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Doctoral Thesis University of Castilla-La Mancha 2017 Adrián Doctoral Thesis University of Castilla-La Mancha 2017 Adrián Rabadán Guerra UNIVERSIDAD DE CASTILLA-LA MANCHA ESCUELA TÉCNICA SUPERIOR DE INGENIEROS AGRÓNOMOS Y DE MONTES DEPARTAMENTO DE PRODUCCIÓN VEGETAL Y TECNOLOGÍA AGRARIA NUTS AS RAW MATERIAL FOR OIL EXTRACTION IN THE FOOD INDUSTRY: CHARACTERIZATION, PRODUCT AND PROCESS INNOVATION AND ECONOMICS Memoria presentada para aspirar al grado de Doctor por la Universidad de Castilla-La Mancha ADRIÁN RABADÁN GUERRA ALBACETE, 2017 Agradecimientos Llega el momento de dar las gracias a todas las personas que de una forma u otra han contribuido y ayudado en la realización de este trabajo. Mirando hacia atrás te das cuenta de a cuanta gente tienes que agradecer el que esta tesis sea hoy una realidad. Fundamental para el correcto desarrollo de una tesis es la adecuada elección de los directores. En este sentido he tenido la enorme suerte de contar con José Emilio Pardo, Ricardo Gómez y Manuel Álvarez, que más allá de una inmejorable guía en todo lo relacionado en la parte más técnica de tesis, han sabido, además, aportarme el apoyo personal que se necesita cuando te embarcas en un proyecto como éste. A los tres, de verdad, muchas gracias. Tengo que agradecer además su ayuda a todos mis compañeros del grupo de investigación de “Calidad, Seguridad e Higiene de Productos Agroalimentarios”, especialmente a Andrés Alvarruiz, Arturo Pardo, Eulogio López y Sergio Díaz, por todo el apoyo técnico, científico y personal. Más allá de mi propio grupo de investigación, tengo que hacer mención especial a otros profesores e investigadores que de una forma u otra han participado en este proyecto. Así, tengo que agradecer a Miguel Olmeda los consejos y el apoyo antes y durante la realización de mi tesis, y a Ángela Triguero por, a pesar de la falta de tiempo, aceptar a dirigirme el TFM que ahora se ha convertido en parte de esta tesis. Tengo que dar las gracias también a Lourdes Gallardo y Beatriz Gandul, del Instituto de la Grasa, a Concepción de Miguel de la Universidad de Extremadura y a Joana Santos y Beatriz Oliveira de la Universidad de Oporto por toda la ayuda en los análisis y en la interpretación de resultados que ha permitido desarrollar esta tesis. La idea original de embarcarme en este proyecto podría no haber llegado a buen fin de no haberse desarrollado en un marco tan motivador como el que me proporcionó mi trabajo de becario en el Vicerrectorado de Investigación y Política Científica de la UCLM. Por ello, tengo que dar las gracias a Paco Sáez, Leonor Prieto, Mercedes Acebal, Antonio Alfaro, Santiaga Gutiérrez, Cecilia Fernández y Julián Garde, por ayudarme en todo en este primer contacto que esta beca supuso con la investigación, y por animarme a realizar la tesis. No puedo olvidarme de Sisco, ni de mis compañeros Agradecimientos becarios allí, Guadalupe, Santa y a “los Joses”, siempre dispuestos a ayudar y a comentar los problemas variados que iban aconteciendo con un café en una mesa del Vice. También agradecer a todo el personal del Departamento de Producción Vegetal y Tecnología Agraria, de la Escuela Técnica Superior de Ingenieros Agrónomos y de Montes (ETSIAM) y de la Escuela Internacional de Doctorado por los medios y las facilidades con todas las gestiones. También merece especial mención la propia UCLM, que en el marco de su Plan Propio de Investigación me ha proporcionado la financiación necesaria para desarrollar esta tesis. No me puedo olvidar tampoco de todos los que contribuyeron a hacer de mi estancia en la Universidad de Adelaida una experiencia inolvidable. A Michelle Wirthensohn, primero por darme la posibilidad de trabajar con ella, y segundo, por su cercanía y ayuda en absolutamente todo, tuviera o no que ver con el doctorado. Como parte de esa experiencia, tengo que nombrar también a Jana Kolesik, a Shashi, y en general a todo el personal del South Australian Research & Development Institute por la excepcional acogida. El desarrollo de una tesis ocasiona sin duda momentos de duda o hartazgo, que deben ser superados para llegar a buen puerto. Para ello, he tenido la suerte de contar con los ánimos de muchos amigos a los que ahora tengo la oportunidad de agradecer ese apoyo. Así, tengo que agradecer a Irene por aguantarme al teléfono hablando de cuartiles y editores, a los belmonteños (imposible nombrarlos a todos) por arrastrarme lejos del ordenador cuando era necesario, y a los albaceteños, Álvaro, Juan Ángel, Javier, Ana, Cristina y los Carlos, por hacer lo propio cuando estaba en la capital. Y por último, a mi familia, a toda ella en general, y de forma muy particular a mis padres y mi hermana, porque sin ellos, esta tesis no hubiera sido posible. Gracias. Abstract/Resumen Abstract/Resumen Abstract The health-promoting properties of nuts encourage their study and the development of industrial processes to obtain high quality oils and other by products derived from the extraction process such as partially defatted flours. Although many papers have focused on these products, there are still many lacks remaining, related to the characterization of cultivars, and their influence on the oils and defatted flours characteristics, the changes originated by the extraction process which leads to the elaboration of high quality products from the sensory and physicochemical point of view, the product innovation to improve oil characteristics and the analysis of economic factors related to nuts and nut oils. Thus, as a first step, the characterization of cultivars from almond, pistachio and walnut was developed attending to physical, chemical and sensory analysis of kernels, to evaluate the differences that raw material may originate in the oils characteristics. In addition, the effect of the crop year was also evaluated. In almond, pistachio and walnut kernels, physical parameters (size, weight and colour) proved to be useful for cultivar discrimination. Regarding sensory analysis, consumers showed preferences in overall visual acceptance and taste for some almond (Vairo, Belona and Penta) and pistachio cultivars (Larnaka, Aegina and Sirora) when affective tests were performed. When the oils from the different cultivars were evaluated, differences were found in physical parameters like viscosity, showing strong correlations with the oil fatty acid profile and the concentration of specific triglycerides. The oils obtained from the studied cultivars showed significant differences in their chemical composition. Oil yield was similar in all the selected almond cultivars, but significant differences were found in the oxidative stability or in their fatty acid profile, mainly in the content of linoleic, stearic and palmitoleic acids. Regarding pistachio oil, three different groups of cultivars were defined according to the physicochemical composition and oil yield. Cultivars in group 1 showed a higher content of linoleic fatty acid (higher than 26.4%), while cultivars in group 3 type showed a stronger presence of oleic acid (higher than 67.8%), resulting in oils that Abstract/Resumen were more stable to oxidation. Cultivars with intermediate characteristics were included in group 2. Among walnut cultivars, significant differences were found in the fatty acid profile and concentration of minor components of interest as polyphenols. Linoleic fatty acid compound more than 47.5% of total fatty acids in all cultivars, accounting up to 62.13% and 60.02% in cvs. Pedro and Mollar de Nerpio, respectively. As expected, the oxidative stability index of walnut oil was lower than the reported in other plant oils due to the high presence of polyunsaturated fatty acids. After oil extraction, the remaining pressing cake may be transformed into partially defatted flour, with a high proportion of protein, fibre and essential minerals. This flour also showed differentiated nutritional characteristics depending on the cultivar of almond, pistachio or walnut considered. In the analysis of the variability reported by the genotype (G), the crop year (CY) and the interaction GxCY, the genotype remained as the main factor determining oil chemometrics. However, significant variability of the crop year and the interaction GxCY was found for most of the parameters. In comparison to almond and pistachio oils, a greater effect of the crop year has been reported for most of the fatty acids in walnut oil, including stearic, oleic and linolenic. Moreover, the crop year affected the concentration of some minor components of crucial nutritional interest in nuts oils as total polyphenols and phytosterols. Regarding oil extraction process, innovation is crucial for the development of high quality products. For this reason, the analysis of the influence of oil extraction parameters on product quality has been addressed. Within extraction methods, pressing by using two different presses (hydraulic and screw) has been considered. The extraction of vegetable oils by means of screw presses originates an increase in oil temperature due to the friction of the raw material. Oil temperature may reach values around 60˚C in almond and pistachio when oil is extracted at low temperatures, being somewhat lower in walnut oil. Results show that extraction temperature influenced greatly the physicochemical parameters of regulated quality of the oils. Abstract/Resumen When the oil obtained from the screw and the hydraulic press are compared, the use of higher temperatures on the first one resulted in changes in physicochemical and sensory properties of the oils. In the crew press, oil extraction with lower rotational speed resulted in higher yields and the oil was more valued by consumers. In the hydraulic press extraction, no differences were found regarding yield and physicochemical characteristics in oils by changing extraction parameters. The lack of influence of extraction parameters in physicochemical characteristics of oil suggest changing the focus to the influence of these parameters in yields and sensory evaluation. To improve sensory attributes, a roasting step can be included in the nut oil production process before extraction.
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