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Elucidation of Odour-Potent Compounds and Sensory Profiles of Vidal Blanc and Riesling Icewines from the Niagara Peninsula: Effect of Harvest Date and Crop Level

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Elucidation of Odour-Potent Compounds and Sensory Profiles of Vidal Blanc and Riesling Icewines from the Niagara Peninsula: Effect of Harvest Date and Crop Level Elucidation of Odour-potent Compounds and Sensory Profiles of Vidal blanc and Riesling Icewines from the Niagara Peninsula: Effect of Harvest Date and Crop Level Amy J. Bowen, B.Sc. Department of Biological Sciences Submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy Faculty of Mathematics and Science, Brock University St. Catharines, Ontario © Amy J. Bowen, 2010 Abstract It was hypothesized that the freeze/thaw cycles endured by icewine grapes would change their chemical composition, resulting in unique chemical fingerprint and sensory properties, and would be affected by harvest date (HD) and crop level (CL). The objectives were: 1) to identify odour-active compounds using gas chromatographic and sensory analysis; 2) to determine the effect of CL and HD on these compounds; 3) to determine the icewine sensory profiles; 4) to correlate analytical and sensory results for an overall icewine profile. CharmAnalysis™ determined the Top 15 odour-potent compounds in Vidal and Riesling icewine and table wines; 24 and 23 compounds, respectively. The majority of the compounds had the highest concentrations in the icewines compared to table wines. These compounds were used as the foundation for assessing differences in icewine chemical profiles from different HD and CL. Vidal and Riesling icewine were made from grapes picked at different HD; HI: 19 December; H2: 29 December; H3: 18 January; H4: 11 February (Vidal only). HI wines differed from H3 and H4 wines in both Vidal and Riesling for aroma compounds and sensory profiles. - Three·CL [control (fully cropped), cluster thin at fruit set to one basal cluster/shoot (TFS), and cluster thin at veraison to one basal cluster/shoot (TV)] were evaluated for Riesling and Vidal cultivars over two seasons. Vidal icewines had the highest concentration of aroma compounds in the control and TV icewines in 2003 and in TFS icewines in 2004. In Riesling, most aroma compounds had the highest concentration in the TV icewines and the lowest concentration in the TFS wine for b<;>th years. The thinned treatments were associated with almost all of the sensory attributes in both cultivars, both years. HD and CL affected the chemical variables, aroma compounds and sensory properties of Vidal and Riesling icewines and freeze/thaw events changed their sensory profile. The most odour-potent compounds were p-damascenone, cis-rose oxide, 1- octen-3-ol, 4-vinylguaiacol, ethyl octanoate, and ethyl hexanoate. The role of P­ damascenone as a marker compound for icewine requires further investigation. This research provides a strong foundation for the understanding the odour-active volatiles and sensory profiles important to icewine. Acknowledgements This thesis would not have been possible without the unwavering support of my supervisor Dr. Andy Reynolds. Thank you for always having "a minute" to discuss and for allowing me the independence to make this project my own. You have enabled me to grow as a researcher and I hope we have the opportunity to work together again in the future. Thank you ... To my committee, Dr. Doug Bruce and Dr. Debbie Inglis for your suggestions and comments throughout my project and my thesis. To, my internal, Dr. Martin Lemaire, and external examiner, Dr. Terry Acree. To the growers who allowed me to work in their vineyards and harvest their icewine grapes; Dave Lambert and Colin Glass. To Dr. Isabelle Lesschaeve, for your help with the sensory and statistical analysis of the icewines and for your support throughout. Dr. Terry Acree and Ed Lavin at Cornell University and Tim Jones at Brock University, I can't thank any of you enough for the time you set aside to answer all my questions and help me trouble shoot. I would still be 'fighting with the GC' and knee­ deep in method development without your help ... thank you! Thank you ... To the many volunteers who donated their time helping me harvest icewine grapes (not as fun as it sounds). To Lynda van Zuiden and Jim Willwerth for helping me press, process and bottle the icewines. To the members of my sensory panel for your hard work and commitment in assessing the icewines. To my "sniff judges" for your concentration and dedication, it's harder than it looks. I would have no results without all of you. To Gail Higenell for being a great friend ... French fries and beer really are a cure-all. Your support and open door were priceless. To everyone at CCOVI for the laughs, support and good times. To my friends, I hope to be seeing a lot more of you now! Thanks for always being there when I needed someone to listen. To my family, thank you for your love, your support, your encouragement and your patience. It means more than you know. Mom and Dad, you've always told me to "Go for it" and given me the belief that I can do anything I want. Manjari, thanks for being the best bodyguard ever and always making me stop and take the time to smell the grass. Jim, you're the best! You're always there to support me, encourage me and to offer a glass of wine (or two) when I need it most. I love you all! TABLE OF CONTENTS CHAPTER 1. INTRODUCTION AND LITERATURE REVIEW 1 1.1. INTRODUCTION 1 1.2. ICEWINE 2 1.2.1. ICEWINEREGULATION 4 1.2.2. ICEWINE: VITICULURAL CONSIDERATIONS 5 1.2.3. ICEWINE: OENOLOGICAL CONSIDERATIONS 8 1.3. WINE VOLATILES ANALYSIS 11 1.3.1. GAS CHROMATOGRAPHY 11 GAS CHROMATOGRAPHY-MASS SPECTROMETRY 12 GAS CHROMATOGRAPHY-OLFACTOMETRY 13 1.3.2. EXTRACTION OF GRAPE AND WINE VOLATILES 16 1.4 WINE AROMA COMPOUNDS 19 1.4.1. ODOUR ACTIVITY VALUES 19 1.4.2. SOURCES OF AROMA COMPOUNDS 21 1.4.3. WINE IMPACT ODOURANTS 23 1.4.4. SENSORY ANALYSIS 26 1.5. RELATING SENSORY AND INSTRUMENTAL DATA 27 1.6. FACTORS AFFECTING WINE COMPOSITION AND SENSORY PROFILES 29 1.6.1. OXIDATION OF GRAPES 30 FREEZE AND THAW EVENTS 30 WINE AGEING 31 1.6.2. CONSEQUENCES OF HANG TIME 33 GRAPE DESICCATION 33 PATHOGEN INFECTION 34 1.6.3. HARVEST DATE AS A DETERMINANT OF WINE COMPOSITION AND SENSORY PROFILE 35 1.6.4. CROP LEVEL AS A DETERMINANT OF WINE COMPOSITION AND SENSORY PROFILE 38 1.7. CONCLUSION 39 1.8. LITERATURE CITED 40 CHAPTER 2. ODOUR POTENCY OF AROMA COMPOUNDS IN RIESLING AND VIDAL BLANC TABLE WINE AND ICEWINE BY GAS CHROMATOGRAPHY-OLFACTOMETRY-MASS SPECTROMETRY 52 ABSTRACT 52 INTRODUCTION 52 MATERIALS AND METHODS 59 WINES 59 CHEMICALS 59 VOLATILE EXTRACTION 59 GAS CHROMATOGRAPHY-MASS SPECTROMETRY 60 GAS CHROMATOGRAPHY -OLFACTOMETRY 61 JUDGE REPRODUCIBILITY 61 LEXICON GENERATION 61 CHARMANALYSIS TM 62 IDENTIFICATION AND QUANTIFICATION 62 STATISTICAL ANALYSIS 62 RESULTS 63 GAS CHROMATOGRAPHY-OLFACTOMETRY 63 GAS CHROMATOGRAPHY-MASS SPECTROMETRY 65 ODOUR ACTIVITY VALVES 66 DISCUSSION 67 COMPARISON OF GC-O AND OAV RESULTS 67 ODOUR-POTENT COMPOUNDS 70 CONCLUSIONS 75 LITERATURE CITED 76 LIST OF TABLES 82 CHAPTER 3. EFFECT OF HARVEST DATE ON VIDAL BLANC AND RIESLING ICEWINE FROM THE NIAGAGARA PENINSULA: I. CHEMICAL VARIABLES AND AROMA COMPOUNDS 88 ABSTRACT 88 INTRODUCTION 88 MATERIALS AND METHODS 93 CHEMICALS 93 WINES 94 FERMENTATION 94 BOTTLING 95 MUST AND WINE ANALYSIS 95 VOLATILE EXTRACTION 96 GAS CHROMATOGRAPHY-MASS SPECTROMETRY 96 IDENTIFICATION AND QUANTIFICATION 97 STATISTICAL ANALYSIS 97 RESULTS 98 MUST CHEMICAL VARIABLES 98 WINE CHEMICAL VARIABLES 99 AROMA COMPOUNDS 99 ANALYSIS OF VARIANCE 99 PRINCIPAL COMPONENTS ANALYSIS 101 DISCUSSION 103 MUST AND WINE CHEMICAL ANALYSIS 103 VOLATILE ANALYSIS 104 EFFECT OF HARVEST DATE 104 CONCLUSIONS 110 LITERATURE CITED 111 LIST OF TABLES 116 LIST OF FIGURES 123 CHAPTER 4. EFFECT OF CROP LEVEL ON VIDAL BLANC AND RIESLING ICEWINE FROM THE NIAGAGARA PENINSULA: II. CHEMICAL VARIABLES AND AROMA COMPOUNDS 130 ABSTRACT 130 INTRODUCTION 130 MATERIALS AND METHODS 134 CHEMICALS 134 TREATMENTS 134 HARVEST AND PRESSING 135 FERMENTATION 135 BOTTLING 135 MUST AND WINE ANALYSIS 136 VOLATILE EXTRACTION 136 GAS CHROMATOGRAPHY-MASS SPECTROMETRY 137 IDENTIFICATION AND QUANTIFICATION 137 STATISTICAL ANALYSIS 138 RESULTS 139 MUST CHEMICAL VARIABLES 139 WINE CHEMICAL VARIABLES 139 VIDAL AROMA COMPOUNDS 140 ANALYSIS OF VARIANCE 140 PRINCIPAL COMPONENTS ANALYSIS 141 RIESLING AROMA COMPOUNDS 143 ANALYSIS OF VARIANCE 143 PRINCIPAL COMPONENTS ANALYSIS 144 DISCUSSION 146 MUST AND WINE CHEMICAL ANALYSIS 146 EFFECT OF CROP LEVEL ON VIDAL AROMA COMPOUNDS 147 EFFECT OF CROP LEVEL ON RIESLING AROMA COMPOUNDS 149 ODOUR ACTIVITY VALVES 151 CONCLUSIONS 151 LITERATURE CITED 152 LIST OF TABLES 156 LIST OF FIGURES 165 CHAPTER 5. EFFECT OF HARVEST DATE AND CROP LEVEL ON VIDAL BLANC AND RIESLING ICEWINE FROM THE NIAGAGARA PENINSULA: III. RELATING SENSORY AND INSTRUMENTAL ANALYSIS 171 ABSTRACT 171 INTRODUCTION 171 MATERIALS AND METHODS 176 HARVEST DATE WINES 176 CROP LEVEL WINES 177 FERMENTATION 178 DIFFERNCE TESTING 178 DESCRIPTIVE ANALYSIS 178 STATISTICAL ANALYSIS 179 RESULTS 180 DIFFERENCE TESTING 180 HARVEST DATE 180 CROP LEVEL 180 DESCRIPTIVE ANALYSIS 181 VIDAL HARVEST DATE 181 RIESLING HARVEST DATE 182 VIDAL CROP LEVEL 182 RIESLING CROP LEVEL 184 CORRELATION BETWEEN SENSORY AND ANALYTICAL RESULTS 186 VIDAL HARVEST DATE 186 RIESLING HARVEST DATE 187 VIDAL CROP LEVEL 189 RIESLING CROP LEVEL 190 DISCUSSION 191 SENSORY PROFILES 191 HARVEST DATE 191 CROP LEVEL 193 CORRELATION BETWEEN SENSORY AND CHEMICAL DESCRIPTORS 194 HARVEST DATE 195 CROP LEVEL 198 CONCLUSIONS 199 LITERATURE CITED 202 LIST OF TABLES 206 LIST OF FIGURES 216 CHAPTER 6. GENERAL DISCUSSION AND CONCLUSIONS 225 6.1. INTRODUCTION 225 6.2.0BJECTIVE 1: IDENTIFY ODOUR-ACTIVE COMPOUNDS THAT CHARACTERIZE NIAGARA ICEWINE 226 6.3. OBJECTIVE 2: EFFECT OF HARVEST DATE AND CROP LEVEL ON ODOUR-ACTIVE COMPOUNDS 227 6.3.1 HARVETDATE 227 6.3.2. CROP LEVEL 230 6.4. OBJECTIVE 3: EFFECT OF HARVEST DATE AND CROP LEVEL ON ICEWINE SENSORY PROFILES 231 6.4.1.
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