IMPACT OF THERMAL AND NON-THERMAL PROCESSING TECHNIQUES ON APPLE AND GRAPEFRUIT JUICE QUALITY By ZAREENA AZHU VALAPPIL A DISSERTATION PRESENTED TO THE GRADUATE SCHOOL OF THE UNIVERSITY OF FLORIDA IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE DEGREE OF DOCTOR OF PHILOSOPHY UNIVERSITY OF FLORIDA 2010 1 © 2010 Zareena Azhu Valappil 2 To my daughter Suha and my husband, Niyas 3 ACKNOWLEDGMENTS I would like to thank my advisor, Dr. Russell Rouseff, for his guidance and unending support throughout the course of my research work. It would not have been possible to conduct my research at the United States Department of Agriculture without his help and encouragement. I would also like to thank my committee members: Dr. M. Marshall, Dr. B. Ache, Dr. W. Yang and Dr. H. Zhang. I would also like to thank my previous committee members, Dr. M. Balaban and Dr. S. Talcott, who have left University of Florida. My specials thanks to Dr. Fan, Dr. Geveke and Dr. Zhang at USDA for helping me successfully conduct my research at USDA. I would also like to thank my lab mates Kim, Jen, Kym, Glen and Tim for their constant help and support and for making my life easier and enjoyable at USDA. A special thanks to Kim for all her help in the lab and participating in GCO and sensory work. I also want to thank my Mom and Dad for their love and guidance throughout my life. Finally, I would like to thank my husband Niyas and daughter Suha for supporting and helping me achieve my goals. Lastly, I want to thank God for everything. 4 TABLE OF CONTENTS page ACKNOWLEDGMENTS .................................................................................................. 4 LIST OF TABLES ............................................................................................................ 9 LIST OF FIGURES ........................................................................................................ 11 ABSTRACT ................................................................................................................... 13 CHAPTERS 1 INTRODUCTION .................................................................................................... 15 2 LITERATURE REVIEW .......................................................................................... 18 Flavor Perception .................................................................................................... 18 Fruit Flavors ............................................................................................................ 22 Apple Juice/Cider Aroma .................................................................................. 22 Grapefruit Juice Aroma .................................................................................... 25 Volatile Extraction ................................................................................................... 28 Gas Chromatography Olfactometry ........................................................................ 30 Processing .............................................................................................................. 31 Thermal Pasteurization .................................................................................... 32 Citrus juice thermal processing .................................................................. 33 Apple juice thermal processing .................................................................. 33 Effect of Thermal Pasteurization on Juice Flavor ............................................. 34 Non-Thermal Processing Methods ................................................................... 36 Pulsed electric field .................................................................................... 38 Radio frequency electric field ..................................................................... 45 Ultraviolet radiation .................................................................................... 46 3 COMPARISON OF THERMAL AND NON-THERMAL TECHNIQUES ON APPLE CIDER STORAGE QUALITY UNDER EQUIVALENT PROCESS CONDITIONS ......................................................................................................... 55 Introduction ............................................................................................................. 55 Materials and Methods............................................................................................ 56 Determination of Processing Conditions That Achieve 6-log Reduction of E. coli K12 ......................................................................................................... 56 Ultraviolet process ..................................................................................... 56 Pulsed electric field process ....................................................................... 57 Thermal process ........................................................................................ 58 Shelf-Life of Processed Apple Cider ................................................................. 58 Processing and packaging ......................................................................... 58 Storage ...................................................................................................... 59 5 Microbial tests ............................................................................................ 59 pH .............................................................................................................. 60 Brix ............................................................................................................. 60 Color .......................................................................................................... 60 Statistical Analysis ............................................................................................ 61 Results and Discussion........................................................................................... 61 Optimization of Equivalent Processing Conditions ........................................... 61 Effect of Thermal and Non-Thermal Processing on Microbial Stability During Storage of Apple Cider .................................................................................. 63 Effect of Thermal and Non-Thermal Processing on Appearance of Apple Cider During Storage .................................................................................... 65 Effect of Thermal and Non-thermal Processing on the pH and Brix of Apple Cider During Storage .................................................................................... 65 Effect of Thermal and Non-Thermal Processing on Color of Apple Cider During Storage .............................................................................................. 66 Conclusion .............................................................................................................. 68 4 IMPACT OF THERMAL AND NON-THERMAL PROCESSING TECHNOLOGIES ON APPLE CIDER AROMA ...................................................... 74 Introduction ............................................................................................................. 74 Materials and Methods............................................................................................ 74 Apple Cider ....................................................................................................... 75 Apple Cider Processing .................................................................................... 75 Heat treatment ........................................................................................... 76 Ultraviolet treatment ................................................................................... 76 Pulsed electric field treatment .................................................................... 76 Packaging and Storage .................................................................................... 77 Microbial Stability ............................................................................................. 77 Volatile Extraction ............................................................................................. 78 Gas Chromatography-Mass Spectrometry Analysis ......................................... 78 Quantification of Apple Cider Volatiles ............................................................. 79 Sensory Evaluation .......................................................................................... 79 Statistical Analysis ............................................................................................ 80 Results and Discussion........................................................................................... 81 Microbial Stability During Storage .................................................................... 81 Volatile Composition ......................................................................................... 81 Odor Activity Values ......................................................................................... 82 Effect of Treatment and Storage on Volatiles ................................................... 83 Effect of Treatment and Storage on Odor Activity Values of Volatiles .............. 85 Aroma Sensory Studies .................................................................................... 86 Conclusion .............................................................................................................. 87 5 COMPARISON OF THERMAL AND NON-THERMAL TECHNIQUES ON GRAPEFRUIT JUICE STORAGE QUALITY UNDER EQUIVALENT PROCESS CONDITIONS ......................................................................................................... 92 6 Introduction ............................................................................................................. 92 Materials and Methods............................................................................................ 93 Determination of Equivalent Treatment Conditions .......................................... 93 Heat treatment ........................................................................................... 93 Ultraviolet treatment ................................................................................... 93 Pulsed electric field treatment .................................................................... 94 Radio frequency electric field treatment ..................................................... 94 Shelf Life Study ................................................................................................ 95 Grapefruit juice pasteurization ................................................................... 95 Packaging and storage .............................................................................. 95 Microbial assay .......................................................................................... 96 Pectin methyl esterase activity assay ........................................................ 96 Ascorbic acid assay ................................................................................... 97 Non enzymatic browning ............................................................................ 97 pH .............................................................................................................. 98 Brix ............................................................................................................. 98 Color .......................................................................................................... 98 Statistical Analysis ............................................................................................ 99 Results and Discussion........................................................................................... 99 Effect of Treatments on Microbial Inactivation .................................................. 99 Effect of Treatments on Microbial Stability During Storage ............................ 101 Effect of Treatments on Pectin Methyl Esterase Activity ................................ 102 Effect of Treatments on Non-enzymatic Browning ......................................... 104 Effect of Treatments on Ascorbic Acid Degradation ....................................... 105 Effect of Treatments on Color ......................................................................... 106 Effect of Treatments on pH, Brix and Total Acidity ......................................... 107 Conclusion ............................................................................................................ 107 6 IMPACT OF THERMAL AND NON-THERMAL PROCESSING TECHNOLOGIES ON AROMA OF RED GRAPEFRUIT JUICE: GC- OLFATOMETRIC COMPARSION ........................................................................ 118 Introduction ........................................................................................................... 118 Materials and Methods.......................................................................................... 119 Grapefruit Juice .............................................................................................. 119 Grapefruit Juice Processing ........................................................................... 120 Heat treatment ......................................................................................... 120 Non-thermal juice treatments .................................................................. 120 Packaging and storage ............................................................................ 120 Extraction of Grapefruit Juice Volatiles ........................................................... 121 Volatile Analysis of Grapefruit Juice Volatiles ................................................. 121 Sensory Evaluation ........................................................................................ 122 Screening and training of panelists .......................................................... 122 Test method ............................................................................................. 123 Statistical Analysis .......................................................................................... 124 Results and Discussion......................................................................................... 124 Effect of Treatment and Storage on Grapefruit Juice Volatiles ....................... 124 7 Gas Chromatography Olfactometry Profile of Grapefruit Juice ....................... 125 Gas Chromatography Olfactometry Profile Comparison of Fresh Untreated and Treated Juice at Week 0 ...................................................................... 128 Thermal treatment .................................................................................... 129 Ultraviolet treatment ................................................................................. 130 Pulsed electric field treatment .................................................................. 131 Radio frequency electric field treatment ................................................... 131 Gas Chromatography Olfactometry Comparison of Fresh Untreated and Treated Juice at Week 4 ............................................................................. 131 Sensory Evaluation ........................................................................................ 132 Conclusion ............................................................................................................ 133 7 CONCLUSION ...................................................................................................... 143 APPENDIX A CHANGE IN APPLE CIDER APPEARANCE DURING STORAGE ...................... 146 B CALIBRATION TABLE FOR APPLE CIDER VOLATILES .................................... 147 C GRAPEFRUIT JUICE VOLATILE CONCENTRATION ......................................... 148 D GRAPEFRUIT JUICE SENSORY RESULTS ....................................................... 152 E SAMPLE SENSORY BALLOT FOR DIFFERENCE FROM CONTROL TEST ...... 154 LIST OF REFERENCES ............................................................................................. 155 BIOGRAPHICAL SKETCH .......................................................................................... 170 8 LIST OF TABLES Table page 2-1 Time – temperature parameters for PE inactivation in citrus juices .................... 52 3-1 Change in pH and Brix values for fresh*, thermal, UV and PEF treated apple cider stored at 4 ºC for 4 weeks .......................................................................... 72 3-2 Change in Hunter color values** for fresh*, thermal, UV and PEF treated apple cider stored at 4 ºC for 4 weeks ................................................................ 73 4-1 Effect of thermal and non-thermal treatments on apple cider volatiles compared to fresh untreated cider after 4 weeks of storage at 4 ºC ................... 89 4-2 Effect of thermal and non-thermal treatments on odor activity values (OAV) of apple cider volatiles after 4 weeks of storage at 4 ºC ......................................... 91 5-1 Yeast & mold count in control, thermal, UV, PEF and RFEF treated grapefruit juice stored at 4 ºC for 4 weeks ........................................................................ 111 5-2 pH, Brix and total acidity (TA) values for control, thermal, UV, PEF and RFEF treated grapefruit juice stored at 4 ºC for 4 weeks ............................................ 117 6-2 GCO analysis results of pasteurized and unpasteurized grapefruit juice .......... 136 6-3 Calculated total aroma intensity values for pasteurized and unpasteurized grapefruit juice belonging to five odor categories ............................................. 138 6-4 GCO comparison of pasteurized grapefruit juice at week 4 to unpasteurized grapefruit juice at week 0 .................................................................................. 140 6-5 Results of ANOVA for mean values from difference from control test .............. 142 6-6 Difference in means between pasteurized and unpasteurized grapefruit juice . 142 6-7 Results of ANOVA of mean values from difference control test at week 4 ....... 142 6-8 Difference in means between pasteurized and unpasteurized grapefruit juice at week 4 .......................................................................................................... 142 B-1 Regression equation for standard compounds ................................................. 147 C-1 Volatile concentration (μg/L) in untreated (control) and treated grapefruit juice at week0 ........................................................................................................... 149 C-2 Volatile concentration (μg/L) in untreated (control week 0) and treated grapefruit juice at week 4 .................................................................................. 150 9 D-1 Difference from control data between hidden control (unpasteurized juice) and pasteurized juices (thermal, PEF, RFEF and UV) at week 0 ..................... 152 D-2 Difference from control data between hidden control (unpasteurized fresh juice ) and pasteurized juices (thermal, PEF, RFEF and UV) at ....................... 153 10
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