منبع پایان نامه درباره of، and، Figure

Supervisor:
Abdorreza Mohammadi Nafchi, PhD
by:
Maliheh Saeidi
November 2013
ACKNOWLEDGEMENT
I would like to express my gratitude and thank to my father for their endless love, support and patience.
I also would like to express my deep gratitude and thanks to my supervisor Dr Abdorreza Mohammadi Nafchi for his professional guidance, moral support and encouragement during the experimental work, detailed comments and editing throughout the writing process of this thesis.
I am also greatly indebted to my friends and technicians of laboratories in Azad University, Damghan branch for their help, support and friendship.
Special thanks also go to Professor Abd Karim Alias from Food Science Malaysia for his special supports.
TABLE OF CONTENTS
Acknowledgement ii
Table of Contents iii
List of Tables vi
List of Figures vii
Abstract 1
Chapter 1: Introduction 2
1.1 Background 3
1.2 Rational of study 5
1.3 Objectives of the study 5
1.4 Research Flowchart 6
Chapter 2: Literature Review 8
2.1 PHARMACEUTICAL CAPSULES 9
2.1.1 Pharmaceutical hard capsules 10
2.1.2 Manufacture of gelatin capsules 11
2.1.3 Properties of gelatin capsules 15
2.1.4 Alternatives to Gelatin 17
2.2. POLYSACCHARIDES STUDY 20
2.2.1 Starch 20
2.2.1.1 Composition and primary structure of starch 21
2.2.1.2 Morphology and ultra-structure of starch grains 24
2.2.1.3 Semi-crystalline structure of starch grains 27
2.2.1.4 Thermal transitions 30
2.2.1.5 Starch modification 35
2.2.1.6 Cassava 41
2.2.2 Carrageenan 53
2.2.2.1 Chemical Structure 53
2.2.2.2 Conformation of κ-carrageenan 54
2.2.2.3 Gelation of κ-carrageenan 60
2.2.2.4 Thermoreversibility of gels and rheological properties 61
2.3 POLYSACCHARIDE MIXTURES 65
2.3.1 Phase Behavior 65
2.3.2 Thermodynamic Incompatibility 66
2.3.3 Gels based on mixtures polysaccharides 68
2.3.3.1 Rheological properties 69
2.3.3.2 Rheology of blends of starch 70
Chapter 3: Materials and Methods 72
3.1 Materials 73
3.1.1 Gelatin 73
3.1.2 κ-carrageenan 73
3.1.3 Acid hydrolyzed hydroxypropylated cassava starch 73
3.2 Methods 74
3.2.1 Preparation of solutions 74
3.2.1.1 Gelatin solutions 74
3.2.1.2 Starch and κ-carrageenan solutions 74
3.2.2 Rheological properties 77
3.2.2.1 Flow properties 77
3.2.2.2 Viscoelastic properties 78
Chapter 4: Results and Discussions 79
4.1 Rheological behavior of gelatin 80
4.1.1 Gelatin solution at 50 °C 80
4.1.2 Sol-gel transitions 82
4.1.3 Viscoelastic properties of gelatin gels at 20 °C 86
4.2 Rheological behavior of starch-κ-carrageenan blends 90
4.2.1 Rheological behavior at 50 °C 90
4.2.1.1 Dually modified cassava starch (HHSS) 90
4.2.1.2 κ-carrageenan 95
4.2.1.3 Dually modified cassava starch/κ-carrageenan blends 96
4.2.2 Rheological behavior in sol-gel transitions (from 50 °C to 20 °C) 102
4.2.2.1 Influence of κ-carrageenan content 104
4.2.2.2 Influence of the different extents of starch hydrolysis 106
4.2.3 Rheological properties of gels at 20 °C 107
4.2.3.1 κ-Carrageenan gels 107
4.2.3.2 Composite gels 108
Chapter 5: Discussion and Conclusion 113
5.1 Synergy and gel state 114
5.1.1 Dually modified cassava starch and κ-carrageenan 114
5.1.2 Mixtures 115
5.2 Comparison with gelatin 120
5.2.1 Solution properties 120
5.2.2 Jellification 121
5.3 Conclusion and recommendation for future research 123
References 126
LIST OF TABLES
Table 2. 1: Properties and applications of modified starches. 35
Table 2. 2: Performance of starch slurry dewatering by a conventional centrifuge from a typical cassava starch factory. 51
Table 3.1: Compositions of the starch- κ-carrageenan solution 76
Table 4.1: Changes in viscosity of gelatin as a function of concentration. Experiments were performed at 50 °C 81
Table 4.2: Gelation temperatures, TGEL and melting temperature TM (G’= G”) during cooling from 50 to 25 °C and heating from 25 to 50 °C. The rate of heating or cooling was 1°C/min. Frequency: 1 rad/s. Strain amplitude: 1%. 86
Table 4.3: Viscosity of κ-carrageenan in different concentrations 95
Table 4. 4: Gelling temperatures (TGEL) and melting temperatures (TM) of κ-carrageenan alone and the mixture HHSS12-κ-carrageenan determined from cooling and heating ramps at 1 °C/min and 1 rad/s. 104
Table 4.5: Storage and loss moduli G’ and G” of κ-carrageenan alone and HHSS12-κC0.5 mixture determined from temperature ramps during cooling and heating at 1 °C/min by rheological measurements. Frequency: 1 rad/s 111
LIST OF FIGURES
Figure 1.1: Research flowchart 7
Figure 2. 1: Formation of hard gelatin capsules by dip molding 12
Figure 2. 2: Position fingers dipping during passage through the drying ovens 13
Figure 2. 3: Steps removing (a) trimming (b), and assembly of capsules (c). 14
Figure 2. 4: Water content at equilibrium of pharmaceutical hard empty gelatin capsules in relationship with the mechanical behavior. The capsules are stored at different relative humidities for two weeks at 20 ° C. 16
Figure 2. 5: Isothermal sorption-desorption capsules hard gelatin and HPMC at equilibrium at 25°C. 19
Figure 2. 6: Test for fragility of the capsules: the percentage of broken capsules according to their water content. a: resistance to pressure with capsules filled with corn starch. b: impact resistance with empty capsules. 19
Figure 2. 7: Structure of amylose 22
Figure 2. 8: Structure of amylopectin 23
Figure 2. 9: Grains of different starches observed in scanning electron microscopy SEM (magnification × 280) 24
Figure 2. 10: The different levels of grain starch 25
Figure 2. 11: Organization of starch grains in “blocklets” 27
Figure 2. 12: X-ray diffraction diagram for crystalline starch type A, B and C. 28
Figure 2. 13: Crystallinity of potato starch: influence of water content on the resolution of the diffraction pattern of X-rays 29
Figure 2. 14: Crystalline arrangement of double helices of amylose type A and B 30
Figure 2. 15: Variation of classical transitions of the potato starch as a function of water content 33
Figure 2. 16: Hydroxypropylation reaction 38
Figure 2. 17: Mass balance of cassava starch manufacturing process in a starch factory with a decanter. 47
Figure 2. 18: Mass balance of cassava starch manufacturing process in a starch factory without a decanter. 48
Figure 2. 19: Starch granules trapped in discharged pulp of cassava starch process. 49
Figure 2. 17: Ideal repeating units of λ-carrageenan (a) (R = H or SO3-), and (b) for ι- carrageenan (R1 = R2 = SO3-) and κ- carrageenan (R1 = H ; R2 = SO3-). 54
Figure 2. 18: Percentage of order of κ-carrageenan solution by polarimetry (0) and conductivity measurements (F) 55
Figure 2. 19: Change in transition temperature Tm at cooling κ-carrageenan based on the total concentration of CT different monovalent cations (1) Rb+, (2) Cs+, (3) K+ ,(4) NH4+, (7) N(CH3)4+ (8) Na+, (9) Li+ and divalent cations (5-6) Ba2+, Ca2+, Sr2+, Mg2+, Zn2+, Co2+ 57
Figure 2. 20: Phase diagram of κ-carrageenan representing the variation of transition temperature on cooling and heating according to the total concentration of potassium (Rochas, 1982; Rochas & Rinaudo, 1980). 59
Figure 2. 21: κ -Carrageenan gelation model, cation to promote gelation. (Morris et al., 1980) 60
Figure 2. 22: Variations of G’ and G” as a function of temperature for a concentration of 1% κ-carrageenan, Frequency 1 Hz, Tg: temperature of gelation, Tm: melting temperature. Cooling G’ (■), G” (•). Heating G’ (□), G” (◊). (Fernandes, Gonçalves & Doublier, 1992). 63
Figure 2. 23: Kinetics of evolution of κ-carrageenan at a concentration of 1%. Temperature is 25 ° C. Frequency 1Hz. G’ (■), G” (•). 64
Figure 2. 24: Phase diagram at 25 °C mixture of waxy hydroxypropyl starch/κ-carrageenan. 67
Figure 3.1: Phase diagram of κ-carrageenan representing the variation of transition temperature on cooling and heating according to the total concentration of potassium 75
Figure 4.1: Newtonian behavior of gelatin at 50 °C and 20% concentration. 80
Figure 4.2: Mechanical spectrum of 25% gelatin solution. G’: filled symbols, G”: empty symbols. Experiments were performed at 50 °C, strain amplitude was 1% 82
Figure 4.3: Storage and loss moduli GF, G, for a 25% gelatin sample during a cooling ramp. Temperature was ramped from 50 to 20 °C at 1°C/min. Frequency: 1 rad/s. Strain amplitude: 1% 84
Figure 4.4: Storage and loss moduli GF, G, as a function of temperature during a heating ramp of a 25% gelatin sample. Temperature was ramped from 25 °C to 50 °C at 1 °C/min. Frequency: 1 rad/s. Strain amplitude: 1% 85
Figure 4.5: Mechanical spectrum of 25% gelatin. G’: filled symbols, G”: empty symbols. The temperature was 20 °C. Strain amplitude: 1%. 87
Figure 4.6: Changes in modulus G’ and G” as a function of time for a 27% gelatin gel. Measurement temperature was 20 ° C. Frequency: 1 rad / s. Strain amplitude: 1%. 88
Figure 4.7: Changes in G’ as function of gelatin concentration. Data obtained after 6 h of time sweep measurement at 20 °C. Frequency: 1 rad/s. Strain amplitude: 1%. 89
Figure 4.8: Flow curves of hydrolyzed hydroxypropylated cassava starch dispersions at a concentration of 25% (g/g): HHSS6 (●), HHSS12 (■), HHSS18 (o), HHSS24 (/). Measurements were performed at 50 °C 91
Figure 4.9: Flow curves for dually modified cassava starch (HHSS12) dispersions at a concentration of 25% (g/g). Measurement was performed at 50 °C 92
Figure 4.10: Flow curves of dispersions of hydroxypropyl cassava starch HHSS12 at concentrations of 20% (■), 23% (●) and 25% (▲). Temperature was 50°C 93
Figure 4.11: Mechanical spectra of different

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