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EFFECTS of WATER CHEMISTRY and PANNING on FLAVOR VOLATILES and CATECHINS in TEAS (Camellia Sinensis)

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EFFECTS OF WATER CHEMISTRY AND PANNING ON FLAVOR VOLATILES AND CATECHINS IN TEAS (Camellia sinensis) Ershad Sheibani Dissertation submitted to the faculty of the Virginia Polytechnic Institute and State University in partial fulfillment of the requirements for the degree of Doctor of Philosophy In Food Science and Technology Sean F. O’Keefe Susan E. Duncan Andrea M. Dietrich David D. Kuhn October 27, 2014 Blacksburg, Virginia Keywords: Tea, Flavor Volatiles, Catechins, Water Chemistry, Panning Copyright 2014 EFFECTS OF WATER CHEMISTRY AND PANNING ON FLAVOR VOLATILES AND CATECHINS IN TEAS (Camellia sinensis) Ershad Sheibani ABSTRACT In the first experiment, effects of brewing time, chlorine, chloramine, iron, copper, pH and water hardness were investigated for their effects on extraction of epigallocatechine gallate (EGCG) and caffeine in green tea and oolong tea aqueous infusions. The extraction of EGCG and caffeine were lower when green tea was brewed in hard water compared to distilled water. Brewing green tea and Oolong tea in tap water resulted in higher extraction of caffeine but had no effect on EGCG compared to distilled water. The extraction of EGCG and caffeine were significantly increased (P<0.05) when green tea and Oolong tea were brewed in the chlorinated water at 4.0 mg free chlorine per liter. The purpose of the second experiment was to optimize SDE conditions (solvent and time) and to compare SDE with SPME for the isolation of flavor compounds in Jin Xuan oolong tea using Gas Chromatography- Mass Spectrometry (GC-MS) and Gas Chromatography- Olfactrometry (GC-O). The concentration of volatile compounds isolated with diethyl ether was higher (P<0.05) than for dichloromethane and concentration was higher at 40 min (P<0.05) than 20 or 60 minutes. For SDE, 128 volatiles were identified using GC-MS and 45 aroma active compounds using GC-O. The number of volatiles identified using GC-MS was lower in SPME than SDE. For SPME, 59 volatiles and 41 aroma active compounds were identified. The composition of the volatiles isolated by the two methods differed considerably but provided complementary information. The goal of the third experiment was to determine effects of panning on flavor volatile compositions of oolong using GC-MS and GC-O. Simultaneous Distillation and Extraction (SDE) and Solid Phase Microextraction (SPME) techniques were applied for extraction of volatiles in panned and unpanned teas. A total of 190 volatiles were identified from SDE and SPME extractions using GC-MS and GC-O. Trans-nerolidol, 2- hexenal, benzaldehyde, indole, gernaiol, and benzenacetaldehyde contents were significantly decreased (P<0.05) by panning; however, panning increased (P<0.05) contents of linalool oxide, cis jasmone, methyl salicylate in oolong tea. Overall, panning significantly changes the volatile compositions of the tea and created new aroma active compounds. iii DEDICATION I dedicate this manuscript to my parents for all love and support through my life. iv ACKNOWLEDGEMENTS I would like to express my sincere gratitude to my esteemed major advisor, Dr. Sean F. O’Keefe, Professor, Department of Food Science and Technology, for all of his invaluable assistance and guidance throughout my study at Virginia Tech. His support, guidance, encouragement are the foundation of my achievement. I would like to thank to respected members of my advisory committee Dr. Susan Duncan, Professor, and Dr. David Kuhn, Assistant Professor, Department of Food Science and Technology, and Andrea Dietrich, Professor, Department of Civil and Environmental Engineering, for their expert guidance and assistance with my research. I also owe special thanks to Jordan Newkirk, Sheldon Masters, Kim Waterman, and Harriet Williams, without their kind cooperation and ever willing help, this work would not have been possible. I would like to thank Water Interface Interdisciplinary Graduate Education Program (IGEP) at Virginia Tech for funding my study at Virginia Tech. I am also very thankful to all the faculty, staff, lab mates and friends at the Department of Food Science and Technology, MBA Program and Water IGEP for providing all kinds of help, knowledge and guidance during my study. Finally, I express my heartiest thanks to my parents, Dr. Ebrahim Sheibani and Dr. Zahra Afshari, for their sustained supports, inspiration and encouragement. No words can suffice my feelings of indebtedness for their love, selfless devotion, blessing and sacrifices in all phases of my life. v TABLE OF CONTENTS ABSTRACT ........................................................................................................................ ii DEDICATION ................................................................................................................... iv ACKNOWLEDGEMENTS .................................................................................................v LIST OF TABLES ............................................................................................................. ix LIST OF FIGURES ........................................................................................................... xi CHAPTER ...........................................................................................................................1 I. LITERATURE REVIEW ..................................................................................1 1.1 Tea and the Global Market ..........................................................................2 1.2 Tea Market in the United States...................................................................5 1.3 Tea Classification.........................................................................................8 1.4 Tea Chemical Components ..........................................................................9 1.5 Catechins in Tea .........................................................................................12 1.6 Solid Phase Microextraction (SPME) ........................................................17 1.7 Simultaneous Distillation and Extraction (SDE) .......................................19 1.8 Gas Chromatography-Olfactometry (GC-O) .............................................21 1.9 Oolong Tea.................................................................................................22 1.10 Panning ....................................................................................................24 1.11 Flavor composition of Oolong Tea ..........................................................25 1.12 Water Chemistry ......................................................................................30 1.13 Water Hardness ........................................................................................31 1.14 Iron ...........................................................................................................33 1.15 Copper ......................................................................................................34 1.16 Chlorine and Chloramine .........................................................................35 1.17 Effects of Water Compositions on Tea infusions ....................................35 1.18 Conclusions and Research Objectives .....................................................39 References ........................................................................................................40 II. Water chemistry Effects on EGCG and Caffeine Extraction in Green and Oolong Tea ....................................................................................54 vi Abstract ............................................................................................................55 2.1 Introduction ................................................................................................56 2.2 Materials and Methods ...............................................................................58 2.2.1 Tea Sources .......................................................................................58 2.2.2.1 Copper and Water Hardness ..........................................................58 2.2.2.1.1 Statistical Analysis ................................................................59 2.2.2.2 Iron, Copper, pH and Water Hardness ...........................................59 2.2.2.2.1 Statistical Analysis ................................................................60 2.2.2.3 Tap Water Vs Distilled Water........................................................60 2.2.2.3.1 Statistical Analysis ................................................................61 2.2.2.4 Chlorine and Chloramines .............................................................61 2.2.2.4.1 Statistical Analysis ................................................................62 2.2.2.5 Free Chlorine .................................................................................62 2.2.2.5.1 Statistical Analysis ................................................................62 2.2.3 Infusion Preparation, and EGCG and Caffeine Extraction ...............63 2.2.4 HPLC-DAD Analysis .......................................................................63 2.3 Results and Discussion ..............................................................................64 2.4 Conclusions ................................................................................................70 References ........................................................................................................73 III. Comparison of SDE and SPME for Analysis of Flavor
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