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Master of Science / Department of Grain Science and Industry / Yong Cheng Shi / Maltogenic amylases are widely being used as an antistaling agent in baking industry. However, their action on starch in granular, swelled and dispersed forms, important components formed during bread baking, is largely unknown. Actions of two maltogenic amylases- A and -B on waxy maize starch (WMS) (100% amylopectin) and normal wheat starch (NWS) (~25% amylose) were studied and compared. For any given starch type, starch form, and hydrolysis time, maltogenic amylase-B hydrolyzed both starches more than maltogenic amylase-A as seen through sugar profile analysis indicating its higher degree of multiple attack action (DMA). Their action on non reducing ends blocked compound, p nitrophenol maltoheptaoside, confirmed their endo action. Maltogenic amylase-B showed a higher endo to total enzyme activity ratio than maltogenic amylase-A at any given enzyme weight. Greater MW reduction of dispersed starches by maltogenic amylase-B indicates its higher level of inner chain attack (LICA). Interestingly, MW distributions profiles of swelled starch hydrolysates did not show significant differences irrespective of swelling temperatures. Both enzymes showed differences in oligosaccharides compositions in dispersed and swelled starches’ reaction mixtures with sugars of degree of polymerization (DP) > 2 being degraded to glucose and maltose during later stages. For granular starches, enzymes followed a random pattern of formation and degradation of sugars with DP >2. MW distributions of hydrolyzed granular starches did not show significant shift until at the end of 24h when a low MW peak was observed. Morphological study of granular starches showed that maltogenic amylase-A mainly caused pinholes on WMS while maltogenic amylase-B caused surface corrosion with fewer pinholes. For NWS, both enzymes degraded A granules with deep cavities formation during later stages. A decrease in crystallinity of granular starches means that enzymes were able to hydrolyze both amorphous and crystalline regions. These results indicate that maltogenic amylase-B with a high LICA and high DMA possesses a better starch binding domain which can decrease the starch MW without affecting bread resilience. Strucuture of maltogenic amylase-A modified amylopectin (AP) in relation to its retrogradation was also studied. AP retrogradation was completely inhibited at % DH ≥ 20. MW and chain length distributions of debranched residual AP indicated with increase in % DH, a high proportion of unit chains with DP ≤ 9 and low proportion of unit chains with DP ≥ 17 were formed. Higher proportion of short outer AP chains which cannot participate in double helices formation supports the decrease and eventually complete inhibition of retrogradation. Thus, maltogenic amylase-A can play a very powerful role in inhibiting starch retrogradation even at limited DH (%).

Submitted by FLÁVIA DE AQUINO CUTRIM FARIAS null (flavia_cutrim@ifma.edu.br) on 2017-07-04T12:32:45Z No. of bitstreams: 1 TESE-FLÁVIA CUTRIM Farias (1).pdf: 1973425 bytes, checksum: b19b213ea6c0f5ad7bd758faa989e1f7 (MD5) / Approved for entry into archive by Luiz Galeffi (luizgaleffi@gmail.com) on 2017-07-04T18:19:07Z (GMT) No. of bitstreams: 1 farias_fac_dr_sjrp.pdf: 1973425 bytes, checksum: b19b213ea6c0f5ad7bd758faa989e1f7 (MD5) / Made available in DSpace on 2017-07-04T18:19:07Z (GMT). No. of bitstreams: 1 farias_fac_dr_sjrp.pdf: 1973425 bytes, checksum: b19b213ea6c0f5ad7bd758faa989e1f7 (MD5) Previous issue date: 2017-06-29 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / Há um grande interesse em se produzir álcool por matérias-primas alternativas à cana-de-açúcar. As fontes amiláceas tropicais são alvos potenciais nestas pesquisas. A taioba é uma planta que contem um teor considerável de amido nos seus tubérculos, mas é pouco explorada cientifica e comercialmente. Este trabalho teve como objetivo avaliar o potencial industrial da taioba. Para isto, determinaram-se as características estruturais e físico-químicas do amido de taioba, e, em seguida, se avaliou o potencial para a produção de etanol. Todas as analises foram realizadas em comparação ao amido de mandioca, por ser uma fonte conhecida e bem difundida no Brasil. Os amidos apresentaram alto grau de pureza e baixo teor de fósforo (< 0,05%). O amido de taioba apresentou 21,80 % de amilose aparente e 16,96 % de amilose absoluta. Os amidos exibiram perda de água (sinérese) durante a estocagem em todas as temperaturas testadas, mas a menor porcentagem de perda em ambos os amidos foi a 25 °C. O amido de taioba apresentou temperaturas de gelatinização mais elevadas, maiores alterações de entalpia de gelatinização e maiores percentagens de retrogradação, mas com valores de hidrólise menores que o amido de mandioca, sendo que essas diferenças podem ser atribuídas à menor proporção de cadeias ramificadas curtas (DP 6-12) da amilopectina e à maior viscosidade final do amido de taioba. O amido de taioba foi sacarificado enzimaticamente e submetido à fermentação usando a levedura Saccharomyces cerevisiae JP1. A concentração máxima de etanol produzida foi de aproximadamente de 56,34 e 48,38 g.L-1, com produtividade de 0,67 e 0,56 g.L-1.h-1 e rendimentos na faixa de 0,49 e 0,46 para os hidrolisados de mandioca e taioba, respectivamente. A eficiência de conversão em álcool dos hidrolisados de mandioca foi de 96,8 % e taioba de 89,57 %. Este estudo obteve resultados inéditos e úteis para avaliar o emprego de tubérculo de taioba para desenvolvimento de produtos de valor agregado destinados a alimentos e combustível. / There is a great interest in producing alcohol for raw materials that are alternative to sugarcane. Tropical amylaceous sources are potential targets in these surveys. Tannia is a plant that contains a considerable amount of starch in its tubers, but is little explored scientifically and commercially. This work aimed to evaluate the industrial potential of this plant. For this, the structural and physicochemical characteristics of the tannia starch were determined, and then the potential for the production of ethanol was evaluated. All the analyzes were carried out in comparison to cassava starch, because it is a known and well-known source in Brazil. The starches presented high purity and low phosphorus content (<0.05%). Tannia starch had 21.80% apparent amylose and 16.96% absolute amylose. Starches exhibited loss of water (syneresis) during storage at all temperatures tested, but the lowest percentage loss in both starches was at 25 oC. Tannia starch showed higher gelatinization temperatures, greater gelatinization enthalpy changes and higher percentages of retrogradation, but with hydrolysis values lower than cassava starch, and these differences can be attributed to the lower proportion of short branched chains (DP 6-12) of the amylopectin and the higher final viscosity of the tannia starch. The tannia starch was saccharified enzymatically and subjected to fermentation using the yeast Saccharomyces cerevisiae JP1. The maximum concentration of ethanol produced was approximately 56.34 and 48.38 g.L-1, with yields of 0.67 and 0.56 gL-1.h-1 and yields in the range of 0.49 and 0.46. For the cassava and tannia hydrolysates, respectively. The alcohol conversion efficiency of cassava hydrolysates was 96.8% and tannia 89.57%. This study has obtained unpublished and useful results to evaluate the use of tuber tubers for the development of value-added products for food and fuel.

Master of Science / Food Science Institute / J. Scott Smith / The tortilla segment of the Mexican food market in the United States is rapidly growing. Tortillas are being used in many different mainstream applications, including wraps, lasagna, pizza, and appetizers. In 2000, the tortilla market was a $4 billion industry and with more than 85 billion tortillas consumed in the United States alone. As Mexican food becomes more common in the American diet, consumers start to branch out into a more authentic presentation of Mexican food. This causes a shift in consumption from flour to corn tortillas. As the consumer demand for corn tortillas increases, food manufacturing companies are challenged with producing a tortilla that will retain its softness, pliability, foldability, and flavor while remaining safe for consumption over several months. Since tortillas have two modes of deterioration, mold and staling, there are several factors that need to be considered. Hurdle technology is employed to prevent mold growth. By adjusting water activity, pH, storage temperature, and addition of preservatives mold growth can be prevented for a period of several months. Retaining tortilla texture over time is much more complicated. Tortillas stale through a complicated process of starch retrogradation. During cooking, the starch granules gelatinize and amylose and amylopectin leech out of the granules. After the tortillas are baked, the starch immediately begins to retrograde. The amylose and amylopectin complex together form a matrix that stiffens the tortilla. Based on current research, the shelf life of a corn tortilla can be extended through a combination of CMC (0.5%), maltogenic amylase (1650 Activity Units), sorbitol (3%), glycerol (4%).

This study investigates the depositional history of the Late Eocene sedimentary record in the northwest of the Thrace Basin in a sequence stratigraphic approach and estimates the contribution of regional tectonics, basin physiography and eustasy. Late Eocene sedimentary succession was analyzed in two third-order sequences based on two major data sets / seismic reflection and well data sets. Depositional Sequence-1, represented by progradational stacking patterns, comprises the coarse-grained Hamitabat turbidite system. The base of the Sequence-1 was defined as the base of channel fill deposits in the northern shelf setting and the base of slope fan deposits in the slope setting. This boundary separates Lower-Middle and Upper Eocene sediments. In the slope setting, the Hamitabat turbidite system was analyzed in three major depocenters / Western, Northwestern and Northeastern depocenters respectively. Hamitabat turbidite system was controlled by the interaction of regional tectonics, basin physiography and eustatic fluctuations in the Late Eocene. This study highlighted the role of the regional variables / tectonic influence and basin morphology on the submarine canyon formation. The facies distribution was controlled by the high subsidence rate of sea-floor dominantly instead of eustasy. Depositional Sequence-2, represented by mostly retrogradational stacking patterns, is a clastic-carbonate mixed system. Depositional Sequence-2 was subdivided into three higher-order sequences. The lower sequence boundaries were induced by the rapid relative sea-level rise. The upper boundary of the Depositional Sequence-2 was defined as the termination of clastic-carbonate mixed system and a candidate for the Eocene-Oligocene contact.

Master of Science / Department of Grain Science and Industry / Yong Cheng Shi / Waxy wheat starch (WWS) containing little or no amylose has unique properties for food and industrial uses. Hydroxypropylation, a widely used means for modifying starches, could enhance functionalities of starch by substituting hydroxyl groups in starch. There are limited numbers of literatures regarding hydroxypropylation of WWS. WWS hydroxypropylated with 3.0-9.0% propylene oxide (PO) were prepared and compared to hydroxypropylated normal wheat starch (NWS) and hydroxypropylated waxy maize starch (WMS). The molar substitution (MS) of the resulting hydroxypropylated NWS, WWS and WMS was 0.055-0.151, 0.048-0.133, and 0.049-0.139, respectively. Gelatinization temperatures and enthalpy of hydroxypropylated starches were significantly lower than those of their unmodified counterparts and the extent of decrease was positively correlated to the MS. Differential scanning colorimetry (DSC) results showed that hydroxypropylation reduced the retrogradation of the starches during the storage after gelatinization but there were differences between the starches. For the same level of PO reaction (3 and 5% PO), hydroxypropylated WWS retrogradated less than hydroxypropylated WMS, suggesting that for the same level of cold storage stability, less PO is needed for WWS. After reacted with 6% PO, MS was 0.092 and 0.094, respectively, for WWS and WMS, and no retrogradation was observed for those hydroxypropylated starches, indicating that at MS ~0.094, hydroxypropyl groups prevents amylopectin chains from re-associating and forming crystalline structures. In contrast, a higher level of PO (9%) was needed to react with NWS to achieve the hydroxypropylated starch with an MS of 0.151 that gave no retrogradation. Consistent with microscopic observation results, Micro-Visco-Amylograph (MVA) analysis showed hydroxypropylated starches developed viscosity at lower temperatures and had improved hot and cold viscosities. The specific characteristics of hydroxypropylated starches are related to the degree of hydroxypropylation. Therefore, it is critical to determine the level of hydroxypropylation in modified starches. 1H NMR is a simple and rapid means of determining hydroxypropyl (HP) group in modified starches. In this study, a method to prepare a HP starch for NMR analysis was improved. The optimum parameters proposed to hydrolyze HP starches were 10% starch solid content, 3.5% (wt.%) DCl in D2O as the solvent, sodium acetate as an internal standard, heating at 90oC for 1 h. Optionally, 6% (v/v) trifluoroacetic acid-d as the water-peak shifting reagent. Six hydroxypropylated starch samples and two commercial cross-linked and hydroxypropylated starch samples were hydrolyzed with this modified method before 1H NMR analysis, and the results of HP group content in the samples were in agreement with the results from an enzyme-catalyzed method, which indicate that the improved acid hydrolysis method is applicable for both hydroxypropylated starch and cross-linked and hydroxypropylated starch.

Les systèmes turbiditiques forment de grands édifices sédimentaires sous-marins situés au large des fleuves en pied de pente continentale et constituent les dépôts terrigènes les plus distaux d’un système fluviatile. Leur structure interne, définie comme un empilement de systèmes chenal-levées, montre des changements architecturaux au cours du temps dont les forçages sont encore mal connus, et le rôle respectif des facteurs de contrôle interne (lié au fonctionnement propre du système) ou externe (climat, variations du niveau marin, tectonique) reste sujet à débats. Afin de mieux comprendre le rôle de ces facteurs de contrôle, une étude détaillée de l’architecture du système Congo a été réalisée. Cette étude a été menée dans le cadre du projet de recherche Reprezaï (Ifremer/IUEM, depuis 2006), faisant suite aux projets Guiness et ZaïAngo (Ifremer/Total, 1992-2003), projets au cours desquels de nombreuses campagnes en mer ont permis l'acquisition d’une importante base de données géophysiques et géologiques. Une analyse quantitative de différents paramètres architecturaux des chenaux (longueur totale, longueur construite après avulsion, entre autres) de l’Edifice Axial du Congo (derniers 200 ka) révèle des cycles sédimentaires de progradation et rétrogradation des dépôt-centres, les plus grandes rétrogradations correspondant à des avulsions situées très en amont dans l’édifice turbiditique. Les dépôts-centres identifiés à la terminaison des chenaux correspondent à des complexes de lobes (selon la nomenclature de Prélat et al., 2009) relativement allongés dont les volumes (de 3 à 196 km3) varient considérablement dans le temps et l'espace sans pour autant montrer de cycles de variation comme pour les autres paramètres. Le volume cumulé de ces complexes de lobes reconnus représente jusqu'à 31% du volume de l’Edifice Axial. L’étude multiproxies (datations 14C, δ18O, mesures XRF, Carbone Organique Total, …) de carottes prélevées sur les chenaux les plus progradants et les plus rétrogradants, a fourni un cadre chronologique permettant de caler temporellement ces cycles sédimentaires. L’évolution temporelle des paramètres architecturaux a été comparée avec les variations des signaux paléoenvironnementaux et paléoclimatiques (pollens, COT, mesures XRF et MSCL, argiles…) enregistrés par une carotte de référence située en domaine hémipélagique et contemporaine de la construction de l’Edifice Axial. Les résultats mettent en évidence un lien étroit entre l’évolution architecturale de l’édifice turbiditique et les décharges fluviatiles du Congo. Ces dernières, mais aussi l’extension du couvert végétal sur le bassin versant, contrôlent le rapport sable/argile et donc, en partie, la capacité de transport des courants turbiditiques. Ces deux facteurs dépendent des précipitations liées aux variations d’intensité de la mousson en relation avec les cycles de précession (19-23 ka, Milankovitch). Un scénario de mise en place des systèmes chenal-levées et lobes de l’Edifice Axial en fonction des variations climatiques arides/humides sur le bassin versant a ainsi pu être proposé grâce à de bonnes contraintes stratigraphiques pour les derniers 40 ka. En période aride, les courants turbiditiques, peu fréquents et avec un fort rapport sable/argile qui diminue leur capacité de transport, sont propices à l'aggradation des chenaux, engendrant des conditions favorables pour la création ultérieure d’avulsions en amont. En période de transition aride/humide, lorsque le couvert végétal est encore peu développé, la décharge fluviatile accompagnée d’une charge solide importante augmente le volume des courants turbiditiques, favorisant les avulsions en amont du système. Enfin, les périodes humides, caractérisées par un débit liquide fort associé à une charge solide essentiellement argileuse qui décroît au fur et à mesure que le couvert végétal s’étend, génèrent des courants de turbidité dont la capacité de transport diminue au cours du temps […] / Turbidite systems are huge submarine sedimentary fans located off rivers, at the foot of the continental slope. They constitute the most distal terrigeneous deposits of a fluvial system. Their internal structure, defined as a stacking of channel-levee systems, show architectural changes through time. Forcing factors of these architectural changesare still poorly understood, and the respective role of internal (related to the own functioning of the system) or external forcing factors (climate, seal-level variations, tectonics) remains debated. To better understand the role of these controlling factors, a detailed study of the Congo system architecture was carried out. This study was conducted as part of the Reprezaï research project (Ifremer/IUEM, since 2006), following the Guiness and ZaïAngo projects (Ifremer/Total, 1992-2003), during which many oceanographic surveys allowed acquiring an important geophysical and geological data base. A quantitative analysis of different architectural parameters from the channels (e.g. total length, length built after avulsion,…) of the Congo Axial Fan (last 200 ka) reveals progradational-retrogradational sedimentary cycles of the depocenters, the highest retrogradations corresponding to avulsions located very upfan. Depocenters identified at the termination of the channels correspond to relatively elongated lobe complexes (according to the nomenclature of Prélat et al., 2009) with greatly variable volumes (from 3 to 196 km3) both in time and space, without any cyclicity like that identified by other parameters. The cumulative volume of these lobe complexes represents up to 31% of the Axial Fan volume. The multiproxies study (14C dating, δ18O, XRF measurements, Total Organic Carbon…) of cores sampled on the most prograding and retrograding channels provided a chronological framework to these sedimentary cycles. The temporal evolution of the architectural parameters was compared with changes in paleoenvironmental and paleoclimatic signals (pollens, TOC, XRF and MSCL measurements, clay mineralogy,…) recorded in the sediments of a reference core deposited simultaneously to the Axial Fan, but located outside the turbidite flows. Results highlight a strong link between the architectural evolution of the turbidite system and the Congo River discharge. These, as well as the expansion of the vegetation cover in the catchment area, control the sand/clay ratio and thus, at least partly, the transport capacity of turbidity currents that build the channel-levee systems. Both factors depend on rainfall related to the monsoon intensity variations in relation with precession (19-23 ka Milankovitch). A scenario for the deposition of channel-levee systems and lobes of the Axial Fan in link with arid/humid climate variations in the catchment area has been proposed thanks to good stratigraphic constraints for the last 40 ka. During arid periods, turbidity currents are infrequent and present a high sand/clay ratio which decreases their transport capacity. These turbidity currents are suitable to channel aggradation, generating favorable conditions for the subsequent creation of upfan avulsion. During periods of transition of arid to humid conditions, when the canopy is still underdeveloped, fluvial discharge and significant sediment load increases result in an increase of the turbidity currents volume, which favors upfan avulsions. Finally, during humid periods, Congo discharge is characterized by a strong liquid flow and a mainly clayey solid discharge which decreases gradually as the canopy extends. These conditions generate turbidity currents with decreasing transport capacity through time. However the transport capacity of these currents remains sufficient to reach distal portions of the systems and favor channels progradation. This climatic factor seems therefore to regularly disrupt the more perennial internal control which is also highlighted by the Congo Axial Fan architecture.

La migration de l’eau est un sujet générique dans divers domaines dont l'analyse permet de mieux comprendre les propriétés rhéologiques, sensorielles et de conservation des produits au cours du temps. Les apports de la relaxométrie et de la micro-imagerie par RMN dans ce domaine sont larges et d’un intérêt majeur au vue des caractéristiques non-invasives, non-destructives et quantitatives de ces méthodes, utilisables alors que le produit est en cours de transformation. Deux méthodologies ont été développées afin d’étudier les transferts de protons sur une large gamme de temps et de distance. La première a consisté à implémenter de nouvelles méthodes d’acquisition et de traitement du signal de RMN à bas champ (20 MHz) en 2D pour corréler non seulement les temps de relaxation T1 et T2 mais également les coefficients de diffusion translationnelle D et T2 sur des échantillons modèles amidon-eau de diverses origines botaniques (blé, pomme de terre et maïs cireux). Les mesures 2D se sont révélées suffisamment robustes pour quantifier les transferts de protons de l’eau et des polymères d’amidon pendant leur gonflement, leur gélatinisation et leur rétrogradation. Une approche complémentaire en micro-imagerie par RMN (500 MHz) a consisté à mesurer au cours du temps des profils de concentration de l’eau pénétrant sur plusieurs millimètres dans un extrudé d’amidon de pomme de terre contenant du glycérol. La diffusion de transport de l'eau et le taux de gonflement de l’extrudé ont été quantifiés à 22°C pendant plus de 20h. / Water migration is a generic subject in various fields, the analysis of which makes it possible to better understand the rheological, sensory and conservation properties of products over time. The contributions of relaxation and NMR micro-imaging in the field are broad and of major interest in view of the non-invasive, non-destructive and quantitative characteristics of these methods, which can be used while the product is under processing. Two methodologies have been developed to study the transfers in a wide range of time and length. The first consisted in implementing new methods of acquisition and processing of the NMR signal in 2D at low-field (20 MHz) to correlate not only the relaxation times T1 and T2 , but also the translational diffusion coefficients D and T2 on starch-water model samples from various botanical origins (wheat, potato and waxy corn). The 2D measurements have proved sufficiently robust to quantify the transfers of protons from water and starch polymers during their swelling, gelatinization and retrogradation. A complementary approach by MR micro-imaging (at 500 MHz) consisted in measuring, over time, the water uptake on several millimeters in an extrudate of potato starch containing glycerol. The diffusion transport of the water and the rate of the extrudate swelling were quantified at 22°C for more than 20 hours.

<p>Maize is one of the top sources of food starch. Industrial use of starch is mostly in its native form and used due to their functional and structural properties. Native starch properties and functionalities have been altered using chemical. An alternative for the development of native starch substituents with desirable starch properties is the use of mutagenesis techniques to increase genetic variation in maize kernels. With this approach, a highly diverse library of native starches with different properties are produced. Traditional analysis of the functional and structural properties requires generous amounts of material as well as a time-consuming and costly breeding process to obtain enough kernels. To address this difficulty, high-throughput techniques are proposed for studying starch properties and functions which includes a 1) single kernel sampling method for the isolation of milligrams of starch, and techniques for studying starch based on functional properties, 2) retrogradation and 3) shear resistance, using low-volume low-concentration starch pastes.</p><p>First, three mechanical approaches were evaluated for the collection of endosperm samples from individual kernels: razor blade, 1.5 mm drill bit, and trephine bur. Furthermore, two methods for the isolation of crude starch from endosperm samples (steeping method and combination of proteases and sonication) were compared. In this study, the mechanical approaches were evaluated using the recovery rate, throughput, and germination rate of sampled kernels. Moreover, yield determination, particle size distribution, and morphological evaluation using a light microscope were performed on crude starch isolated from the endosperm samples. The use of trephine bur to collect endosperm samples and isolation of crude starch using protease digestion and sonication showed the best combination for a high-throughput setting. </p><p>Second, a high-throughput technique using milligram sample for the screening of retrogradation-resistant starch was evaluated by comparing two spectrophotometric techniques: turbidity method and molecular rotor (MR). MRs are fluorescent probes with high sensitivity to the viscosity of their environment, polarity of the media, molecular crowding, and free volume. After excitation, MRs relax through rotational movement and reduces the emission of fluorescence. In this study, hydroxypropylated waxy corn starch (WCS) and hydroxypropylated normal corn starch (NCS) were used and their retrogradation kinetics was compared with retrogradation kinetics of native WCS and NCS. </p><p>It was found that the molecular rotor 9-(2-carboxy-2-cyaovinyl)-julolidine (CCVJ) was effective to sense changes during slow retrogradation of amylose-containing starch pastes. Development of elastic modulus of retrograded NCS pastes obtained from dynamical rheology showed high correlation with the development of fluorescence intensity of the CCVJ. Furthermore, rate of retrogradation using fluorescence intensity was affected by the introduction of a retrogradation inhibitor, hydroxypropyl groups. Accelerated retrogradation of low-concentration WCS pastes was measured using the turbidity method and fluorescence intensity of CCVJ in a microplate. Accelerated retrogradation was performed by subjecting the low-concentration WCS pastes to six freeze-thaw cycles of -20 ºC for 1 hour and 30 ºC for 1 hour. Overall, development of turbidity resulted in the more sensitive technique to detect rate of retrogradation of amylopectin-containing starch. </p><p>The last part of this research studied the use of CCVJ as a technique to identify shear-resistant starch in starch slurries using milligram sample. For this purpose, WCS was cross-linked with sodium trimetaphosphate (STMP) and phosphoryl chloride (POCl₃). Low-volume starch slurries having CCVJ were prepared ranging from 0.5% to 1% starch concentration in a 96-well PCR plates and subjected to heat and shear treatments. It was found that fluorescence intensity measured in native WCS pastes were the lowest. Furthermore, fluorescence intensity of the CCVJ in the gelatinized starch increased as the amount of cross-linker increased in the cross-linked WCS. After shear treatments, the same trend in fluorescence intensity increase was recorded in all the crosslinked WCS. Results obtained using fluorescence intensity were compared with rapid viscosity analyzer (RVA) and images from microscope. Results obtained from both techniques corroborated the findings using fluorescence intensity.</p><p>In general, the findings of this research provide new insights into the possibilities of developing a high-throughput screening platform of milligram starch sample based on their physical properties. </p>

Made available in DSpace on 2017-07-21T18:53:04Z (GMT). No. of bitstreams: 1 ANDRESSA GABARDO GRANZA.pdf: 2807698 bytes, checksum: a0442acfb9a8bff732a7ec5ecaa9a286 (MD5) Previous issue date: 2015-02-05 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / The development of gluten free products is becoming increasingly important as the number of celiac people have increased. Cheese breads and sour cassava starch biscuits are examples of gluten free baked products widely consumed in Brazil, however, these products have problems related to starch retrogradation, in other words, a very rapid staling in the case of baked products and the cheese breads marketed as frozen dough are susceptible to release of water (syneresis). Thus, the objective of this study was to develop a anti-staling premix able to increase freeze-thaw stability of gluten free baked products (cheese bread and sour cassava starch biscuits) without interfere negatively on the expansion property of these products. Binary and ternary mixtures were prepared using native cassava starch and oxidized cassava starch ranging the type of gum (guar, locust, xanthan and carrageenan) and the concentration used (2, 4 and 6 %). Mixtures using the acid modified cassava starch instead of oxidized cassava starch were also tested, but in this case using only guar gum at concentrations of 2, 4 and 6 %. The mixtures were evaluated for freeze-thaw stability and expansion property and the results were compared with those obtained for sour cassava starch (PA) native cassava starch (N), oxidized cassava starch (O) and acid modified cassava starch (A). The binary and ternary mixtures with better results and samples PA, N and O were evaluated for technological properties (pasting properties, swelling power and solubility and paste clarity), thermal properties (Differential Scanning Calorimetry - DSC), structural properties (Fourier Transform Infrared Spectroscopy - FTIR) and crystalline properties (X-ray diffraction); moreover, cheese breads were prepared with these samples and the staling of these products was evaluated (hardness parameter in texturometer and crumb moisture content). The mixture made with the native cassava starch, oxidized cassava starch and guar gum at a concentration of 4 % (MNO+GG 4 %) showed the best results of syneresis (loss of 4,87; 7,79 and 11 % in the 1st, 2nd and 3rd freeze-thaw cycle, respectively) compared with the other samples and the low retrogradation of this sample was confirmed by DSC analysis (enthalpy of retrogradation was non-existent) and FTIR (sample separated from others by principal component analysis - PCA). The expansion property of MNO GG+4 % sample was high (> 10 mL.g-1) and the cheese breads developed with this sample had a later staling compared with other samples, with lower hardness after 24 and 30 h of storage (23.71 and 29.59 N, respectively) and a wetter crumb (38.8 and 37.07%, respectively). These results indicate the possibility of using the premix MNO+GG 4% in gluten free baked products in place of sour cassava starch and/or native cassava starch. / O desenvolvimento de produtos livres de glúten está se tornando cada vez mais importante uma vez que o número de pessoas celíacas tem aumentado. Pães de queijo e biscoitos de polvilho são exemplos de produtos panificados livres de glúten consumidos em território brasileiro, porém, estes produtos possuem problemas relacionados com a retrogradação do amido, ou seja, um envelhecimento muito rápido no caso de produtos assados e os pães de queijo comercializados na forma de massa congelada estão susceptíveis à liberação de água (sinérese). Dessa forma, o objetivo do presente trabalho foi desenvolver uma pré-mistura capaz de retardar o envelhecimento e aumentar a estabilidade ao congelamento-descongelamento de produtos panificados livres de glúten (pães de queijo e biscoitos de polvilho), além de não interferir negativamente na propriedade de expansão dos mesmos. Misturas binárias e ternárias foram elaboradas utilizando-se o amido de mandioca nativo e o amido de mandioca oxidado variando-se o tipo de goma (guar, locusta, xantana e carragena) e a concentração utilizada (2, 4 e 6 %). Misturas utilizando o amido de mandioca ácido modificado ao invés do amido de mandioca oxidado também foram testadas, mas neste caso utilizando somente a goma guar nas concentrações de 2, 4 e 6 %. As misturas foram avaliadas quanto à estabilidade a ciclos de congelamento-descongelamento e propriedade de expansão e os resultados foram comparados com os obtidos para o polvilho azedo (PA), amido de mandioca nativo (N), amido de mandioca oxidado (O) e amido de mandioca ácido modificado (A). As misturas binárias e ternárias com melhores resultados e as amostras PA, N e O foram avaliadas quanto às propriedades tecnológicas (propriedade de pasta, poder de intumescimento e solubilidade, e claridade de pasta), térmicas (calorimetria exploratória diferencial - DSC), estruturais (Espectroscopia de infravermelho por transformada de Fourier - FTIR) e cristalinas (difração de raios X); além disso, foram elaborados pães de queijo com essas amostras e o envelhecimento dos mesmos foi avaliado (parâmetro dureza em texturômetro e teor de umidade dos miolos). A mistura feita com o amido de mandioca nativo, amido de mandioca oxidado e goma guar na concentração de 4 % (MNO+GG 4 %) apresentou os melhores resultados de sinérese (perdas de 4,87; 7,79 e 11 % no 1º, 2º e 3º ciclo de congelamento-descongelamento, respectivamente) em comparação com as demais amostras e a baixa retrogradação desta amostra foi confirmada pela análise de DSC (entalpia de retrogradação foi inexistente) e FTIR (amostra separada das demais pela análise de componentes principais – PCA). A propriedade de expansão da amostra MNO+GG 4 % foi considerada elevada (>10 mL.g-1) e os pães de queijo desenvolvidos com esta amostra tiveram um envelhecimento mais tardio em relação as demais amostras, apresentando menor dureza após 24 e 30 h de armazenamento (23,71 e 29,59 N, respectivamente) e um miolo mais úmido (38,8 e 37,07 %, respectivamente). Esses resultados indicam a possibilidade de utilização da pré-mistura MNO+GG 4 % em produtos panificados livres de glúten, em substituição do polvilho azedo e/ou amido de mandioca nativo.