermentation has been obtained (Varela and Varela, 2019). Furthermore, with the recent developments in genomic engineering such as CRISPR/Cas technology, studies and applications of conventional and nonconventional yeasts have advanced rapidly, and show great potential (Lo¨bs et al., 2017; Stovicek et al., 2017). Therefore using different species with similar characteristics, or making genetic changes in current species is an emerging production method in NA beer.

6.3.1.3 Altered Mashing Mashing is one of the main steps in beer production in which the starch is degraded into fermentable sugars with the help of enzymes. Specifically, α-amylases hydrolyze starch into fermentable sugars and dextrin, and β-amylases further degrade dextrin into maltose. This process determines the fermentability of wort and changes in the mashing process can reduce the utilization of sugars, thus resulting in less ethanol production. The changes might be: 1. The inactivation of β-amylase: The inactivation of this enzyme can be achieved in elevated temperatures (75 C).

Nonalcoholic Beer 181 2. The extraction of malt in cold water: With this method, wort with good flavor compounds but less gravity than usual can be obtained. 3. Remashing with a second extract: This method can be applied by the addition of partially fermentable extracts such as rice. 4. Using β-amylase deficient barley varieties. However, mash altering alone may not be sufficient for the production of a good quality NA beer, thus it must be combined with other methods (Bra´nyik et al., 2012).

6.3.2 Physical Methods Various physical methods are applied for separating alcohol from regular beer for different quality low or NA beer production. Physical methods, also called dealcoholization methods, are based on thermal or membrane processes. Ideally, a dealcoholization method should remove ethanol without affecting the other beer constituents. However, each technique applied at lab or industrial scale has its own advantages and drawbacks. 6.3.2.1 Thermal Methods Most conventional methods of dealcoholization in the past have focused on thermal base processes because ethanol is more volatile compared to water. Distillation at atmospheric pressure is the most common and simple method for thermal dealcoholization (Montanari et al., 2009). Alcohol can be removed completely from beer by heating processes. Until the end of the 1970s, various studies have been published on thermal dealcoholization by distillation (Mu¨ller et al., 2017). Thermal dealcoholization methods also have eligibility in terms of continuous and automatic operation. However, thermal processes have some considerable drawbacks such as high energy requirements and the thermal degradation and loss of some volatile substances due to the elevated temperatures used (Bra´nyik et al., 2012; Mangindaan et al., 2018). Nowadays, the production of dealcoholized beer at the industrial scale is carried out under vacuum (rectification and evaporation) to reduce thermal stress on the organoleptic properties (Andres-Iglesias et al., 2015a). Rectification

Conventional distillation has been replaced with rectification (distillation under vacuum) for preventing thermal damage to the taste and color of beer. Rectification is considered as one of the most economic dealcoholization processes among the physical methods (AndresIglesias et al., 2015a). Modern continuous vacuum distillation (rectification) equipment basically consists of a plate heat exchanger, a degasser, a rectification column, and a cooler (Liguori et al., 2018). Rectifying processes generally occur in a packed bed rectifying column. Before feeding into the stripping section of a rectifying column, beer is degassed and preheated with a plate heat exchanger. Simultaneously, volatile compounds and CO2 in

182 Chapter 6 the beer are released into a vacuum degasser (Bra´nyik et al., 2012). In a rectification system, vacuum is applied generally between 4 and 20 kPa and the beer is evaporated at mild temperatures (30 C
60 C) in order to decrease the thermal stress on the beer (Sohrabvandi et al., 2009; Liguori et al., 2018). After the dealcoholized beer is passed through a cooler, the vapors rich in alcohol are concentrated in the rectification section and the aroma components are recovered and redirected to the beer (Montanari et al., 2009). A significant loss of beer flavor and body may occur during thermal processes due to the fact that beer quality mainly depends on the evaporation temperature and exposure time (Bra´nyik et al., 2012). Therefore the recovery of volatile compounds in beer is necessary in terms of enriching the flavor. Vacuum evaporated, low-alcoholic beers are rich in higher alcohol (up to 6%) and esters (up to 20%) as compared those obtained through conventional distillation (Andres-Iglesias et al., 2015b). Andres-Iglesias et al. (2015a) observed that most aroma compounds were evaporated in the first vapor fraction during dealcoholization by vacuum distillation. The amount of propanol and ethyl acetate were significantly decreased, which are associated with fruity and alcoholic characters. 2Phenyl ethanol, which is another important chemical that affects flavor, is partially evaporated in the process since a prolonged residence time is used at high temperatures (Andre´s-Iglesias et al., 2016). Evaporation

The main evaporation system consists of thin-layer evaporators as the separation quality depends on the time that the beer is on the heat exchange surface (Montanari et al., 2009). To reach an improved product quality as well as to reduce the residence time in the heat exchanger, thin-film evaporators with large surface areas were used (Bra´nyik et al., 2012). Thin-layer evaporators work under vacuum in an extremely short residence time and operate with gravimetric (falling film evaporator) or rotational movements (spinning cone column, SCC) (Liguori et al., 2018). SCC and Centritherm are evaporation systems that operate under rotational movement, and that can be used to produce a thin film mechanically (Bra´nyik et al., 2012). The Centritherm evaporator, designed with 1 2 12 hollow cones, has minimum thermal stress due to its low operating time (1 s) and temperature (35 C 2 60 C). In contrast, conventional evaporators have operation times of 30 s or more (Liguori et al., 2018). Regular beer is spread with centrifugal force as a thin layer (0.1 mm) over a heating surface that is heated by steam (Montanari et al., 2009). The steam fills a steam chamber, and then enters each hollow cone. As the steam condenses, the condensate instantaneously spreads to the upper wall and is removed from the evaporator. The dealcoholized beer is collected from the outer edge of the cones with 0.5 2 100 hL/h production capacities and then leaves the system via a paring tube (Bra´nyik et al., 2012).

Nonalcoholic Beer 183

Figure 6.3 Schematic diagram of the production of NA beer by SCC separation system. (1) Production feed tank, (2) feed pump, (3) heat exchanger, (4) discharge pump, (5) spinning cone column, (6) reinjection pump, (7) reinjection heater, (8) condenser, (9) vacuum pump, and (10) recovered extract pump. Adapted from Schmidtke, L.M., Blackman, J.W., Agboola, S.O., 2012. Production technologies for reduced alcoholic wines. J. Food. Sci. 77 (1), R25
R41.

SCC also allows for the rapid and efficient separation of ethanol from beer by applying gentle mechanical force (Catarino and Mendes, 2011a). SCC separation systems contain fixed and rotating cones which are alternated vertically (Fig. 6.3). A line of cones is fixed to the inside wall of a column while another line of cones is attached to a rotating shaft (Schmidtke et al., 2012). Beer drops onto a fixed cone as a thin film and passes toward the rotating cone with gravitational force (Makarytchev et al., 1998). The liquid film flows to further spinning cones until the liquid film reaches the bottom of the column while the vapor is pumped by countercurrent flow by a stripping agent (Wright and Pyle, 1996). In SCC processes, beer is fed into the top of the column, and unlike in conventional distillation, rectification or enrichment is unnecessary (Catarino and Mendes, 2011a). Feeding rate, temperature, and stripping rate are important parameters for the quality of the end product in SCC technology. Therefore this parameter was optimized with an ethanol
water (14.8%, v/v) model system. In SCC distillation, a high feeding rate and mild temperatures were proposed to maximize ethanol recovery (Huerta-Pe´rez and Pe´rez-Correa, 2018). SCC also has particular characteristics for the flavor management of heat-sensitive foods as well as dealcoholization (Mu¨ller et al., 2017). The main advantage of SCC distillation is that thermal stress is minimized without an adverse effect on the separation efficiency (Wright and Pyle, 1996). Drawbacks of the process are the possible oxygen input into the product stream, high maintenance expenditure, and extensive amounts of energy (Mu¨ller et al., 2017; Mangindaan et al., 2018).

184 Chapter 6 Falling film evaporators are the cheapest technology because of their low operating and investment costs. Furthermore, falling film evaporators have high efficiencies, are easy to construct, and easy to clean. The beer stay in evaporator only for a few seconds with a high speed vapor flow (20 2 80 m/s) (Montanari et al., 2009). In the food industry, falling film evaporators are preferred to centrifugal ones due to these advantages (Liguori et al., 2018). In falling film evaporators, beer is preheated to 60 C with saturated steam under vacuum (3.5 2 20 kPa). Beer then enters the evaporator and gradually evaporates while flowing downward (Bra´nyik et al., 2012). The beer film gets thinner and the vapor mass increases, then the vapor stream passes into a condenser (Liguori et al., 2018). The beer is not only dealcoholized, but also concentrated while passing through the falling film evaporator (Montanari et al., 2009). The liquefied condensate is always a mixture of ethanol and water, and can never be pure ethanol (Mu¨ller et al., 2017). Esters are completely removed, while the loss of ethanol reaches up to 97%, and acetaldehyde is accumulated up to 17% (Bra´nyik et al., 2012). Furthermore, dealcoholized beer contains less organic acids, volatile compounds, pH, and is slightly darker in color (Montanari et al., 2009). Expectedly, a reduction in ethanol as well as an increase in higher alcohol and esters is observed with increased evaporation temperatures (Mu¨ller et al., 2017). In thermal dealcoholization at an industrial scale, dealcoholized beer can be blended with a small quantity of original beer in order to compensate for the sensorial defects (Montanari et al., 2009). Alternatively, additional systems such as pervaporation to recover the flavor compounds might be installed to minimize volatile depletion (Andre´s-Iglesias et al., 2016). 6.3.2.2 Membrane-Based Methods The idea of membrane-based dealcoholization relies on the separation of ethanol using semipermeable membranes with temperature, concentration, or pressure differences. These methods emerged because the processes can be carried out at low temperatures; hence any thermal damage to the constituents of beer is limited. Studies on membrane-based systems have been increasing steadily over the past 30 years, and in the past few years, almost half of the dealcoholization studies investigated membrane-based methods (Mangindaan et al., 2018). Dialysis

Dialysis is a ubiquitous membrane process used in different fields from medical to chemical and biological research. The driving force for this system is the concentration difference between two sides of the membrane. Ethanol removal via dialysis is one of the earliest applications of membrane-based beer dealcoholization methods. Ethanol is removed via diffusion through a semipermeable membrane in aqueous form. One of the advantages of this method is the ability to work under very low (1 C
6 C) temperatures (Liguori et al., 2018). The dialysate should be recycled to keep the concentration difference at an optimum level

Nonalcoholic Beer 185 (Lipnizki, 2015). Although the system relies on the concentration difference, pressure (10
60 kPa) must be applied to the beer at the CO2 saturation level at least in order to minimize CO2 loss. Additionally, the concentration of CO2 might be increased in the dialysate (Leskosˇek and Mitrovic´ , 1994). Dealcoholized beers are marked with a lack of body in a high dialysate flow rate. A higher flow rate of the dialysate evidences a higher dealcoholization degree. The potential of dialysis as a dealcoholization method has been studied for over 30 years (Moonen and Niefind, 1982). Since then, a number of studies have explored the optimization of the process conditions and quality (Leskoˇsek and Mitrovi´c, 1994; Leskoˇsek et al., 1995; Petkovska et al., 1997). However, in more recent studies have shifted to more recent techniques. Reverse osmosis

Reverse osmosis (RO) is a membrane-based technology that is used in diverse applications such as desalination, wastewater treatment, juice concentration, and dealcoholization (Wenten, 2016). The smaller pore size used in RO compared to other pressure-driven membrane systems allows for a more selective separation (Fig. 6.4A). However, a smaller pore size also means a lower flux rate and higher pressure requirement (Johnson and Nguyen, 2017).

Figure 6.4 Schematic diagrams of the production of NA beer by membrane separation system. (A) Reverse osmosis, (B) osmotic distillation, and (C) pervaporation. Adapted from Mangindaan, D., Khoiruddin, K., Wenten, I.G., 2018. Beverage dealcoholization processes: past, present, and future. Trends Food Sci. Technol. 71, 36
45.

186 Chapter 6 The pressure used should be above the osmotic pressure of the solution in order to be separated. As a result, high pressure (up to 60 bar) is required in this operation. One of the biggest advantages of this system is the ability to retain temperature sensitive molecules (Catarino et al., 2007). In this technique, mostly asymmetric structures coupled with cellulose acetate, polyamide, and polyester sulfone layer membranes are used (Alcantara et al., 2016). For dealcoholization, an ideal membrane has a high permeability to ethanol and water while a low permeability to flavor components. Also, the membrane should be chemically, mechanically, and thermally resistant (Bra´nyik et al., 2012). Asymmetric membranes have heterogeneous composite membrane configurations and are the most useful membranes for RO. Thin-film composite membranes are durable under high pressure and have good flux rates. However, cellulose-based membranes have low flow rates and are not as selective as synthetic polymers are (Schmidtke et al., 2012). Dealcoholization based on RO has four suboperations, namely preconcentration, diafiltration, alcohol adjustment, and posttreatment (Lipnizki, 2015). Preconcentration is the first stage in which the feed-beer volume is reduced. In this step, permeate is removed while retentate is returned to the tank. In diafiltration, the permeate is replaced with demineralized water until the alcohol content reaches the desired volume. The alcohol concentration is adjusted by the redilution of retentate with demineralized water until the initial volume is reached. Also, a carbonation process may be necessary after RO (Bra´nyik et al., 2012). RO has been used to dealcoholize various beverages from cider (Lo´pez et al., 2002) to red wine (Catarino and Mendes, 2011b), lager beer (Catarino et al., 2006, 2007), and stout beer (Alcantara et al., 2016). Catarino et al. (2007) tested several membranes and operational parameters. In this study, a cellulose acetate membrane gave a high permeate flux with a low ethanol rejection. The authors suggested that at low temperatures, RO effectively reduced the ethanol level to under 0.5% without affecting the aroma (Catarino et al., 2007). In another study, Alcantara et al. (2016) used RO to dealcoholize stout beer. When RO was applied at 20 C, several quality parameters including color, bitterness, and antioxidant activity were similar to those of regular beer. However, the authors stated that more studies need to be conducted for the optimization of the parameters (e.g., pressure, fouling rate) (Alcantara et al., 2016). It was also stated in a study that the use of RO is not economically feasible to reduce the alcohol content to under 0.45% (Pilipovik and Riverol, 2005). Nanofiltration

Nanofiltration is a pressure driven, membrane process in which 0.0005 μm or bigger sized molecules are rejected. Nanofiltration stands between ultrafiltration and RO in that it has a higher flux than RO and rejects smaller molecules than ultrafiltration does (Johnson and Nguyen, 2017). The separation performance of a membrane is closely related to chemical

Nonalcoholic Beer 187 composition, temperature, pressure, feed flow, and membrane surface. Most nanofiltration membranes are manufactured polymeric composite materials that are designed in a spiral configuration (Salehi, 2014). However, the polymeric membrane structure changes when the membrane gets wet due to the swelling that occurs when solvents enter and pass through the membrane. Swelling may be used as an advantage as it can cause a denser structure of micro- or nanoporous nanofiltration membranes (Verhoef et al., 2008). A dense structure has an additional advantage, which is to avoid the permeation of important components during beer dealcoholization. Salehi (2014) argued that with nanofiltration, the alcohol content of beer can be reduced up to 10 times without harming the flavor. However, this might be an optimistic guess that overestimates the ability of nanofiltration systems. Catarino and Mendes (2011b) investigated ethanol removal from wine using several nanofiltration membranes. The authors stated that some membranes effectively reduced ethanol from 12 vol.% to approximately 5 vol.%. However, all membranes showed different characteristics in terms of flux rates and keeping aroma compounds (Catarino and Mendes, 2011b). Dealcoholization of beer via nanofiltration is not commonly reported in the literature (Mangindaan et al., 2018). Studies on wine show that nanofiltration is promising in terms of aroma rejection. In addition, nanofiltration exhibits a higher flux rate than RO (Banvolgyi et al., 2016). As a result, the application of nanofiltration in dealcoholization during brewing may be a promising alternative to RO (Mangindaan et al., 2018). Membrane distillation

Membrane distillation is a thermally driven separation process in which only vapor molecules are able to pass through a microporous hydrophobic membrane, the driving force being the vapor pressure difference between the two sides of the membrane due to the existing temperature gradient (Alkhudhiri et al., 2012). The volatile components evaporate at the warm feed solution
membrane interface, are transport through a microporous membrane, and then condensate at the cold side of the membrane
solution interface (Jiao et al., 2004). The process takes place at atmospheric pressure and at a temperature that may be much lower than the boiling point of the solutions; therefore, it can deal with heatsensitive solutions (Ilame and Satyavir, 2015). Depending on the methods to induce a vapor pressure gradient across the membrane and to collect the transported vapor from the permeate side, different MD configurations can be used (Drioli et al., 2015). Direct contact membrane distillation (DCMD) is a form of MD that has attracted the most amount of attention, in which permeate is in liquid phase and, therefore, the membrane on both sides is in direct contact with aqueous solutions (Macedonio, 2016). Although the main food related applications of DCMD are desalination, wastewater treatment, and concentrating

188 Chapter 6 aqueous solutions such as fruit juices (Onsekizoglu, 2012), this process can also be applied to remove ethanol from fermentation media (Gryta, 2001; Gryta and Barancewicz, 2011). In the ethanol removal by MD process, water vapor is also transported throughout the membrane. However, since ethanol has a high vapor pressure, the permeation rate of ethanol is always higher than that of water (Purwasasmita et al., 2015). Vacuum membrane distillation (VMD) is another configuration of MD, in which the vaporized solvent is recovered by vacuum and condensed, if needed, in a separate device (Macedonio, 2016). VMD has a relatively high permeate flux as compared to DCMD; on the other hand, it also carries a high risk of liquid entering the membrane pores (Johnson and Nguyen, 2017), which is the basic drawback of this system (Rezaei et al., 2018). Therefore, the strip side vacuum must be regulated to prevent the transmembrane pressure drop (Johnson and Nguyen, 2017). Purwasasmita et al. (2015) studied a VMD system for beer dealcoholization by applying both feed pressure (2
3 bar) on the feed side and vacuum pressure (490
660 mbar) on the permeate side in order to have ethanol transfer. At the end of 6 h under those operating conditions, the VMD process had reduced the alcohol content of the beer from 5 to 2.25 vol.%. The authors also indicated that VMD can be used to dealcoholization beer without losing other important nutrients and flavoring components such as maltose and glycerol. However, as also mentioned by Liguori et al. (2018), other aroma components and organoleptic analysis were not evaluated in that study. Osmotic distillation

Osmotic distillation (OD), also known as membrane evaporation, isothermal MD, or osmotic evaporation, is a separation process in which a liquid mixture containing a volatile component is contacted with a hydrophobic microporous membrane whose other side is exposed to a second liquid phase capable of absorbing that component, and this process can be accepted as another extension of MD (Field et al., 2017). The principle of operation is similar to that of DCMD, differing only in the way in which the water vapor pressure gradient across the membrane is generated (Johnson and Nguyen, 2017). In OD, the vapor pressure gradient results from a concentration gradient from the feed to the permeate side of the membrane generated using a stripping solution on the permeate side of the module (Fig. 6.4B) (Souhaimi and Matsuura, 2011). There is also a basic technical difference between MD and OD, which is reflected in the type of membrane best suited to their operation. Although the same membranes, which are porous, hydrophobic, and typically made of polytetrafluoroethylene or polypropylene, can be used in both processes, theoretically, MD membranes should be fabricated from a material of low thermal conductivity in order to reduce conductive heat loss to the permeate side and thereby minimize the energy needed to maintain the required temperature gradient across the membrane. On the other hand, OD does not have an applied temperature gradient to be maintained, and this process ideally uses a membrane of high thermal conductivity to

Nonalcoholic Beer 189 remove the latent heat (which causes a temperature gradient in opposition to the osmotically induced vapor pressure gradient) deposited at the membrane
stripping solution interface (Johnson and Nguyen, 2017). Because OD is performed at ambient temperature and atmospheric pressure, it is appropriate for applications in the food and pharmaceutical industries (Macedonio, 2016). In this context, many studies are focused on the concentration of heat-sensitive products such as fruit juices, since this process can achieve concentration to a very high level under mild operating conditions without product damage (Cassano and Drioli, 2007; Valdes et al., 2009; Kujawski et al., 2013; Bahceci et al., 2015; Zambra et al., 2015). OD has also been presented as a novel and promising technology to reduce the ethanol content in alcoholic beverages such as wine (Varavuth et al., 2009; Gambuti et al., 2011; Diban et al., 2013; Liguori et al., 2013a,b) and beer (Ejikeme et al., 2013; Russo et al., 2013a,b; De Francesco et al., 2015a; Liguori et al., 2015a,b). The transport mechanism of ethanol in OD is similar to that of MD. Because of the difference in ethanol vapor pressure between the two sides of the membrane, ethanol evaporates at the feed solution
membrane interface, is transported by vapor diffusion through the membrane pores, and condenses into stripping solutions at the membrane
stripping solution interface (Hogan et al., 1998; Varavuth et al., 2009; Mu¨ller et al., 2017). In addition to the membrane material, flux rate, temperature, and content and amount of stripping solution affect the quality of NA beer produced by OD processes, of which the content of stripping solution is the most important. Although salt solutions such as calcium chloride or sodium chloride are generally used as stripping solutions in OD for juice concentration, water is a more promising stripper of ethanol compared to salts for beverage dealcoholization. It is reported that the use of water as a stripper solution provides a higher ethanol flux and lower counter transport of water due to the low water activity differences (Varavuth et al., 2009; Liguori et al., 2018). However, when applying water as the stripping solution, CO2 loss and oxygenation of beer occur during the process, which adversely affect the flavor attributes of the beer. Using carbonated water as the stripper solution might be preferred to overcome this problem (Liguori et al., 2018). It is also possible to use permeates as stripping solutions to reduce waste. For example, Russo et al. (2013a) successfully dropped the alcohol content of regular beer to ,0.5% ABV using OD. In this study, the efficacy of different stripping solutions was also tested. First pure water was used as a stripping agent, and the ethanol concentration was dropped to under 0.5% ABV in four cycles. Then, to reduce water consumption, the permeate solutions from the first analysis were used as stripping solutions. Although the process lasted slightly longer compared to pure water, the delay might be ignored because of the waste management benefits. When compared to regular beer, NA beer showed no difference in pH, antioxidant activity, phenolic content, and color values (Russo et al., 2013a). In a successive study, Liguori et al. (2015b) used recycled permeates from former

190 Chapter 6 dealcoholization processes as stripping solutions to reduce the water consumption and decrease the loss of volatile compounds. In four cycles, the alcohol content of beer was reduced from 4.95% to 0.46% ABV. Similar to their previous study, the color, pH, polyphenols, and antioxidant activity were found to be similar (P..005). However, bitterness, foam stability, turbidity, and CO2 and O2 levels of NA beer were significantly different to regular beer. In addition, there were significant losses in total esters (99%) and total aldehydes (93%), both of which have a major impact on the aroma (Liguori et al., 2015a). Pervaporation

Pervaporation is an emerging technology to produce non- or low-alcoholic beverages with acceptable flavors and aromas (Schmidtke et al., 2012). The energy consumption is generally lower than in other conventional distillation processes (del Olmo et al., 2014). Pervaporation theory is based on the solution diffusion transport mechanism (Feng and Huang, 1997). Permeation and evaporation occur over a semipermeable membrane at low temperatures (Catarino et al., 2009). The permeate, which exists as a gas phase under low pressure, is condensed and transferred into the final product and the retentate keeps the other components (del Olmo et al., 2014) (Fig. 6.4C). The process selectivity is related to solubility, diffusion coefficient, membrane properties (thickness, permeability), and pressure difference (Mu¨ller et al., 2017). Membranes used in pervaporation are generally dense or microporous, asymmetric, polymeric membranes, and they can be hydrophilic or hydrophobic depending on the application. Hydrophilic membranes are favorable for dehydration processes, while hydrophobic membranes are used for removing organic compounds from aqueous mixtures (Van der Bruggen and Luis, 2015). The use of hydrophobic membranes in aroma recovery preferentially permit the permeation of organic components, and hence the permeate has at least 100 times greater aroma compounds than raw mixtures (Karlsson and Tragardh,1996). Therefore pervaporation is assessed as the most effective membrane-based process for the recovery of aroma compounds in beverages (del Olmo et al., 2014). Over the past decade, pervaporation has been applied for recovering aroma compounds from beer (Catarino et al., 2009; Paz et al., 2017), and in the dealcoholization of wine (Taka´cs et al., 2007) and beer (Catarino et al., 2009; del Olmo et al., 2014). Catarino and Mendes (2011a) produced NA beer using a combination of SCC and pervaporation. The dealcoholization of pilsner-type beer (5.5% ABV) was conducted using a SCC process and the aroma compounds (ethanol, propanol, isobutanol, amyl alcohols, ethyl acetate, isoamyl acetate, and acetaldehyde) were extracted using polyoctylmethylsiloxane/ polyetherimide (POMS/PEI) composite membranes. The dealcoholized (0.45% ABV) beer was enriched with pervaporated aroma in order to obtain an acceptable beer taste.

Nonalcoholic Beer 191 Similarly, del Olmo et al. (2014) recovered three aroma compounds (amyl alcohols, ethyl acetate, and isoamyl acetate) from special (5.5% ABV) and reserve (6.5% ABV) beer using pervaporation. Low-alcohol beer (,1% ABV) and alcohol-free beer (,0.1% ABV) were enriched with recovered aroma compounds. A pervaporation process was carried out with a polydimethylsiloxane (PDMS)/polyethylene terephthalate composite membrane, which allows a high flow rate of organic compounds due to its hydrophobic/organophilic characteristics. The results demonstrated that the selection of the membrane material in pervaporation processes could be a key factor in obtaining a higher performance of aroma recovery in beer (del Olmo et al., 2014). The membrane area, process time, temperature, and flow rate also affect the aroma recovery rate. The process time should be comparatively longer to remove alcohol in higher amounts. For instance, a process time of 5.6 h decreased the alcohol content from 5.0% to 2.6%. However, an increased process time of up to 17 h decreased the alcohol content to 0.6% (Mu¨ller et al., 2017). In a similar study, Paz et al. (2017) optimized the operating parameters for longer transport times with bigger membrane areas. After 7 h of pervaporation, the recovery of aroma reached near maximum. Appropriate aroma recovery percentages (5%
35%) were obtained in tasted aromas using two commercial pervaporation membranes (PDMS). Thus NA beer which has quite a similar quality to the original beer was produced with pervaporation (Paz et al., 2017). Catarino et al. (2009) also optimized the operation parameters such as the permeate flux, the aroma/ethanol selectivity, and the ethanol concentration using response surface methodology. The extraction of aroma compounds from beer was carried out with pervaporation using a POMS/PEI membrane. The optimum pervaporation conditions for feed temperature, feed velocity, and permeate pressure were determined as 12.4 C, 0.45 m/s, and 1.0 mbar, respectively. The results suggested that permeate pressure decreases the membrane flux, while the temperature and feed velocity increase the membrane flux. Esters selectivity is affected negatively by temperature, while it is affected positively by permeate pressure and velocity. This study generated models that describe the relationship between the operating conditions and process responses (Catarino et al., 2009).

6.3.3 Other Methods Each technique discussed in this chapter has advantages and drawbacks. It might be possible to overcome the drawbacks of a single technique by combining methods. In a recent study, Jiang et al. (2017) combined a biological and a physical method to produce NA beer at pilot scale. First, the fermentation was started using Saccharomyces ludwigii at 18 C, and after the fermentable sugar content was reduced by 25%, the fermentation was stopped by adjusting the temperature to 0 C. After this limited fermentation, vacuum distillation was applied to remove the alcohol (1%). The vacuum distillation was carried out

192 Chapter 6 at 0.05
0.06 MPa and 64 C
68 C. In the end, regular beer was added to increase the aroma. The authors reported that the final product showed similar aroma characteristics to those of regular beer (Jiang et al., 2017). Another alternative approach to dealcoholization and aroma recovery is using supercritical CO2 extraction. The removal of ethanol from cider (Medina and Martı´nez, 1997), model systems (Fornari et al., 2009), and wine (Ruiz-Rodriguez et al., 2010, 2012) was studied. In this system supercritical CO2 is used for ethanol removal from aqueous systems. However, to date there is no study conducted on beer. CO2 is supercritical at very high pressure (73 atm at 31 C). Due to its high cost it is not feasible, at least in the short term, for beer production (Mangindaan et al., 2018). Solid CO2 extraction has been used for the dealcoholization of beverages besides supercritical CO2. Antonelli et al. (1996) applied this system to dealcoholize wine. Wine samples were spouted over solid CO2 for 5 min at 5 C. Thus the alcohol content was reduced to 1.2%
1.4% from the initial value (9.4%
10.7%). However, this method cannot be defined as an effective dealcoholization process due to the high energy consumption and loss of major volatile compounds. Forward osmosis (FO) might be a promising dealcoholization method. FO is a membranebased separation technology that relies on concentration difference. Two solutions, a feed solution with a low osmotic pressure and a draw solution with very high osmotic pressure, are separated with a semipermeable membrane (Ambrosi et al., 2018). FO has been studied in different applications including waste management, desalination, food processing, drug release, and power generation (Zhao et al., 2012). FO was used to remove ethanol from aqueous solutions, and the results were comparable with RO (Ambrosi et al., 2017, 2018). Microbial fuel cells (MFC) represent a promising waste management tool in which anaerobic bacteria are used to produce electricity from waste (Liu and Logan, 2004). This technology has been tested in brewery wastewater (Wrighton and Coates, 2009). In a novel application, Szollosi et al. (2016) used S. cerevisiae in an MFC to produce low-alcoholic beer. In this study, the authors found that increasing the anode surface area or the addition of electron shuttles such as riboflavin to wort decrease the ethanol production by up to 2% ABV while increasing the electricity generation. The results showed that MFC might be an alternative for NA beer production.

6.4 Conclusion With the increasing health awareness, drinking habits have changed to moderate drinking and low or alcohol-free beverages. As a result, demand of NA beer has increased significantly. Although NA beer resembles regular beer in various quality parameters such as pH, color, and turbidity, there are significant differences in aroma compounds including alcohols, aldehydes, and esters. Unfortunately, the lack of aroma compounds creates

Nonalcoholic Beer 193 sensorial differences which draw negative attention from consumers. In this chapter, biological methods of NA beer production and physical dealcoholization methods have been discussed. Among the biological methods, due to the rapid advances in molecular biology and biotechnology, the utilization of special yeasts has been trending over the past decade. This trend is expected to continue increasingly. The emergence of GM yeasts with the development of state-of-the-art genomic tools such as TALON and CRISPR/Cas9, creates many opportunities in this field. However, consumer preference should be observed closely as GM products are not favorable in many countries. Physical dealcoholization methods have been studied for decades. Rectification and SCC systems are separated from other thermal methods because of their ability to preserve aroma compounds. However, membrane-based removal of ethanol has been emerging. Studies with RO and OD have been highly successful. Besides, pervaporation and nanofiltration systems are promising alternatives. Furthermore, there are other alternatives such as MFC or supercritical CO2 extraction. In the near future, more studies on these operations are expected. The feasibility of these methods has not been fully explored, and the cost of these systems should also be considered. It is expected that biological methods are the most advantageous economically, while membrane systems are the most expensive production methods in terms of installation and operating costs. On the other hand, membrane systems are expected to overcome the economic disadvantages with the development of technological advances, and these processes are expected to be much more attractive. The marketing of NA beer should also be studied. Instead of promoting NA beer as a substitute that is consumed when regular beer is not an option, maybe it would be a better idea to introduce NA beer as a specialty beer that has all the bioactive compounds of regular beer while having other advantages mentioned previously.

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Further Reading Cortacero-Ramı´rez, S., de Castro, M.H.B., Segura-Carretero, A., Cruces-Blanco, C., Fernandez-Gutierrez, A., 2003. Analysis of beer components by capillary electrophoretic methods. TrAC Trends Analyt. Chem. 22 (7), 440
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307. Bakish Materials Corporation Englewood, Englewood, NJ.

CHAPTER 7

Nonthermal Technologies for Nonalcoholic Beverages G.J. Swamy1, K. Muthukumarappan1, A. Sangamithra2, V. Chandrasekar3 and S. Sasikala4 1

Department of Agricultural and Biosystems Engineering, South Dakota State University, Brookings, SD, United States 2Department of Food Technology, Kongu Engineering College, Perundurai, India 3 ICAR-CIPHET, Ludhiana, India 4Department of Food Process Engineering, School of Bioengineering, SRM University, Kattankulathur, India

Chapter Outline 7.1 Introduction 202 7.2 Ultrasound 202 7.2.1 Generation of Power Ultrasound 202 7.2.2 Microbial Inactivation in Nonalcoholic Beverages

7.3 7.4 7.5 7.6 7.7 7.8

204

Ozonation 207 Ozone Generation 208 High-Pressure Processing 210 High-Pressure
Processing Equipment 211 Ultraviolet and Pulsed-Light Technology 212 Irradiation 213 7.8.1 Mode of Inactivation of Microbes

7.9 Cold Plasma

216

217

7.9.1 Mode of Action of Cold Plasma 218 7.9.2 Treatment of Nonalcoholic Drinks with Plasma

7.10 Pulsed Electric Field Processing 7.10.1 PEF Equipment Design

220

220

7.11 Dense-Phase Carbon Dioxide Technology 7.12 Conclusion 226 References 227

Trends in Non-alcoholic Beverages. DOI: https://doi.org/10.1016/B978-0-12-816938-4.00007-0 © 2020 Elsevier Inc. All rights reserved.

221

201

218

202 Chapter 7

7.1 Introduction Traditional thermal treatment processes are a keystone of the food industry to provide the required safety profile and addendums to the food’s existing shelf-life period. However, such processes may lead to losses of preferred organoleptic properties and damage to thermolabile nutrients. Nonthermal technology has been researched to satisfy food safety demands. In addition, it prevents adverse impacts on nutritional and sensory aspects of the food products. Novel technologies are of benefit to both food processors and consumers; however, depending on the complexity of the food material and the variety of foods produced, the validation process is a challenge for the food industry. The factors that drive the necessity of the validation process include extension of shelf life, nutritional and sensory aspects, organoleptic properties, consumer acceptance, and impact on the environment.

7.2 Ultrasound Ultrasound is known to have a major influence on the rate of different processes in the food and bioprocessing industry. Most processes can be completed in a few seconds or minutes with high reproducibility using ultrasound, thereby reducing the processing cost, with higher purity of the final product and consuming only a small portion of the energy normally needed for conventional processes. Several ultrasound-assisted processes such as extraction, freezing and thawing, and cutting and drying have been carried out efficiently in the food industry. Food processes executed by the action of ultrasound are supposed to be influenced by cavitation phenomena and mass transfer enhancement. From various researches who deal with the impact of ultrasound on the quality and stability of liquid foods, it is clearly evident that sonication can be successfully implemented to extend the shelf life of nonalcoholic beverages (Swamy et al., 2018). Combining ultrasound with mild temperature (thermosonication) or pressure-temperature (manothermosonication) can create a better effect. Two or more nonthermal techniques may also be combined to produce a synergistic effect; however, in large-scale applications, the process is expensive and tedious to scale-up. Food analysis and food processing are the segments of ultrasonic application. Ultrasound can be classified as illustrated in Fig. 7.1:

7.2.1 Generation of Power Ultrasound Sound is created from electrical energy through the vibration created by ultrasonic transducers. Piezoelectric and magnetostrictive transducers may be employed, although the former are preferred as they are efficient in terms of power consumption. Acoustic cavitation is the factor that drives the processing effects of sonication. In spite of cavitation being a source of erosion in fluid flow through pipes, its harnessed form is used for sonic applications. Cavitation bubbles are formed when sonic waves pass through the liquid, as in

Nonthermal Technologies for Nonalcoholic Beverages

203

Ultrasound

Low power (