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Low Temperature Processes on Cellular Materials Related to Foods

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Low Temperature Processes on Cellular Materials Related to Foods Impact of High Pressure - Low Temperature Processes on Cellular Materials Related to Foods vorgelegt von Diplom-Ingenieur Oliver Schlüter von der Fakultät III – Prozesswissenschaften der Technischen Universität Berlin zur Erlangung des akademischen Grades Doktor der Ingenieurwissenschaften - Dr.-Ing. - genehmigte Dissertation Promotionsausschuss: Vorsitzender: Prof. Dr.-Ing. Dr. e. h. Friedrich Meuser Berichter: Prof. Dr. Dipl.-Ing. Dietrich Knorr Berichterin: Dir’in. u. Prof’in. Dr.-Ing. Heike Schuchmann Tag der wissenschaftlichen Aussprache: 28.07.2003 Berlin 2003 D 83 ACKNOWLEDGEMENTS This thesis is an extract of my work during the years from 1998 to 2003 in the Department of Food Biotechnology and Food Process Engineering, Berlin University of Technology and I would like to take this opportunity to thank the people who contributed in all sorts of ways to this thesis. First of all I am very grateful to Prof. Dr. Dipl.-Ing. Dietrich Knorr for inspiring me to focus on high pressure-supported phase transitions, for his constant enthusiasm concerning this interesting field of research and his extensive scientific support. I would like to express my gratitude to Dir’in. and Prof’in. Dr.-Ing. Heike Schuchmann, her generous reviewing with critical comments and alternative views greatly added to the quality of this thesis. I would also like to thank Prof. Dr.-Ing. Dr. e. h. Friedrich Meuser for being the chairman of my thesis defence. I wish to express my heartfelt thanks to Dr.-Ing. Volker Heinz and Dr. Ing. Alexander Angersbach for being a constant source of help, encouragement and inspiration to me. I especially acknowledge the substantial contribution of Mr. Sujith George, Mr. Edwin Ananta, Mr. Cornelius Luscher and Mr. Gabriel Urrutia Bennet. I gratefully acknowledge the help rendered by all my friends and colleagues, especially Mr. Stefan Boguslawski. Furthermore, I would like to acknowledge Dr. Carsten Meyer and Dr. Reinhard Schubring for the fruitful co-operation within the “Hochdruck-Verbundprojekt” and the impressive experiences during our high pressure experiments on the Atlantic ocean. The financial support provided by the German Research Foundation (DFG), the German Federal Ministry of Education and Research (BMBF) and the European Commission (EC) is thankfully acknowledged. III Dedicated to my inner source of love, sunshine and lightness: Christine, Paul Linus and Julina Fee IV CONTENTS LIST OF NOTATIONS VIII ABSTRACT XI KURZFASSUNG XII 1 INTRODUCTION 1 2 THEORY AND LITERATURE REVIEW 8 2.1 LOW TEMPERATURE PRESERVATION 8 2.1.1 PHASE TRANSITIONS 8 2.1.2 PRINCIPLE AND PROCESSING STEPS 11 2.1.3 PRODUCTS AND FREEZING SYSTEMS 13 2.1.4 QUALITY AND SAFETY ASPECTS 16 2.1.5 SUBSEQUENT THAWING 19 2.1.6 HEAT TRANSFER AND MODELLING 21 2.2 APPLICATION OF HIGH HYDROSTATIC PRESSURE 28 2.2.1 GENERAL ASPECTS 28 2.2.2 PHYSICAL PROPERTIES OF WATER 30 2.2.3 WATER-ICE TRANSITION 32 2.2.4 BIOMOLECULAR COMPOUNDS 35 2.2.5 CELLULAR SYSTEMS 37 2.3 HIGH PRESSURE - LOW TEMPERATURE PROCESSES 38 2.3.1 INDUCTION OF PHASE CHANGES 38 2.3.2 PRESSURE SUPPORTED FREEZING 39 2.3.3 PRESSURE SUPPORTED THAWING 42 2.3.4 MODELLING OF HIGH PRESSURE SUPPORTED FREEZING/THAWING 45 2.3.5 SUBZERO TREATMENT IN THE LIQUID STATE 48 2.3.6 SPECIAL APPLICATIONS 49 2.3.7 REQUIREMENTS FOR THE TECHNICAL EQUIPMENT 50 3 MATERIAL AND METHODS 54 3.1 TEST SAMPLES 54 3.1.1 POTATO TISSUES 54 3.1.2 FISH FILLETS 54 3.1.3 MICROORGANISMS 55 3.2 HIGH PRESSURE UNITS 55 3.2.1 MULTI-VESSEL-SYSTEM 55 3.2.2 LOW TEMPERATURE SYSTEM I57 3.2.3 LOW TEMPERATURE SYSTEM II 58 3.2.4 PILOT SCALE SYSTEM I60 3.2.5 PILOT SCALE SYSTEM II 61 3.3 PROCESS EVALUATION 61 3.3.1 PHASE TRANSITION POINTS 61 3.3.2 DESCRIPTION OF MELTING CURVES 63 V CONTENTS 3.3.3 CALCULATION OF PHASE TRANSITION TIMES 64 3.3.3.1 Modelling 64 3.3.3.2 Thermodynamic properties 64 3.3.3.3 Stability criteria 65 3.3.3.4 Treatment & procedure 66 3.4 QUALITY ASSESSMENT 68 3.4.1 PLANT DERIVED TISSUE 68 3.4.1.1 High pressure treatments 68 3.4.1.2 Impedance measurement 69 3.4.1.3 Texture measurement and analyses 70 3.4.1.4 Colour measurement and visual appearance 71 3.4.1.5 Thermal analyses 71 3.4.2 ANIMAL DERIVED TISSUE 72 3.4.2.1 Thawing experiments 72 3.4.2.2 Water holding capacity 72 3.4.2.3 Thawing loss 72 3.4.2.4 Sensory tests 73 3.4.2.5 Texture analyses 73 3.4.2.6 Colour changes 73 3.4.2.7 Calorimetric analyses 73 3.4.2.8 Viable count of microorganisms 73 3.4.2.9 Parasites 74 3.4.2.10 Statistical analysis 74 3.4.3 INACTIVATION OF MICROORGANISMS 74 3.4.3.1 Sample preparation 74 3.4.3.2 Treatment 75 3.4.3.3 Enumeration of viable cells 75 3.4.3.4 Regression analysis 76 4 RESULTS AND DISCUSSION 78 4.1 PROCESSING CRITERIA FOR CONTROLLED PRESSURE-SUPPORTED PHASE TRANSITIONS 78 4.1.1 INTRODUCTION 78 4.1.2 PHASE TRANSITION LINES OF PLANT TISSUE 78 4.1.2.1 Melting curve ice I 78 4.1.2.2 Melting curve ice III 80 4.1.2.3 Melting curve ice V 81 4.1.2.4 Solid-solid phase boundary 83 4.1.2.5 Phase diagram 84 4.1.2.6 Liquid-solid contour plot 85 4.1.3 MODELLING HIGH PRESSURE SUPPORTED FREEZING OF PLANT TISSUE 87 4.1.3.1 Relevant aspects 87 4.1.3.2 Pressure assisted freezing to ice I 88 4.1.3.3 Pressure assisted freezing to ice III 91 4.1.3.4 Pressure assisted freezing in metastable zones 92 4.1.3.5 Pressure shift freezing 94 4.1.3.6 Discussion on temperature profiles 95 4.1.3.7 Supercooling and instantaneously formed ice 97 4.1.4 HIGH PRESSURE SUPPORTED THAWING OF PLANT TISSUE 99 4.1.4.1 Temperature evolution during pressure-assisted thawing 99 4.1.4.2 Modelling thermophysical properties 100 VI CONTENTS 4.1.4.3 Calculation of pressure-assisted thawing times 103 4.1.4.4 Impact of sample size 105 4.1.4.5 Prediction of thawing profiles 107 4.1.4.6 Pressure assisted and pressure induced thawing 108 4.1.4.7 Critical parameters for pressure supported melting 109 4.2 QUALITY AND SAFETY ASPECTS OF HIGH PRESSURE - LOW TEMPERATURE PROCESSES 113 4.2.1 IMPACT OF HIGH PRESSURE-LOW TEMPERATURE PROCESSING ON PLANT TISSUE 113 4.2.1.1 Characteristic pressure and temperature plots 113 4.2.1.2 Indication of phase transitions by impedance spectra 116 4.2.1.3 Process induced changes of the cell membrane 118 4.2.1.4 Effects of phase transitions on textural properties 120 4.2.1.5 Evaluation of changes in colour and visual appearance 122 4.2.2 IMPACT OF HIGH PRESSURE THAWING ON ANIMAL TISSUE 125 4.2.2.1 Evaluation of the required processing time 125 4.2.2.2 Effects of thawing and subsequent heating on sensory attributes 126 4.2.2.3 Pressure and heat induced changes in texture 127 4.2.2.4 Evaluation of processing effects on colour and proteins 128 4.2.2.5 Treatment effects on water loss and pH value 130 4.2.2.6 Effect on microorganisms and parasites 132 4.2.3 IMPACT OF HIGH PRESSURE-LOW TEMPERATURE PROCESSING ON MICROORGANISMS 134 4.2.3.1 Inactivation kinetics of Listeria innocua 134 4.2.3.2 Bacteria inactivation in frozen solutions 136 4.2.3.3 Influences of p,T-combinations on the rate constant 137 4.2.3.4 Pressure resistance of Listeria innocua in food matrix 138 5 SUMMARY AND CONCLUSION 140 5.1 MODELLING OF HIGH PRESSURE SUPPORTED WATER-ICE TRANSITIONS 140 5.2 DEFINITION OF METASTABLE STATES IN THE PHASE DIAGRAM 143 5.3 IMPROVEMENT IN HIGH PRESSURE – LOW TEMPERATURE PROCESSES 144 5.4 IMPACT OF PROCESS PARAMETERS ON QUALITY AND SAFETY ASPECTS 146 5.5 PERSPECTIVES OF HIGH PRESSURE – LOW TEMPERATURE PROCESSES 149 6 REFERENCES 154 LIST OF PUBLICATIONS 170 VII LIST OF NOTATIONS LIST OF NOTATIONS Symbols α thermal diffusivity m2 s-1 α thermal expansion coefficient K-1 β isothermal compressibility Pa-1 λ thermal conductivity W m-1K-1 ϕ electrical conductivity µS cm-1 ρ density kg m-3 Θ temperature quotient - α, χ adjustable coefficient (equation 3.1) - β, δ adjustable exponent (equation 3.1) - -1 ∆Gact activation energy J mol ∆H enthalpy J ∆Tsup degree of supercooling K 3 -1 ∆Vact reaction volume cm mol µ viscosity Pa s A peak parameter (equation 3.7) A constant (equation 2.10) - 2 Ai cross-sectional area of a cylindrical sample before mm compression 2 Ax heat flux area normal to the direction of heat flow m B scale parameter (equation 3.5, 3.6, 3.7) B constant (equation 2.10) - Bi Biot number - C reaction order C shape parameter (equation 3.5, 3.6, 3.7) -1 -1 cp specific heat at constant pressure J kg K -3 eq rate of heat generation per unit volume W m F force N Fo Fourier number - Fp fractional pore area % G Gibbs energy J mol-1 H sample height mm H surface heat transfer coefficient W m-2K-1 J temperature dependence - K rate constant s-1 K equilibrium constant - k1,2,3...20 coefficients - L latent heat J kg-1 lc length of the cell m lm thickness of the cell membrane m mi mass of ice g mw mass of liquid water g N nucleation rate mol-1 s-1 -1 N0 initial number of cells ml o1,2,3 adjustable coefficients (eqn.
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