Master of Science / Department of Grain Science and Industry / Yong-Cheng Shi / Sorghum flour is a gluten-free ingredient and can be used to prepare foods for celiac patients. In addition, sorghum flour is a good source of fiber in the form of resistant starch. The objectives of this research were to develop an effective process to increase resistant starch content of sorghum flour and investigate the effects of sorghum protein matrix on starch digestibility. Samples of white sorghum flour (28.9% amylose content) with different moisture contents (0%, 12.5%, 20%, and 30%) were treated at different temperatures (100, 120, and 140 [degrees]C) for different times (1, 2, and 4 h). Samples after heat treatments were tested for starch digestibility, protein digestibility, differential scanning calorimetry (DSC), size-exclusion chromatography (SEC), and X-ray diffraction. The sample treated with 20% moisture at 100[degrees]C for 4 h had high resistant starch (RS) content (22.1% compared with 5.6% of the native sample) and low protein digestibility (8.4% compared with 68.3% of the native sample). The same heat-moisture treatment on isolated sorghum starch showed no significant change in RS content. DSC showed a very low degree of gelatinization for samples treated at moisture contents 20% and below. X-ray diffraction also suggested minimal change in starch crystallinity after heat treatment at low moisture contents (20% and below). Sorghum protein solubility after heat treatment was reduced, suggesting that protein structure was altered during the heat treatments. In conclusion, heat-moisture treatments were successful in increasing resistant starch content of sorghum flour by altering sorghum protein without gelatinizing the starch to retain starch functionality in food product applications. Sorghum flour with increased resistant starch content after heat treatment was evaluated and compared with normal sorghum flour for starch digestibility using the Integrated Total Dietary Fiber method, and for food applications in tortillas.

The main objectives of this study were to develop an effective process to produce modified pea starch with enhanced enzyme resistance property (RS) for food applications. The work compares a non-chemical method (heat moisture treatment) versus a chemical method (crosslinking). One type of commercial pea starch (Nutri-Pea) was used exclusively as the raw material in this study. A number of methods were used to characterize the properties of the modified pea starches: water solubility index (WSI), titration (conversion, iodine value), intrinsic viscosity, infrared spectroscopy (FT-IR), Englyst digestion method, total starch content, and rapid visco analysis (RVA). The effects of heat-moisture treatment on native pea starch and enzyme treated pea starch were examined. The results showed that the produced samples with both native starch and enzyme treated starch exhibited a sharp increase in intrinsic viscosity. Overall, this method was deemed undesirable and not extensively examined past preliminary evaluations. The main focus of the study was on a citric acid crosslinking reaction, chosen for its food compliancy. A temperature of 120 oC was considered ideal for the reaction. FT-IR confirmed the presence of the citric acid incorporation in the starch samples. To improve the extent of reaction, Butanetetracarboxylic acid (BTCA) was considered as a replacement for citric acid and its treated samples showed higher conversion and lower water solubility index than that of the citric acid treated samples. Sodium propionate (NaP) was also considered in the reaction, this time as a food-grade catalyst and found to have minor benefit in cross-linking. BTCA/NaP treated sample reached the highest conversion of the study (96.8±2.3 %) and the lowest WSI (13.1±2.0 %), which increased the RS fraction of the starch from 18% to 32%. The RVA pasting profiles examined were too low to compare due to the high degree of cross-linking. Further improvements to RS were sought by debranching the starch before acid crosslinking. A BTCA/NaP treated sample with enzyme treatment showed a low WSI (31.7±2.3 %) yet substantially higher RS fraction (80.81±0.18 %). Similar to the non-debranched acid modified samples, there were no significant RVA pasting results because of the high cross-linking. Finally, crosslinking with an epoxidized oil was tested to continue looking at food-grade solution yet possible increase the rate of the crosslinking reaction. The results of WSI indicated that this method had little influence on cross-linking, possibly due to the low epoxidation efficiency of vegetable oils, as determined by iodine value. / Thesis / Master of Applied Science (MASc)

Submitted by Eunice Novais (enovais@uepg.br) on 2018-05-08T17:08:35Z No. of bitstreams: 2 license_rdf: 811 bytes, checksum: e39d27027a6cc9cb039ad269a5db8e34 (MD5) Luísa Thomaz.pdf: 3102790 bytes, checksum: ae052fcfec624f47d0de773ff533ce4f (MD5) / Made available in DSpace on 2018-05-08T17:08:35Z (GMT). No. of bitstreams: 2 license_rdf: 811 bytes, checksum: e39d27027a6cc9cb039ad269a5db8e34 (MD5) Luísa Thomaz.pdf: 3102790 bytes, checksum: ae052fcfec624f47d0de773ff533ce4f (MD5) Previous issue date: 2018-03-09 / Conselho Nacional de Desenvolvimento Científico e Tecnológico / O taro (Colocasia esculenta L. Schott) é um tubérculo que apresenta até 80 % de material amiláceo em sua composição (base seca), possuindo grânulos pequenos, medindo de 1 μm a 6 μm, enquanto que outras fontes chegam a 100 μm. Amidos nativos podem apresentar limitações tecnológicas e, portanto, modificações físicas, químicas e biológicas são realizadas para ampliar a gama de sua utilização. Neste estudo foi utilizado o amido de taro orgânico, o qual foi modificado por tratamento hidrotérmico (HMT) a partir da variação do teor de umidade (13, 19 e 25 %) e tempo (45, 60 e 75 min), mantendo fixa a temperatura (120 °C). Após esses tratamentos foi aplicado o ultrassom em todas as amostras durante 30 min e amplitude de 60 % (frequência fixa de 20 kHz). Para avaliação e caracterização da amostra nativa e das modificadas foram obtidas imagens por microscopia eletrônica de varredura por efeito de campo (MEV/FEG), as propriedades de pasta por viscoamilografia (RVA), decomposição térmica por termogravimetria (TG), evento de gelatinização por calorimetria exploratória diferencial (DSC) e padrão de cristalinidade por difratometria de raios X (DRX). Houve alteração significativa na cristalinidade relativa, variando de 26,9 % a 32,7 %. O perfil de pasta obteve redução em todos os parâmetros de viscosidade e, no evento de gelatinização, foi observado um aumento de entalpia para todas as condições de HMT, chegando a 14,88 J/g (amostra nativa: 9,45 J/g), além de um alargamento do pico, sugerindo uma maior estabilidade frente ao aquecimento. Devido a esta característica, estudos sugerem aplicação do amido hidrotermicamente tratado em produtos enlatados e congelados. As amostras duplamente modificadas promoveram um encurtamento do evento de gelatinização e redução da entalpia, tendo como menor valor 4,1 J/g; tais resultados ocorreram devido a maior hidratação e menor inchamento do grânulo, o que sugere uma boa dispersibilidade, com possível aplicação em filmes biodegradáveis. / Taro (Colocasia esculenta L. Schott) is a tuber that possesses up to 80% of starchy material in its composition (dry basis) and the size of its granules ranges from 1 μm to 6 μm, while other fonts may have granules up to 100 μm. Native starches can present technological processing limitations, and thus, physical, chemical and biological modifications are performed to improve its application range. In this study, organic taro starch was modified by heat-moisture treatment (HMT), with different moisture levels (13, 19 and 25%) and different time intervals (45, 60 and 75 min). All treatments were performed at 120 °C followed by ultrasound (US) for dual modification. The US was applied for 30 min and 60% of amplitude, at a fixed frequency of 20 kHz, for all samples. The morphology of the native and modified samples where evaluated by scanning electron microscopy (SEM), the pasting properties by viscoamilography (RVA), the gelatinization event by differential scanning calorimeter (DSC) and cristallinity pattern by X-ray difratometry. The major differences where in the relative crystallinity that increased from 26.9% to 32.7%. Additionally, the pasting profile showed a decrease in all parameters. The gelatinization showed an enthalpy increase for all HMT-modified samples, up to 14.88 J/g (native sample: 9.45 J/g). Moreover, a peak broadening was observed, suggesting higher heating stability. Due to this, previous studies suggest that HMT starch can be used in canned and frozen food. The dual modified samples resulted in gelatinization shortening and had a decrease in enthalpy, reaching 4.1 J/g at the minimum. This is due to the higher hydration and lower swelling power of the granule, which indicates a good dispersibility. This gives the taro potential to be used in biodegradable films. Keywords: modified starch, ultrasound, heat-moisture treatment, non-convetional starch.

Submitted by Liliane Ferreira (ljuvencia30@gmail.com) on 2019-01-29T14:52:14Z No. of bitstreams: 2 Dissertação - Marília Cândido Fideles - 2018.pdf: 3128955 bytes, checksum: 7c96987d4cfb19f05d0952999fb570df (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) / Approved for entry into archive by Luciana Ferreira (lucgeral@gmail.com) on 2019-01-30T09:52:29Z (GMT) No. of bitstreams: 2 Dissertação - Marília Cândido Fideles - 2018.pdf: 3128955 bytes, checksum: 7c96987d4cfb19f05d0952999fb570df (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) / Made available in DSpace on 2019-01-30T09:52:29Z (GMT). No. of bitstreams: 2 Dissertação - Marília Cândido Fideles - 2018.pdf: 3128955 bytes, checksum: 7c96987d4cfb19f05d0952999fb570df (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) Previous issue date: 2019-12-20 / Arrowroot is a plant that has abundant starch content and does not present gluten in its composition, arousing the interest of its use in the production of pasta. However, gluten substitution must be provided through the use of techniques, such as the arrowroot flour modification through physical processes. Starch is the highest percentage of arrowroot composition, so enrichment of the dough is an interesting alternative, and a fortification with agroindustrial coproducts sources of fiber and protein, such as passion fruit peel and bovine rumen, may be viable. The objective of this study is to produce flours from agroindustrial coproducts, to modify by different methods (ultrassonic and heat-moisture treatment) the starch of arrowroot obtained and determine the viability technological and nutritional aspects of the use of modified flours and agroindustrial coproducts, source of fiber and protein, in the production of different types of pasta. The hydration, paste and thermal properties of raw and modified flours were evaluated. The results of the ultrasound treatments vary with the temperature between 35.83 and 62% with time between 5 and 15 minutes. For heat-moisture treatment, the best results were those using the lowest temperature (105 ° C) and shorter times (15 and 30 minutes). Taking into account the use of modified flours in the production of pasta, ultrasonic treatments with parameters of intensity of 43.5% and time of 15 min and heat-moisture treatment with 105 ° C for 15 min were selected. With the technological techniques of the pasta produced, it was possible to analyze and choose the best parameters to obtain a pasta with less cooking time, loss of solids, intermediate increase of pasta, and small values of firmness, angle Hue and C* chromaticity. The proximal composition of the pasta was satisfactory, being able to be characterized as a food with high protein content and high fiber content. The pastas with the greatest desirability are a good sensory acceptance. The results obtained have the possibility to develop and improve the pasta formulated with raw and modified arrowroot flour and agroindustrial coproducts. / A araruta é uma planta que apresenta conteúdo abundante de amido e não glúten em sua composição, despertando o interesse da sua utilização na produção de massas alimentícias. Porém a substituição do glúten deve ser suprida através da utilização de diferentes técnicas, como, por exemplo, a modificação da farinha por meio de processos físicos. O amido é o maior percentual da composição da araruta, portanto o enriquecimento da massa é uma alternativa interessante, e a fortificação com coprodutos agroindustriais fontes de fibra e proteína, como a casca de maracujá e o rúmen bovino, pode ser viável. O objetivo deste trabalho é produzir farinhas a partir de coprodutos agroindustriais, modificar por métodos distintos (ultrassom e tratamento térmico em baixa umidade - TTBU) o amido da farinha de araruta obtida e determinar a viabilidade tecnológica e nutricional da utilização das farinhas de araruta modificadas e de coprodutos agroindustriais na produção de diferentes tipos de massas alimentícias. Foram avaliadas as propriedades de hidratação, de pasta e térmicas das farinhas cruas e modificadas. Os melhores resultados dos tratamentos com ultrassom são os com intensidade variando entre 35,83 e 62% com tempo entre 5 e 15 minutos. Já para o TTBU os melhores resultados da modificação são os que utilizaram menor temperatura (105°C) e menores tempos (15 e 30 minutos). Levando em consideração o uso das farinhas modificadas na produção de massas alimentícias, foram selecionados os tratamentos de ultrassom com parâmetros de intensidade 43,5% e tempo 15 min e TTBU com temperatura de 105°C por 15 min. Através das análises tecnológicas das massas alimentícias produzidas foi possível analisar e escolher os melhores parâmetros para se obter uma massa com menor tempo ótimo de cozimento, perda de sólidos, intermediário aumento de massa, e menores valores de firmeza, ângulo Hue e cromaticidade C*. A composição proximal das massas foi satisfatória, podendo ser caracterizada como um alimento com alto teor de proteína e alto teor de fibra, de acordo com a legislação. As massas com maior desejabilidade apresentaram uma boa aceitação sensorial. Os resultados encontrados indicam a possibilidade de se desenvolver e aperfeiçoar massas alimentícias formuladas com farinha de araruta crua e modificadas e coprodutos agroindustriais.

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.