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Definition of Chocolate THE IMPACT OF NUT INCLUSIONS ON PROPERTIES AND STABILITY OF DARK CHOCOLATE by ANDREA ROSSI-OLSON A Dissertation submitted to the Graduate School-New Brunswick Rutgers, The State University of New Jersey in partial fulfillment of the requirements for the degree of Doctor of Philosophy Graduate Program in Food Science written under the direction of Karen M. Schaich and approved by ________________________ ________________________ ________________________ ________________________ ________________________ New Brunswick, New Jersey May 2011 2011 Andrea Rossi-Olson ALL RIGHTS RESERVED ii ABSTRACT OF THE DISSERTATION The Impact of Nut Inclusions on Properties and Stability of Dark Chocolate By ANDREA ROSSI-OLSON Dissertation Director: Karen M. Schaich Chocolate bars have become increasingly gourmet in the types of chocolate used and addition of a variety of inclusions such as nuts, fruits, and cereal grains. These factors all have marked impacts on shelf life, as do storage conditions and handling. Understanding interactions among ingredients is crucial for developing improved approaches to maximize shelf life and maintain quality of chocolate products over time. The most noticeable defect in chocolate is bloom, which presents itself as a white haze on the chocolate surface. Bloom is inevitable over time, but the goal is to prolong its onset as long as possible. One of the many theories proposed to explain the complex phenomenon of bloom is that migration of incompatible fats, specifically from nuts, imposes a second crystal phase, dissolves some cocoa butter, and causes a rearrangement of cocoa butter crystals to highly structured, high melting point forms that deposit on the chocolate surface. Nuts readily develop rancidity and introduce off-flavors into chocolate. Migration of oil from nuts also affects the chocolate matrix itself, altering snap, molding, and gloss as well as crystal form and texture stability. Although nuts are extensively added to chocolate as inclusions, very little basic research has focused on how different nuts affect chocolate properties and stability. iiiii To provide a base of fundamental information that can be applied to improving a wide variety of chocolate products, this study follows migration of oils from roasted monounsaturated almonds and polyunsaturated walnuts into dark chocolate with and without anhydrous milk fat as a crystallization modifier. Oil migration kinetics, nut fatty acid and antioxidant profiles, as well as chocolate melting patterns, crystal forms and shifts, texture properties (snap), bloom, lipid oxidation products and oxidative storage stability, and sensory qualities are being measured to determine the major failure mode (texture, flavor, or bloom) in chocolate. Current industry theories are based primarily on unsaturation and oxidative instability of nuts, but there is little data available. An investigation of nut fatty acid profiles and effects on chocolate crystallization may offer new ways to use nuts that previously have been avoided. iiiiv ACKNOWLEDGEMENTS It has been a long journey to achieve this milestone. I have many people to thank for their support. I would first like to thank my advisor Dr. Karen Schaich, who has worked with me through three degrees and has always been encouraging and inspiring. Thank you for your flexibility and your mentorship. Next I would like to acknowledge Mars Inc., especially Dr. Christopher Johnson. Dr. Johnson has taught me a plethora of analytical techniques, but also the basics to being a great investigator. I appreciate your practical approach to research and its application and your patience and support through this project. I would also like to thank the following Mars Inc. associates for training me in the analytical techniques I needed for my research: Dana Carpenter (tocopherols-HPLC), Haroon Malak (FAME-GC and XRD), Paul Spitz (DSC), Julia Li (Peroxide Value, Alkenals and Proanthocyanidins), James Zimmer (Texture Analysis), John Munafo and Vivianna Chaparro (SAFE analysis), Maria Lenzi and Karl Ritter (Colorimeter) and Tom Collins and Rodrigo Campos for assistance with model system set up. I would also like to thank Barry Glazier, Doug Valkenberg and David Hausman for chocolate making instruction, Mark Kline for nut roasting assistance, Charlotte Liang for sensory testing guidance as well as the Mars Sensory team for descriptive analysis participation and Wendy Kessell for chocolate and bar making assistance. Lastly, I would like to thank my family and my husband Dain for allowing me to follow my dreams while being the perpetual student. This has been a very long road and I am grateful to have you all by my side along this journey. v iv TABLE OF CONTENTS Abstract ii Acknowledgement v Table of Contents vi List of Tables xii List of Figures xiv 1. Introduction 1 2. Literature Review 4 2.1. Chocolate Processing 10 2.1.1. Chocolate Components Structure and Function 10 2.1.1.1. Cocoa butter 10 2.1.1.2. Cocoa liquor 12 2.1.1.3. Milk Products 12 2.1.1.4. Milk Fat 12 2.1.1.5. Milk Protein 14 2.1.1.6. Emulsifiers 14 2.1.1.7. Sugar 15 2.1.2. Molecular interactions responsible for chocolate properties and stability 15 2.1.2.1. Impact of Particle Size 15 2.1.2.2. Cocoa butter crystallization / Texture in chocolate 17 vvi 2.1.2.2.1. Fat Migration in Chocolate 22 2.1.2.2.2. Effect of Minor Lipids 24 2.1.2.2.3. Compatibility 25 2.1.2.3. Bloom 29 2.1.2.3.1. Bloom Theories 31 2.1.2.3.2. Phase Separation 31 2.1.2.3.3. Polymorphic Transitions 31 2.1.2.3.4. Fat Migration 32 2.1.2.3.5. Bloom in Filled Pieces 33 2.1.2.3.6. Chocolate Coatings 36 2.1.2.3.7. Impact of Chocolate Microstructure 37 2.1.2.3.8. Effect of Milk Fat 38 2.1.2.3.9. Effect of Storage 40 2.2. Effects of nuts on chocolate properties 40 2.2.1. Nut Varieties 43 2.2.1.1. Peanuts 43 2.2.1.2. Hazelnuts 44 2.2.1.3. Walnuts 46 2.2.1.4. Macadamia 48 2.2.1.5. Cashews 48 2.2.1.6. Almonds 49 2.2.2. Properties of Nuts that Affect Their Use as Chocolate Bar Inclusions 51 2.2.2.1. Impact of Roasting 52 vivii 2.2.2.2. Impact of Chop Size 54 2.2.2.3 Impact of Storage and Processing 55 2.2.2.4. Impact of Nut Lipids on Chocolate Stability 55 2.2.2.5. Interaction with Chocolate 55 2.2.2.5.1. Oil Migration 55 2.2.2.5.2. Lipid Oxidation 56 2.2.2.6. Antioxidants in Nuts 59 2.2.2.7. Nuts and Health 62 2.3. Measuring Quality Parameters in Chocolate 62 2.3.1. Current Detection Methods 62 2.4. Challenges and Trends 63 2.5. Knowledge Gaps 67 3. Hypothesis and Objectives 68 3.1. Hypothesis 68 3.2. Goals and Objectives of This Study 68 4. Preliminary Experiments to Establish Standards and Methodology 71 4.1. General approach and observations 71 4.2. Experimental Methods for Raw Ingredient Testing and Evaluation 76 4.4. Evaluation of Raw Materials 76 4.5. Ingredient Processing 80 4.5.1. Nut Roasting 80 4.3.2. Nut Grinding 80 4.3.3. Sensory Analysis of Roasted Nuts 82 viiivii 4.3.4. Chocolate Processing 82 4.3.4.1. Chocolate Ingredients 84 4.3.4.2. Nut Inclusion Specifications 84 5. Experimental Methods and Procedures 85 5.1. Overall Experimental Design 85 5.1.1. Model Systems 89 5.2. Analytical Procedures 93 5.3. Theory of Methodology, Information Expected and Detailed Procedures 94 5.3.1. Particle Size 94 5.3.2. FAME Gas Chromatography 95 5.3.3. Colorimeter 99 5.3.4. Texture Profile Analysis 101 5.3.5. DSC 102 5.3.6. Lipid Oxidation 106 5.3.6.1. Peroxide Values 107 5.3.6.2. Secondary Products 111 5.3.6.3. Rancimat 113 5.3.6.4. Tocopherols 116 5.3.6.5. Other Antioxidants 121 5.3.6.6. Crystallography X-Ray Diffraction 127 5.3.6.7. SAFE Analysis 131 5.3.6.8. Sensory 134 5.3.6.9. Model System 139 viiiix 5.3.7.0. Accelerated Shelf Life 140 6. Results 141 6.1. Nut Stability Testing 141 6.1.1. Oxidative Stability 141 6.1.2. Tocopherols 150 6.1.3. Procyanidins 159 6.1.4. Sensory 161 6.2. Stability of Chocolate Bars with Almonds and Walnuts 166 6.2.1. Lipid Oxidation Products 166 6.2.2. SAFE Test 175 6.2.3. Tocopherols 180 6.2.4. Proanthocyanins 184 6.3. Fat Migration from Nuts to Chocolate 188 6.3.1. FAME-GC Data 188 6.3.2. Texture Analysis for Softening Due to Fat Migration 194 6.3.3. DSC evidence of multiple crystal forms 199 6.4 Quantification of Bloom 215 6.4.1. Accelerated Chamber 220 6.5. Sensory Results 221 6.6. Model System 229 6.6.1. FAME Results 230 6.6.2. DSC Results 230 6.6.3. XRD Results 235 ixx 7. Summary and Integration of Results 245 8. Significance and Impact of Results 259 9. Future Work 261 10. References 262 11. Curriculum Vita 271 xxi LIST OF TABLES 1. Fatty Acid Composition of Cocoa Butters 11 2. Fatty Acid Profile of Milk Fat 12 3. Polymorphs of Cocoa Butter 19 4. Fatty Acid and Total Fat Content of Nuts 42 5. Typical Shelf Life Values for Almonds 51 6. Volatile Carbonyl Compounds formed by Autoxidation 59 7. Average Polyphenol Content of Almonds and Walnuts 62 8. Roasting Conditions Producing Acceptable Nuts 72 9.
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