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Different Strategies to Improve the Functionality of Biodegradable Films

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Different Strategies to Improve the Functionality of Biodegradable Films UNIVERSITAT POLITÈCNICA DE VALÈNCIA INSTITUTO UNIVERSITARIO DE INGENIERÍA DE ALIMENTOS PARA EL DESARROLLO Different strategies to improve the functionality of biodegradable films based on starch and other polymers DOCTORAL THESIS Presented by: Amalia I. Cano Embuena Supervisors: Chelo Gónzalez Martínez Amparo Chiralt Boix Maite Cháfer Nácher Valencia, September 2015 DEPARTAMENTO DE TECNOLOGÍA DE ALIMENTOS INSTITUTO UNIVERSITARIO DE INGENIERÍA DE ALIMENTOS PARA EL DESARROLLO Dª. Chelo Gónzalez Martínez y Dª. Amparo Chiralt Boix, Catedráticas de Universidad y Dª. Maite Cháfer Nácher, profesora titular de Universidad, pertenecientes al Departamento de Tecnología de alimentos de la Universitat Politècnica de València. CONSIDERAN: que la memoria titulada “DIFFERENT STRATEGIES TO IMPROVE THE FUNCTIONALITY OF BIODEGRADABLE FILMS BASED ON STARCH AND OTHER POLYMERS” que presenta Dª. Amalia Isabel Cano Embuena para aspirar al grado de Doctor por la Universitat Politècnica de València, reúne las condiciones adecuadas para constituir su tesis doctoral, por lo que AUTORIZAN a la interesada para su presentación. Valencia, 1 de Septiembre de 2015 Fdo. Chelo González Martínez Fdo. Amparo Chiralt Boix Fdo. Maite Cháfer Nácher Directora de Tesis Directora de Tesis Directora de Tesis A toda mi familía, Y en especial a Jorge, Agradecimientos A Amparo Chiralt por concederme la oportunidad de formar parte del grupo de “films”. Ha sido un placer poder trabajar junto a un referente internacional en el ámbito de la investigación como tú. Gracias por tus aportes científicos y técnicos, por tu paciencia y dedicación, y por permitirme aprender y trabajar a tu lado. A Chelo González, tu apoyo durante estos cuatro años, la fuerza que me has transmitido para ir hacia delante, tus conocimientos científicos y las oportunidades que me has brindado para iniciarme en la investigación a nivel nacional e internacional son tan sólo algunas de las cosas que tengo que agradecerte. Gracias también por toda la confianza depositada en mí durante estos años y por el apoyo personal. A Maite Cháfer por haberme introducido en el área de la investigación dándome la oportunidad de conocer al grupo de “films”. Tu apoyo profesional y personal y tu positividad frente a los problemas han sido de gran ayuda. Gracies! Al Profesor José María Kenny de la Università degli Studi di Perugia (Italia) y a todo su grupo de investigación. Especialmente a la Dra. Elena Fortunati y a Francesca Luzzi por su ayuda y colaboración durante y después de la estancia. Grazie mille! Thanks to Dr. Kristberg Kristbersoon for giving me the opportunity to stay at the Innovation Center of Iceland. I also want to thank my colleague Ragnhildur Einarsdóttir for all the help received during those 3 months. A todos los compañeros del laboratorio con los que he coincidido, vuestros ánimos y consejos han hecho que estos cuatro años hayan sido una gran experiencia. Mª José, Jeannine, Rodrigo, Justine y Raquel, de todos vosotros me llevo algún momento especial. Marco, Marta y María, gracias por ayudarme a aprender a enseñar. Olga, Anna y Emma, gracias por vuestras reflexiones y por ayudarme a desconectar cuando más lo necesitaba. Alberto, gracias por tus explicaciones sobre el mundo de los envases y por tu colaboración en la Tesis. Clara, gracias por estar siempre a punto para ayudarme y hacerme la vida más fácil con tus consejos. Neus y Ángela, me habéis ayudado tanto con los problemas a nivel experimental como personal, gracias por vuestro apoyo. A las compañeras de los laboratorios vecinos por la ayudada brindada para poder llevar a cabo la Tesis. En especial a Susana y a Ángela, habéis sido grandes compañeras y mejor amigas, gracias por vuestra confianza, vuestros consejos y por las largas conversaciones por Skype durante las estancias, ¡nunca podré olvidarlas! A todos mis amigos, Bárbara, Silvia, Jordi, Susana, Ampy, Javi, Ruth, Carol, Gonzalo, Laury, Jose, Chelo, Carlos, Gloria, Marieta, Víctor, María, Paquito y en especial a Lorena, vuestro apoyo continuo y confianza en mí ha sido una de las fuerzas impulsoras de esta Tesis. A mis dos familias, sin vuestro apoyo esta Tesis no habría sido posible. En especial a Arturo, Mónica, José, Susana, Genaro, Merche y Arturo, nunca habéis puesto objeción a mis decisiones, apoyándome en todas y cada una de ellas. Gracias por la comprensión que habéis tenido conmigo cuando los nervios me han pasado alguna mala jugada. A mis pequeños, Diego, Josep, Rubén y Amalia, vuestra inocencia y alegría han sido dos cosas muy importantes para poder coger fuerzas para realizar un buen trabajo, os quiero. A mi madre, por empujarme siempre hacia los sueños, por hacerme creer que puedo y sobre todo por escucharme. Tus esfuerzos para aceptar todas las decisiones, respetar y compartir las idas y venidas que algún disgusto te han costado y acompañarme durante toda esta andadura han sido un pilar fundamental para mí. A Jorge, su confianza, su apoyo incondicional, sus ánimos, sus reflexiones y su participación activa en este gran proyecto desde que lo inicié, hoy dan su fruto. Sabes que muchas veces te he dicho que esta Tesis ha sido cosa de dos porque sin tu paciencia, sin el equilibrio y la estabilidad que me transmites y la felicidad que me aportas no hubiera llegado hasta el final. Gracias y mil gracias! Abstract In the present Doctoral Thesis, different strategies to improve functional properties of starch films for food packaging applications were analysed: study of the effect of amylose:amylopectin ratio, blend with other polymers poly(vinyl alcohol) (PVA), and incorporation of different fillers (rice bran and cellulose nanocrystals-CNCs) and antimicrobial agents (neem oil-N, oregano essential oil-O and silver nanoparticles- AgNPs). Likewise, a biodegradation study of the films as affected by antimicrobials was carried out. Among different starches with distinct amylose:amylopectin ratio, pea starch was selected with higher values of this ratio. The high content of amylose gave rise to stiffer and more resistant to fracture films, with lower oxygen permeability, which decreased during storage. Pea starch-PVA (S-PVA) blend films represented a good strategy to improve film properties without a notable increase in cost. The PVA addition led to films which were less water soluble and not as sensitive to water sorption, more extensible and resistant than neat starch films, while they maintained the high oxygen barrier and provided stability to the matrix during ageing. In this sense, S-PVA ratios near to 1:1 are recommendable. When rice bran with the smallest particle size was used as filler, it improved the elastic modulus of the films, but reduced the film stretchability and barrier properties, due to the enhancement of the water binding capacity and the introduction of discontinuities in the matrix. Incorporation of CNCs into S-PVA films, as a reinforcing material, enhanced phase separation of polymers, did not imply changes in water vapour barrier of the films but improved the film mechanical performance: they became stiffer and more stretchable, while crystallization of PVA was partially inhibited. Silver loaded S-PVA films exhibited antimicrobial activity against the fungi (Aspergillus niger and Penicillium expansum) and bacteria (Listeria innocua and Escherichia coli) genera, depending on the silver concentration. Silver nanoparticles provoked notable changes in the film colour and transparency but no relevant changes in the other physical properties. Silver was completely delivered to aqueous simulants within the firsts 60 minutes of contact, but the film release capacity drastically decreased in the non-polar simulant, where the overall migration limit for food contact packaging materials (60 mg/Kg simulant) was accomplished. So, the use of the developed films as food packaging materials should be restricted to fat-rich foodstuffs. The incorporation of oregano essential oil (O), as antimicrobial agents, into the S- PVA matrix gave rise to active films against bacteria and fungi, whereas films containing neem oil (N) were not effective. Higher O concentration in the films was required to observe antifungal effect with respect to the antibacterial activity. Oils did not notably affect water sensitivity and water barrier properties of the films, but at high ratio, oils implied weaker film networks, affecting their mechanical performance. Blend of starch with PVA significantly improved PVA biodegradation and disintegration behaviour. Incorporation of silver species to S-PVA films slowed down their biodegradation kinetics while increased their degradation ratio. However, no significant effect of O was observed on the biodegradability indices despite the antimicrobial activity detected for this oil. N even promoted biodegradation of S-PVA films. Finally, a food application of biopolymer coatings was studied, using chitosan and essential oils (oregano or rosemary) to prevent weight loss and fungal development of semi-hard goat’s milk cheeses. Coating were highly effective at reducing fungal growth and cheese weight loss while slightly reduced lipolytic and proteolytic activities in the cheese. Sensory evaluation revealed that the cheeses double coated with chitosan- oregano oil were the best evaluated in terms of aroma and flavour. Resumen En la presente Tesis Doctoral, se han analizado diferentes estrategias para mejorar las propiedades funcionales de películas de almidón para aplicaciones de envasado de alimentos: el estudio del ratio amilosa:amilopectina, mezclas con otros polímeros
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