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Rheology and Thermodynamics of Starch-Based Hydrogel –Mixtures

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Rheology and Thermodynamics of Starch-Based Hydrogel –Mixtures RHEOLOGY AND THERMODYNAMICS OF STARCH-BASED HYDROGEL –MIXTURES DISSERTATION zur Erlangung des Grades eines „Doktor der Naturwissenschaften“ im Promotionsfach Chemie am Fachbereich Chemie, Pharmazie und Geowissenschaften der Johannes Gutenberg -Universität in Mainz Natalie Ruß geb. in Kirchheim -Bolanden Mainz, April 2016 1. Berichterstatter: Prof. Dr. Thomas A. Vilgis 2. Berichterstatter: PD Dr. Wolfgang Schärtl Tag der mündlichen Prüfung: 17. Mai 2016 Prüfungskommission: Prof. Dr. Thomas A. Vilgis PD Dr. Wolfgang Schärtl Prof. Dr. Angelika Kühnle Prof. Dr. Heiner Detert “A Thing is a Thing, not what is said of that Thing.” II Abstract Abstract The present work presents two different ways to achieve physically modified tapioca starch and the influence on mechanical properties of an aqueous starch paste is investigated. A completely cold soluble tapioca starch powder is produced by spray drying a previously gelatinized starch paste. Rehydrating the received white powder forms a viscous paste with significant loss in elasticity. Heating of a native tapioca starch suspension in contrast yields highly viscous paste with dominating elastic behavior. The combination of the spray dried tapioca starch with nongelling food hydrocolloids, such as xanthan gum, ι-carrageenan, and guar gum restores the mechanical properties and creates new starch-based thickening agents with stable structure. Rheological measurements of a gelatinized native tapioca starch paste compared to a rehydrated paste made from the spray dried starch show significant differences in viscosity and viscoelastic properties, which depend on temperature, amplitude, frequency, or shear rate. Further rheological, optical, and scattering investigations indicate weakening of the amylose network structure generated by the harsh shear and heat conditions during the spray drying process. The addition of water soluble hydrocolloids stabilizes the degraded gel structure by different mixing behaviors. According to the molecular nature of the added hydrocolloids, such as chain flexibility or charge distribution, different phase behavior in the starch-based composite system is induced. Thus, the stepwise replacement of starch by hydrocolloids influences the mechanical properties to various extents. The mixtures of spray dried tapioca starch and hydrocolloids have hydrocolloid dominated functional properties, and mixing the cold soluble tapioca starch with xanthan gum, ι-carrageenan, or guar gum on dry basis, a thickening effect with a weak gel character can be easily produced by hydration without heating. Depending on the desired application, the mechanical properties and texture can be controlled and tuned by the choice of hydrocolloid and by varying the mixture composition. Amylose and ι- carrageenan molecules are thermodynamically compatible, and a stable and well-mixed phase is formed. The mixture with xanthan gum and guar gum results in a phase separation where the hydrocolloid molecules separate into local domains. Phase separation is induced by thermodynamic incompatibility and mutual exclusion effects between amylose and xanthan or guaran molecules. The different phase behavior in the mixed systems is supported by confocal laser scanning microscopy and by covalent labeling of the hydrocolloids with specific fluorescence dyes. Kurzfassung III Kurzfassung In der vorliegenden Arbeit werden zwei Methoden der physikalischen Modifikation an Tapiokastärke und deren Einflüsse auf die mechanischen Eigenschaften einer wässrigen Dispersion präsentiert. Dazu wird zunächst eine vollständig kaltlösliche Tapiokastärke durch Sprühtrocknung einer zuvor gelatinisierten Stärkepaste hergestellt. Das erhaltene weiße Pulver bildet nach Resuspension eine schwach viskose Dispersion aus und zeigt einen deutlichen Verlust des Elastizitätsmoduls. Native Tapiokastärke bildet hingegen, nach ausreichender Wärmezufuhr, in wässriger Suspension eine hochviskose Paste mit dominierenden elastischen Anteil aus. Durch Zugabe von nichtgelierenden, wasserlöslichen Hydrokolloiden, wie Xanthan, ι-Carrageen oder Guar, können die viskoelastischen Eigenschaften der nativen Stärkepaste zurückgewonnen werden wodurch die Herstellung von neuen und stabilen stärkebasierten Verdickungsmitteln ermöglicht wird. Rheologische Untersuchungen der Viskosität und der viskoelastischen Eigenschaften einer gelatinisierten nativen Stärkepaste im Vergleich zu einer rehydrierten Paste der sprühgetrockneten Stärke, zeigen in Abhängigkeit von Temperatur, Amplitude, Frequenz und Scherrate deutliche Unterschiede. Durch zusätzliche rheologische und optische Analysen, sowie verschiedenen Streuungsversuchen kann eine deutliche Schwächung des Amylosenetzwerks, verursacht durch die hohe Scher- und Hitzebelastung während des Sprühtrocknungsprozesses, aufgezeigt werden. Der Einsatz der wasserlöslichen Hydrokolloide stabilisiert die Gelstruktur durch unterschiedliche Mischungsverhältnisse. Je nach molekularer Beschaffenheit der Hydrokolloide, wie Kettenflexibilität oder Ladungsverteilung, kann in den stärkebasierten Kompositsystemen verschiedenes Phasenverhalten generiert werden. Dabei können die mechanischen Eigenschaften des Mischsystems durch schrittweises Ersetzen von sprühgetrockneter Stärke unterschiedlich stark beeinflusst werden. Die Mischungen aus sprühgetrockneter Tapiokastärke und Hydrokolloiden zeigen deutlich Hydrokolloid dominierte funktionelle Eigenschaften, wodurch ein Verdickungseffekt mit schwachem Gelcharakter bereits ohne Wärmezufuhr induziert werden kann. Je nach gewünschter Anwendung können so die mechanischen Eigenschaften des Mischsystems durch die Wahl des entsprechenden Hydrokolloids und durch die Mischungskomposition angepasste werden. Zwischen Amylose- und ι-Carrageenmolekülen kann eine gewisse thermodynamische Kompatibilität gefunden werden, wodurch eine gemischte Phase mit stabiler Netzwerkstruktur aufgebaut wird. In der Mischung mit Xanthan und Guar hingegen, resultiert eine Phasenseparation, in der sich die Hydrokolloidmoleküle in lokalen Domänen separieren. Diese Phasenseparation ist durch molekulare Inkompatibilität und gegenseitige Ausschlusseffekte bedingt. Mit Hilfe von konfokaler Laserscanning Mikroskopie und durch das kovalente Färben der Hydrokolloide mit Fluoreszenzfarbstoffen, kann das unterschiedliche Phasenverhalten in den Kompositgelen nachgewiesen werden. IV Acknowledgment Acknowledgment First of all, I would like to thank my supervisor Prof Thomas A. Vilgis who has supported and encouraged me and my research during the last nine years. A profound thank you for the motivation and meaningful support throughout my whole studies and along this sometimes very exhausting way. I will always be grateful for showing and providing me a deeper insight on food and its physicochemical approach, which enriched my expertise in exceptional manner and inspired my personal handling with food. Many thanks also to Prof Kurt Kremer who put me up in his Theory Group and who has always supported the Food science group with all specific projects. Special thanks also to PD Wolfgang Schärtl from the University Mainz for supervising this thesis and for supporting this project with the superior master thesis of Thomas Limbach. At this point, also many thanks to Thomas Limbach for the brave acceptation of this very complex systems. I also want to thank the other members of my committee, Prof Angelika Kühnle and Prof Heiner Detert. Exceptional thanks go out to Birgitta Zielbauer for her painful help, patience, and endurance. Due to her special expertise and practical experience, many questions and problems could be successfully solved. I am really indebted for her spared time and assistance with different experiments. I also would like to thank some special colleagues of the MPIP for generous support with some technical applications: Andreas Hanewald for the fruitful technical support with the rheometer; Kaloian Koynov and Andreas Best for providing the CLSM and for helpful discussions concerning the evaluation of the CLSM images; and Kristin Mohr and Christiane Rosenauer for intensive help with some polymer analytical challenges. In addition, special and cordial thanks to Thomas Wagner and Jürgen Thiel for their help and counsel since the beginning of my MPIP’s career. A deep thank you also to Steffen Beccard, Marta Ghebremedhin and Doris Kirsch not only for the work referred help, but also for the very pleasant and funny atmosphere; a special and deep bow to Steffen for the shared struggles during our entire studies. I also Acknowledgment V would like to thank some former Foodies, Sania Maurer, Felix Bröcker, Gustav Waschatko, Julia Mann, and Johannes Franz for many scientific and culinary discussions and shared kitchen experiences. I am deeply grateful for my friends and family who have encouraged and loved me; I am so fortunate you are in my life and I am humbled by your friendship and kindness. In particular I will thank my parents and my best friend, you know who you are, for their mentorship, honest feedback and endless love which meant the world to me. They never let me forget that life and love matters the most. VI Content Content Abstract ........................................................................................................................... II Kurzfassung .................................................................................................................. III Acknowledgment .......................................................................................................... IV
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