Made available in DSpace on 2017-07-21T18:53:09Z (GMT). No. of bitstreams: 1 SIMONE CRISTINE WOSNIACKI BICUDO.pdf: 856559 bytes, checksum: d069ed257c254bc2a62e80ada3a1d5a0 (MD5) Previous issue date: 2008-02-29 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / Starch is a very imp ortant polysaccharide for food processing. It is extracted from different sources and presents very important particular thermal characteristics. The most important temperature for food industry applications is the gelatinization, investigated in this work by techniques of thermal analysis, Differential Scanning Calorimetry (DSC), in various native starches. The thermal behaviour of starch granules was investigated by Thermogravimetry (TG), Differential Thermogravimetry (DTG) and Differential Thermal Analysis (DTA). Also the amylose content was measured for characterization of the native starches. The native starch that presented the lowest gelatinization temperature was the pinhão seed, with peak temperature of 50.8ºC, whereas the lowest amylose content, among non waxy starches, was of banana, with apparent amylose content of 8.1% and total amylose of 9.0%. / O amido é um carboidrato muito importante para o processamento dos alimentos. Está presente em diferentes fontes e apresenta características térmicas também variadas. O intervalo de temperatura de maior importância para a indústria é a de gelatinização, investigada neste trabalho através da técnica de análise térmica, Calorimetria Exploratória Diferencial (DSC), em diversos amidos nativos. Como muitos fatores influenciam o processamento dos alimentos, outras análises foram feitas para auxiliar na obtenção de informações para caracterizar diferentes amidos nativos, como Termogravimetria (TG) Termogravimetria Derivada (DTG) e Análise Térmica Diferencial (DTA), para investigar a degradação térmica dos grânulos de amido e os teores de amilose. O amido nativo que apresentou as menores temperaturas de gelatinização foi o de pinhão, com temperatura de pico de 50,8ºC enquanto que, os menores teores de amilose apresentados, dentre os amidos nativos não cerosos, foi o de banana, com amilose aparente de 8,1% e amilose total de 9,0%.

Made available in DSpace on 2014-06-11T19:24:40Z (GMT). No. of bitstreams: 0 Previous issue date: 2006-02-17Bitstream added on 2014-06-13T20:52:19Z : No. of bitstreams: 1 horimoto_lk_me_botfca.pdf: 643530 bytes, checksum: a89cce04a174ddfc6169b6fc1e10b14b (MD5) / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / Universidade Estadual Paulista (UNESP) / Apesar dos amidos serem quimicamente iguais, a organização e funcionalidade desses polímeros dependem das propriedades físico-químicas de cada fonte botânica. Esses amidos podem sofrer diferentes modificações com a finalidade de aperfeiçoar certas características para aplicações industriais específicas. Dentre os amidos modificados, os catiônicos são largamente utilizados na fabricação de papel/papelão a fim de aumentar sua resistência física e mecânica. Neste trabalho, amidos de mandioca, batata doce e mandioquinha salsa foram cationizados com o reagente 3-cloro-2-hidroxipropil-trimetilamônio que em meio alcalino reage com o amido tornando-o carregado positivamente.As amostras foram submetidas a diferentes tempos de reação (0,5 a 24 horas) e relação molar de hidróxido de sódio/monômero. Os melhores parâmetros encontrados para as amostras foram de 6 horas de reação e relação molar de 2,0 NaOH/monômero, que resultaram em maiores DS (grau de substituição) e rendimento percentual, determinados a partir do teor de nitrogênio presente em cada amostra. Em seguida os amidos catiônicos com os melhores parâmetros foram submetidos a diferentes tratamentos após a derivatização: etanol a 25%, etanol a 50% e água a temperatura de 35°C, para avaliar a interferência dos sais residuários no grau de substituição das amostras derivatizadas. A seguir essas amostras de amidos catiônicos de mandioca, batata doce e mandioquinha salsa foram aplicadas em folhas de papel, onde testes físicos-mecânicos como resistências ao rasgo, arrebentamento, tração, permeância ao ar entre outros foram realizados com a finalidade de verificar a influência da adição de diferentes tipos de amido. / In spite of starches are chemically the same, the organization of biopolymers and the functionality of the starches depend on physical and chemical properties of each botanical source, which can undergo modifications with the purpose of improving certain characteristics for specific industrial applications. Among the modified starches, the cationic are widely used in the papermaking process in order to increase their physical and mechanical resistances. In this study, cassava, sweet potato and Peruvian carrot starches were cationized with 3-chloro-2-hydroxypropyltrimethylammonium choride reagent, that in a high pH reacts with starch become it positively loaded. The samples were submitted to different reaction time (0.5 to 24 hours) and the NaOH/monomer mole ratio. The best parameters found for the samples were of 6 hours of reaction time and 2.0 NaOH/monomer mole ratio, which resulted in larger degree of substitution (DS) and reaction efficiency (RE), determined by the 3 content of nitrogen present in each sample. Then the cationic starches with the best parameters were submitted to different treatments after derivatization: ethanol at 25%, ethanol at 50% and water at the temperature of 35°C, in order to evaluate the interference of the residual salts in the degree of substitution of the derivatized samples. In the sequence, these samples of cationic cassava, sweet potato and Peruvian carrot starches were applied in sheets of paper, where physical and mechanical tests such as air resistance, bursting strength, tensile strength, internal tearing resistance, among others, were performed with the purpose of verifying the influence of the addition of different types of starch.

Les ciments acryliques osseux sont une solution courante pour traiter des lacunes osseuses. L'incorporation de charges permet d'en améliorer les propriétés, ainsi l'amidon pour la dégradabilité, associé à l’acétate de cellulose pour les propriétés mécaniques, et les phosphocalciques pour ces dernières et la bioactivité. Très souvent, le polymère est le polyméthacrylate de méthyle et l'amidon, celui issu du maïs. La majorité des études les concernent. Celle-ci porte donc sur des formulations classiques mais à base de 2-hydroxyéthylméthacrylate, incorporant un amidon de waxy-maïs, maïs, amylomaïs, blé, pois ou pomme de terre, avec ou sans enzyme (α-amylase). L’HEMA apporte sa capacité à s’hydrater et les amidons à se dégrader. Temps et température maximale de prise ont été étudiés en fonction de la formulation, de même, le taux d'hydratation du ciment et sa perte de masse en fonction du temps d'immersion dans un fluide biologique. Les propriétés mécaniques ont été approchées à travers des essais de traction et de compression. La radio-opacité a été prise en compte. Paramètres de prise et taux d'hydratation (d'où un gonflement in situ favorable au comblement d'une lacune) se sont révélés peu influencés par l’origine botanique de l'amidon ou la présence de l'enzyme, contrairement à la dégradabilité. Le gonflement, néfaste si trop important, a été contrôlé grâce à une pré-saturation en eau, la perte des propriétés mécaniques après immersion en découlant l'étant par ajout de plâtre. Le dioxyde de zirconium s’est révélé le radio-opacifiant le plus approprié. L’ensemble des résultats a conduit à formuler deux ciments optimisés en fonction de la dégradabilité recherchée. / Acrylic cements are a current solution to deal with osseous gaps. The incorporation of fillers allows improving the properties, so starch for the degradability, associated with cellulose acetate for the mechanical properties, and calcium phosphates for the latter and the bioactivity. Very often, the polymer is polymethyl methacrylate and the starch is issued from corn. So the majority of the studies concern them. Thus this one concerns classic formulations but with 2-hydroxyethylmethacrylate, incorporating starch from waxy-maïs, corn, amylomais, wheat, pea or potato, with or without enzyme (α - amylase). HEMA brings its capacity to hydrate and starches to degrade. Setting time and maximal temperature were studied according to the formulation, also, the water uptake of the cement and its weight loss according to the immersion time in a biological fluid. The mechanical properties were approached through tensile and compression tests. The radio-opacity was taken into account. Curing parameters and water uptake (leading to in situ swelling favourable to the filling of a gap) were little influenced by the botanical origin of starch or by the presence of enzyme, contrary to the degradability. The swelling, negative if too important, was monitored through a pre-saturation by water and the resulting loss of the mechanical properties after immersion through addition of plaster. The zirconia was the most appropriate radio-opacifier. The results led to formulate two cements optimized according to the desired degradability.

Orientador: Claudio Cabello / Banca: Claudio Angeli Sansígolo / Banca: José Luis Agapito Fernandes / Resumo: Apesar dos amidos serem quimicamente iguais, a organização e funcionalidade desses polímeros dependem das propriedades físico-químicas de cada fonte botânica. Esses amidos podem sofrer diferentes modificações com a finalidade de aperfeiçoar certas características para aplicações industriais específicas. Dentre os amidos modificados, os catiônicos são largamente utilizados na fabricação de papel/papelão a fim de aumentar sua resistência física e mecânica. Neste trabalho, amidos de mandioca, batata doce e mandioquinha salsa foram cationizados com o reagente 3-cloro-2-hidroxipropil-trimetilamônio que em meio alcalino reage com o amido tornando-o carregado positivamente.As amostras foram submetidas a diferentes tempos de reação (0,5 a 24 horas) e relação molar de hidróxido de sódio/monômero. Os melhores parâmetros encontrados para as amostras foram de 6 horas de reação e relação molar de 2,0 NaOH/monômero, que resultaram em maiores DS (grau de substituição) e rendimento percentual, determinados a partir do teor de nitrogênio presente em cada amostra. Em seguida os amidos catiônicos com os melhores parâmetros foram submetidos a diferentes tratamentos após a derivatização: etanol a 25%, etanol a 50% e água a temperatura de 35°C, para avaliar a interferência dos sais residuários no grau de substituição das amostras derivatizadas. A seguir essas amostras de amidos catiônicos de mandioca, batata doce e mandioquinha salsa foram aplicadas em folhas de papel, onde testes físicos-mecânicos como resistências ao rasgo, arrebentamento, tração, permeância ao ar entre outros foram realizados com a finalidade de verificar a influência da adição de diferentes tipos de amido. / Abstract: In spite of starches are chemically the same, the organization of biopolymers and the functionality of the starches depend on physical and chemical properties of each botanical source, which can undergo modifications with the purpose of improving certain characteristics for specific industrial applications. Among the modified starches, the cationic are widely used in the papermaking process in order to increase their physical and mechanical resistances. In this study, cassava, sweet potato and Peruvian carrot starches were cationized with 3-chloro-2-hydroxypropyltrimethylammonium choride reagent, that in a high pH reacts with starch become it positively loaded. The samples were submitted to different reaction time (0.5 to 24 hours) and the NaOH/monomer mole ratio. The best parameters found for the samples were of 6 hours of reaction time and 2.0 NaOH/monomer mole ratio, which resulted in larger degree of substitution (DS) and reaction efficiency (RE), determined by the 3 content of nitrogen present in each sample. Then the cationic starches with the best parameters were submitted to different treatments after derivatization: ethanol at 25%, ethanol at 50% and water at the temperature of 35°C, in order to evaluate the interference of the residual salts in the degree of substitution of the derivatized samples. In the sequence, these samples of cationic cassava, sweet potato and Peruvian carrot starches were applied in sheets of paper, where physical and mechanical tests such as air resistance, bursting strength, tensile strength, internal tearing resistance, among others, were performed with the purpose of verifying the influence of the addition of different types of starch. / Mestre

Regular starches contain two principal types of glucan polymers: amylopectin and amylose. The structure of amylopectin is characterized according to the unit chain length profile and the nature of the branching pattern, which determine the alignment of glucan chains during biosynthesis. The organization of glucan chains in amylopectin and their impact on the structure of starch are still open to debate. The location of amylose and its exact contribution to the assembly of crystalline lamellae in regular and high-amylose starch granules also remain unknown. The primary focus of this thesis is the organization and flexibility of glucan chains in crystalline lamellae. The organization and flexibility of glucan chains in native, annealed (ANN), and heat-moisture treated (HMT) normal, waxy, hylon V, hylon VII, and hylon VIII corn starches were examined. This study has shown for the first time that increased amounts of apparent amylose in B-type starches hinder the polymorphic transition (from B to A+B) during HMT. The research has also demonstrated that an iodine-glucan complex transformed the B-type polymorphic pattern of hylon starches into a V-type pattern. The differential scanning calorimetry (DSC) results showed that ANN- and HMT-induced changes were most pronounced in hylon starches. These findings suggest that the glucan tie chains influences the assembly of crystalline lamellae in high-amylose starches. The relationship between the internal unit chain composition of amylopectin, and the thermal properties and annealing of starches from four different structural types of amylopectin was investigated by DSC. The onset gelatinization temperature (To) correlated negatively with the number of building blocks in clusters (NBbl) and positively with the inter-block chain length (IB-CL). The enthalpy of gelatinization (∆H) correlated positively with the external chain length of amylopectin. Annealing results showed that starches with a short IB-CL were most susceptible to ANN, as evidenced by a greater increase in the To and Tm. The increase in enthalpy was greater in starches with long external chains and IB-CLs. These data suggest that the internal organization of glucan chains in amylopectin determines the alignment of chains within the crystalline lamellae and thereby the thermal properties and annealing of the starch granules.

<p>Prema najnovijim istraživanjima modifikovanim skrobovima može se pripisati jo&scaron; jedna uloga &ndash; aditivi u pekarstvu, s obzirom da utiču na pobolj&scaron;anje kvaliteta hleba i<br />usporavaju proces starenja. Međutim, prema saznanjima autora ove disertacije, ne<br />postoje istraživanja na temu uticaja emulgujućih skrobova (skrob-natrijum<br />oktenilsukcinata, OSA skrobova) na kvalitet testa i hleba od p&scaron;eničnog bra&scaron;na.<br />Uzimajući u obzir činjenicu da druge vrste modifikovanih skrobova ispoljavaju dobre<br />osobine u smislu pobolj&scaron;anja kvaliteta hleba i da je OSA skrob nutritivno vredna<br />sirovina, s obzirom da se u organiznu pona&scaron;a kao prehrambeno vlakno, od velike je<br />važnosti ispitati ulogu OSA skroba kao aditiva u pekarstvu.<br />Međutim, usled kompleksne prirode testa kao sistema, bilo je te&scaron;ko odrediti relativni<br />uticaj pojedinačnih komponenti (proteina, p&scaron;eničnog skroba, OSA skroba) i njihovih<br />međusobnih interakcija na osobine testa. Stoga je, u cilju rasvetljavanja uticaja različitih OSA skrobova na viskoelastične osobine testa i retrogradaciju skrobne komponente (fenomen povezan sa starenjem hleba), p&scaron;enično bra&scaron;no frakcionisano na gluten i skrob, i vr&scaron;ena su ispitivanja strukturnih, reolo&scaron;kih i termičkih osobina hidratisanog glutena i skrobnih gelova sa dodatkom OSA skroba. Takođe su pripremani i model sistemi testa.<br />Ispitivanja na realnim sistemima (testo i hleb) izvođena su zamenom 2,5; 5 i 10%<br />p&scaron;eničnog bra&scaron;na, jednim od tri vrste OSA skroba: skrob-natrijum oktenilsukcinatom<br />(OSA-ST), preželatiniziranim skrob-natrijum oktenilsukcinatom (Pregel OSA-ST) i<br />hidrolizovanim su&scaron;enim u spreju skrob-natrijum oktenilsukcinatom (Hydrol OSA-ST).<br />Cilj je bio da se ispita uticaj dodatka OSA skrobova na strukturu testa (SEM), empirijske (miksolab, alveograf i reofermentometar) i fundamentalne (oscilatorna merenja i testovi puzanja i deformacije) reolo&scaron;ke osobine, kao i parametre kvaliteta hleba (specifična zapremina, boja kore i sredine hleba, vlaga sredine hleba, parametri raspodele veličine pora i tekstura sredine). Pored pomenutog, praćena je i promena kvaliteta hleba tokom skladi&scaron;tenja, kako bi se dobio uvid u kinetiku starenja hleba.<br />Rezultati dobijeni u ovoj disertaciji ukazali su da reolo&scaron;ko pona&scaron;anje testa sa dodatkom OSA skrobova zavisi od strukture skrobnih granula, tj. od stepena dezintegracije i depolimerizacije granule tokom procesa modifikacije. Stoga je dodatak OSA-ST doveo do ojačavanja glutenske mreže &scaron;to se odrazilo na porast modula elastičnosti i testa i glutena. Nasuprot tome, Pregel and Hydrol OSA-ST uticali su na kontinualnost glutenske mreže koja je u njihovom prisustvu bila poroznija, a time su i dobijena testa bila mek&scaron;a i rastegljivija. Istraživanja na realnim i model sistemima (p&scaron;enični skrob sa dodatkom OSA skroba) ukazala su da sva tri OSA skroba usporavaju retrogradaciju p&scaron;eničnog skroba. Takođe je dokazano da svi ispitivani emulgujući skrobovi povećavaju specifičnu zapreminu hleba u poređenju sa kontrolnim, pri čemu je Pregel OSA ispoljio najjači efekat. To se odrazilo i na strukturne osobine sredine hleba, a posledično i na mehaničke osobine sredine, čija promena je praćena u cilju određivanja kinetike starenja hleba. Prema dobijenim rezultatima, vrednosti čvrstoće sredine hleba koji je sadržao OSA-ST i Pregel OSA-ST su i nakon 24 h bile slične ili značajno niže od vrednosti čvrstoće kontrolnog uzorka određene 2 h nakon pečenja.</p> / <p>Recent studies have demonstrated that modified starches can be used as novel additives in breadmaking since they improve bread quality and retard stalling. However, up to the author&#39;s knowledge, there are no investigations concerning the influence of emulsifying starches (starch sodium octenyl succinates - OSA starches) on wheat flour dough and bread quality. Taking into account the fact that other modified starches have exhibited significant bread improving properties and that OSA starch has special nutritional value since it can act as functional fibre, it is of a great importance to investigate the feasibility of OSA starch as bread improver.<br />However, due to the complex nature of dough, it was difficult to determine the relative contributions of protein, native and modified starch components and their interactions on dough properties. Therefore, in order to resolve the influence of different OSA starches on dough viscoelastic properties and starch retrogradation (the phenomenon related to bread stalling), wheat flour was fractionated into gluten and starch; and the structural, rheological and thermal behaviour of the hydrated gluten samples and starch gels supplemented with emulsifying starches was also studied. Dough model systems were also prepared.<br />Experiments on real systems (dough and bread) were performed by incorporating<br />starch sodium octenyl succinate (OSA-ST), pregelatinized OSA starch (Pregel OSA-ST) and hydrolysed spray-dried OSA starch (Hydrol OSA-ST) at 2.5, 5 and 10 % into wheat flour. The aim was to investigate the effect of incorporating OSA starches on dough structural (SEM imaging), empirical (Mixolab, Alveograph, Rheofermentometre) and fundamental (oscillatory and creep measurements) rheological properties as well as bread quality parameters (specific loaf volume, crust and crumb colour, crumb moisture, crumb grain features, crumb texture). In addition, the bread quality attributes during storage were also monitored in order to get insight into bread stalling kinetics.<br />The results obtained in this thesis revealed that the rheological behaviour of OSA starch supplemented dough depended on the OSA starch granule rigidity, i.e. extent of OSA starch granule disintegration and polysaccharide degradation during modification. OSA-ST starch caused a reinforcement of the gluten network, as shown by the increase in storage modulus of doughs and gluten. On contrary, Pregel and Hydrol OSA-ST affected the continuity of gluten network which became porous and thus produced softer and stickier doughs in comparison to control. Investigations on real dough and model systems containing wheat and OSA starches revealed that all three types of OSA starches reduced starch retrogradation.<br />In general, all the examined emulsifying starches increased bread loaf volume in comparison to control bread with no added polymers, while Pregel OSA starch has expressed the greatest impact. It also reflected on bread crumb structural features and consequently on the crumb mechanical properties which were used for bread stalling monitoring. Firmness values of OSA-ST and Pregel OSA-ST starch supplemented bread crumbs, after 24 h of storage, were similar to or significantly lower than those of control determined 2 h after baking.</p>