The topic of my dissertation is Comparison of the quality of eggs depending on the method of feeding. The aim of this study was to investigate whether the quality of hen eggs changes after adding crushed grape seeds in the compound feed of the hens. Grape seeds are formed as a side product during wine making processes and contain large amounts of biologically active substances and suitable acids, which can improve the feed conversion and subsequently also improve the technological properties of eggs. With processing of grape seeds the effective utilization of crop residues in vineyards comes about. The experiment was conducted in two experimental periods and in each period 100 laying hens were surveyed. They were separated into two groups an experimental and a control one. In the control group the hens were fed with a standard mixture of N2 feed and in the experimental group there was a supplement of 5 weight percent of crushed grape seeds in the compound feed. Eggs were collected daily and once every two weeks an analysis of technological properties of eggs was conducted. The results of the experiment showed that the addition of crushed grape seeds containing a biologically active substance did not have a statistically significant effect on the quality and selected technological parameters of eggs.

Orientadores: Eduardo Augusto Caldas Batista, José Vladimir de Oliveira / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos / Made available in DSpace on 2018-08-22T05:44:32Z (GMT). No. of bitstreams: 1 Dalmolin_IredeAngelaLucini_D.pdf: 9550332 bytes, checksum: 061256cf12d61dd7b97065d987efd625 (MD5) Previous issue date: 2013 / Resumo: A utilização de resíduos e o emprego de tecnologias ambientalmente seguras são tendências gerais de pesquisa da comunidade científica, impulsionadas pelas exigências governamentais e apelo do mercado consumidor, que buscam cada vez mais produtos naturais de alta qualidade. Neste contexto, o objetivo deste trabalho foi obter o extrato de sementes de uva através de extração por fluido supercrítico, caracterizá-lo química e fisicamente, e aplicá-lo ao encapsulamento em poli-(hidroxibutirato-cohidroxivalerato) utilizando tecnologia de antissolvente supercrítico. Para tanto, o estudo do ponto de vista termodinâmico, através de dados de equilíbrio de fases e modelagem, fez-se necessário para obtenção de informações dos sistemas de interesse à extração bem como ao encapsulamento. A caracterização desse extrato aponta uma importante fonte natural de ácido linoléico, como componente majoritário, e também de ácidos oléico, palmítico e esteárico, e de antioxidantes e fitoesteróis. Através de separadores dispostos em série foi possível fracionar por meio de despressurização e obter extratos com diferentes composições desejadas. Na determinação de dados de equilíbrio de fases do sistema Extrato de Sementes de Uva (ESU) + Dióxido de Carbono (CO2) + Etanol, verificou-se que a quantidade de água no extrato, remanescente da matéria-prima, prejudicava a obtenção de dados de equilíbrio com porcentagens de (CO2 + Etanol) inferiores a 70 %. Observaram-se transições bifásicas do tipo Líquido-Vapor Ponto de Bolha (LV-PB), Líquido-Vapor Ponto de Orvalho (LV-PO) e Líquido-Líquido (LL), e trifásicas do tipo Líquido-Líquido-Vapor (LLV). Com a redução de água no ESU foi possível descrever o comportamento do equilíbrio de fases, porém para ambas as temperaturas estudadas ocultaram-se as transições LV-PO. Para o mesmo sistema, a modelagem foi feita utilizando a equação de Peng-Robinson, que foi capaz de correlacionar os dados com a utilização de dois parâmetros de interação binária ajustados. Dados de equilíbrio de fases do sistema ESU + CO2 +Diclorometano (DCM) foram determinados onde transições bifásicas do tipo LV-PB e LVPO foram observadas. Verificou-se que a adição de ESU em solução de DCM, em concentrações de até 15 kg·m-3, não influenciou nas pressões de transição do sistema binário CO2 + DCM. O encapsulamento foi realizado com percentual de encapsulamento de até 72 % de ESU / Abstract: The use of residues and environmentally safe and benign technologies comprise a general research trend of scientific community, stimulated by government requirements and appeal to the consumer market which increasingly seek natural products of high quality. In this context, the aim of this work was to obtain grape seed extract by supercritical fluid extraction, characterize it chemically and physically, and apply it to the encapsulation in polymer poly-(hydroxybutyrate-co-hydroxyvalerate) using supercritical anti-solvent technology. Thus, the study from the thermodynamic point of view, by phase equilibrium data and modeling, was necessary to obtain information of the interest system for the extraction and for encapsulation. According to the characterization, grape seed extract is an important natural source of linoleic acid, as major component, and also by oleic, palmitic and stearic acids, and antioxidants and phytosterols. Through separators displayed in series was possible to fractionate the depressurization and to obtain extracts with different desired compositions. In the determination of phase equilibrium data of the system Grape Seed Extract (GSE) + Carbon Dioxide (CO2) + Ethanol, it was found that the amount of water in the extract, remaining in the raw materials, limited obtaining equilibrium data with percentages of (CO2 + ethanol) lower than 70 %. Two-phase transitions were observed, Vapor-Liquid Bubble Point (VL-BP), Vapor-Liquid Dew Point (VL-DP), and Liquid-Liquid (LL), and three-phase transitions Vapor-Liquid-Liquid (VLL). With the reduction of water in the GSE was possible to describe phase equilibrium behavior, but for both temperatures studied were put out transitions VL-DP. For the same system, the modeling was performed using Peng-Robinson equation which was able to correlate data with the use of two adjusted binary interaction parameters. Phase equilibrium data of GSE + CO2 +dichloromethane (DCM) system were determined where two-phase transitions VL-BP and VL-DP were observed. It was verified that the addition of GSE to the DCM solution in concentration up to 15 kg·m-3 did not affect the transition pressure of the binary system CO2 + DCM. The encapsulation was realized with percentage of encapsulation up to 72 % of GSE / Doutorado / Engenharia de Alimentos / Doutora em Engenharia de Alimentos

Ce travail de thèse concerne l’utilisation des décharges électriques de haute tension (DEHT) en milieu aqueux comme méthode d’extraction des polyphénols à partir de pépins de raisin.Les arcs électriques produits en milieu aqueux provoquent une succession de phénomènes (ondes de choc, bulles de cavitation) qui ont pour effet de fragmenter toute matière première située à proximité de l’arc électrique. L’objectif de cette thèse est d’étudier ces phénomènes afin d’améliorer la compréhension et l’efficacité des DEHT en tant que méthode d’extraction.Dans un premier temps, une étude des conditions d’apparition de l’arc électrique dans l’eau a permis de montrer que l’arc apparaît initialement dans des bulles de vapeur générées à la surface de l’électrode à cause de l’échauffement du liquide par effet Joule. Des mesures électriques, des prises de vues à haute vitesse, ainsi qu’une simulation numérique du problème ont permis de vérifier cette hypothèse. Une étude paramétrique des phénomènes générés par l’arc électrique (onde de choc et bulle de cavitation) a été menée. Grâce à des mesures de la pression des ondes de choc, des mesures de la taille des bulles de cavitation, et grâce des mesures électriques précises (notamment de la résistance électrique de l’arc), il apparaît que l’amplitude des phénomènes dépendent essentiellement de l’énergie dépensée dans l’arc. Cette énergie doit être distinguée de l’énergie totale d’une impulsion électrique, dont une partie est dépensée avant le claquage, mais également de l’énergie disponible au moment du claquage, dont une partie importante est dépensée dans le circuit électrique. La partition de cette énergie entre l’arc et le circuit électrique dépend du rapport entre la résistance du circuit et la résistance de l’arc. Ainsi une méthode pour augmenter significativement l’amplitude des phénomènes étudiés, et donc l’efficacité du procédé est d’améliorer le rapport entre ces résistances. Il a par exemple été observé qu’en augmentant la longueur de l’arc électrique de 2.5 mm à 2 cm, la résistance de l’arc augmente de 40 m à 0.55, et l’amplitude de l’onde de choc augmente de 135%. Pour finir, une étude paramétrique sur l’efficacité des DEHT comme procédé d’extraction des polyphénols des pépins de raisin a été menée. Entre autres, les effets sur l’extraction de la conductivité du liquide, du rapport liquide-solide, du nombre d’impulsion, de l’énergie par impulsion, de la distance inter-électrode ont été étudiés. Ces études ont mis en évidence l’importance de la répartition de l’énergie totale d’une impulsion en énergie dépensée avant le claquage, énergie dépensée au claquage dans le circuit électrique et énergie dépensée dans l’arc électrique. Ces études ont montré comment cette répartition est influencée par ces différents paramètres, et comment cela influence l’efficacité d’extraction. L’influence de la distance inter-électrode, et donc de la longueur de l’arc, a été particulièrement été mise en évidence par les résultats d’extraction. / This thesis work focuses on the use of high voltage electrical discharges (HVED) in aqueous media as a method for extracting polyphenols from grape seeds. Electric arcs generated in an aqueous environment cause a succession of phenomena (shock waves, cavitation bubbles) that have the effect of fragmenting any raw material located near the electric arc. The objective of this thesis is to study these phenomena in order to improve the understanding and effectiveness ofHVED as an extraction method. First, a study of the conditions under which the electric arc appears in water showed that the arc initially appears in vapour bubbles generated on the electrode surface due to the heating of the liquid due to Joule effect. Electrical measurements, high-speed photography and a numerical simulation of the problem have allowed this hypothesis to be verified. A parametric study of the phenomena generated by the electric arc (shock wave and cavitation bubble) was carried out. Through measurements of shock wave pressure, of cavitation bubble size, and precise electrical measurements (including the electrical resistance of the arc), it appears that the amplitude of the phenomena depends essentially on the energy consumed in the arc. This energy mustbe distinguished from the total energy of an electrical pulse, part of which is spent before the breakdown. The energy spent in the electric arc must also be distinguishedfrom the energy available at electrical breakdown, as a significant part of breakdown energy is spent in the electrical circuit. The partition of breakdown energy between the arc and the electrical circuit depends on the ratio between the resistance of the circuit and that of the arc. Thus a method to significantly increase the amplitude of the studied phenomena (and therefore the efficiency of the process), is to improve the ratio between these resistances. For example, it has been observed that by increasing the length of the electric arc from 2.5 mm to 2 cm, the resistance of the arc increases from 40 m to 0.55, and the amplitude of the shock wave increases by 135%. Finally, a parametric study on the efficiency of DEHT as a process for extracting polyphenols from grape seedswas carried out. Among other things, the effects on the extraction of liquid conductivity, liquid-solid ratio, number of pulses, energy per pulse, and distance between electrodes were studied. These studies highlighted the importance of the distribution of the total pulse energy into energy spent before the breakdown, energy spent after breakdown in the electrical circuit and energy spent in the arc. These studies have shown howthis distribution is influenced by these different parameters, and how it influences extraction efficiency. The influence of the inter-electrode distance, and therefore the length of the arc, was particularly highlighted by the extraction results.

L’équilibre gustatif des vins secs repose notamment sur les saveurs amère et sucrée, dont les déterminants moléculaires n’ont été que partiellement élucidés. Un premier axe a consisté en l’étude de la contribution gustative des lignanes du chêne et neuf composés ont été observés pour la première fois dans le vin. Le (±)-lyonirésinol a été établi comme le plus amer et le plus abondant des lignanes isolés. Ses deux énantiomères ont été séparés, caractérisés par VCD et leur dégustation a révélé que seul le (+)-lyonirésinol possède une amertume modifiant le goût du vin. Dans un second axe, la saveur sucrée conférée par les raisins aux vins secs a été étudiée. Des expérimentations de vinification combinées à des outils sensoriels ont montré un gain de saveur sucrée au cours de la macération post-fermentaire à chaud et un effet des pépins de raisin sur le moelleux des vins secs. La mise en place d’un protocole de fractionnement d’extrait de pépins et de vin, par des techniques séparatives couplées à la gustatométrie, a permis la purification de six composés sapides. Plusieurs marqueurs de la sucrosité des vins secs ont ainsi été identifiés par FTMS et RMN : le mélange de deux nouvelles molécules, les acides 2-hydroxy-3-méthylpentanoïque-2-O-β-glucopyranoside et 2-hydroxy-4-méthylpentanoïque-2-O-β-glucopyranoside ; l’acide gallique-4-O-β-glucopyranoside et l’acide epi-DPA-3′-O-β-glucopyranoside, identifiés pour la première fois dans les vins, ainsi que l’ILA-Glc et l’astilbine. Ces nouveaux marqueurs ont été quantifiés dans les vins ainsi que dans les différentes parties de la baie pour préciser leur localisation et établir leur contribution gustative. / Dry wines taste balance is mainly based on bitter and sweet tastes, whose molecular determinants have been only partially explained. The first key objective was the study of the gustatory contribution of oak lignans. Nine compounds were identified in wines for the first time. (±)-lyoniresinol has been established as the bitterest and the most abundant of the isolated lignans. Its two enantiomers have been resolved, characterized by VCD and their tasting revealed that only (+)-lyoniresinol is bitter and modifies wine taste. In the second part of this work, the contribution of grapes to wine sweet taste has been studied. The combination between vinification experimentations and sensorial tools showed a gain of sweetness during a warm post-fermentative maceration as well as an influence of grape seeds on dry wine sweetness. A fractionation protocol of grape seeds macerates and wines has been established. Separation techniques coupled with gustatometry allowed the isolation of six taste active compounds. Several markers of dry wines sweetness have been identified by FTMS and NMR: the mix of two new compounds, 2-hydroxy-3-methylpentanoic-2-O-β-glucopyranoside and 2-hydroxy-4-methylpentanoic-2-O-β-glucopyranoside acids; gallic-4-O-β-glucopyranoside acid and epi-DPA-3′-O-β-glucopyranoside acid, identified for the first time in wines, ILA-Glc and astilbin. These new markers have been quantified in wines and in different parts of grape berry in order to refine their localization and to establish their gustatory contribution.

L’extraction d’huile végétale à partir des graines repose principalement deux procédés : le pressage mécanique et ’extraction par solvants. Dans un contexte actuel de limitation de la consommation de solvants et de recherche de procédés adaptés à la production d’huile végétales thermosensibles, un procédé alternatif d’extraction d’huile a été étudié dans ce mémoire : le pressage mécanique assisté par CO2 supercritique (GAME). Pour évaluer le potentiel de cette technique en terme de rendement en huile et de co-extraction de composés antioxydants dans l’huile, l’extraction par CO2 supercritique (EPCO2-SC) et le pressage à vis (procédé de référence en trituration) ont été préalablement étudiés. Deux espèces ont été étudiées, les graines de lin et les pépins de raisin. En EPCO2-SC, des rendements en huile moins importants sont obtenus, cependant il est possible d’augmenter la teneur en polyphénols co-extraits dans l’huile par le contrôle des paramètres opératoires. L’évaluation des deux modes de pressage assisté (sous flux continu de CO2-SC et après un conditionnement en CO2-SC) a montré que le rendement en huile pouvait être augmenté de 30 à 40% en comparaison au pressage hydraulique seul malgré l’application de faibles pressions mécaniques effectives (de l’ordre de 3,5 à 7 MPa). Toutefois, les rendements obtenus restent inférieurs à ceux observés en pressage en continu. La teneur en antioxydants dans l’huile est fonction de la température et de la pression appliquée, mais reste inférieure à celle obtenue pour des conditions identiques en EPCO2-SC. / Screw pressing or solvent extraction are processes commonly used at an industrial scale to extract oil from oilseeds. However, in a context of continuous improvements, i.e. reduction ofsolvent consumption and production of high-quality oils, gas assisted mechanical expression appears as an interesting alternative, among emerging technologies. To assess the latter in terms of oil extraction yield and co-extraction of antioxidant compounds in oil, supercritical CO2 extraction and screw pressing were preliminarily studied. Two raw material were studied; flaxseeds and grape seeds. Supercritical CO2 extraction lead to low oil yields, but by controlling CO2 pressure and temperature, total polyphenol content in oil could be enhanced. For gas assisted mechanical expression, two different procedures were applied: (i) conditioning of seeds in supercritical CO2 followed by expression and (ii) expression under a simultaneous flux of CO2, flowing through the compacted seed bed. By those two procedures,oil yield could be increased from 30 to 40% by comparison to conventional hydraulic expression (even though low effective mechanical pressure were applied (3,5 to 7 MPa)). However, although antioxidant level in oil could be increased by modulating CO2 pressure and temperature for gas assisted mechanical expression, this level remained lower than those obtained in oil by supercritical CO2 extraction in the same conditions. Screw pressing enabled the highest oil yields among the three studied processes. Furthermore, oil composition was unaffected by screw pressing operational conditions.