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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
321

Accuracy and Interpretability Testing of Text Mining Methods

Ashton, Triss A. 08 1900 (has links)
Extracting meaningful information from large collections of text data is problematic because of the sheer size of the database. However, automated analytic methods capable of processing such data have emerged. These methods, collectively called text mining first began to appear in 1988. A number of additional text mining methods quickly developed in independent research silos with each based on unique mathematical algorithms. How good each of these methods are at analyzing text is unclear. Method development typically evolves from some research silo centric requirement with the success of the method measured by a custom requirement-based metric. Results of the new method are then compared to another method that was similarly developed. The proposed research introduces an experimentally designed testing method to text mining that eliminates research silo bias and simultaneously evaluates methods from all of the major context-region text mining method families. The proposed research method follows a random block factorial design with two treatments consisting of three and five levels (RBF-35) with repeated measures. Contribution of the research is threefold. First, the users perceived a difference in the effectiveness of the various methods. Second, while still not clear, there are characteristics with in the text collection that affect the algorithms ability to extract meaningful results. Third, this research develops an experimental design process for testing the algorithms that is adaptable into other areas of software development and algorithm testing. This design eliminates the bias based practices historically employed by algorithm developers.
322

Att leva är att känna - en pilotstudie i affektfokuserad terapi för unga vuxna / Living is worth feeling - a pilot study of affect focused therapy for young adults

Berg, Anna, Enlöf, Magdalena January 2014 (has links)
No description available.
323

Comparing outcome measures derived from four research designs incorporating the retrospective pretest.

Nimon, Kim F. 08 1900 (has links)
Over the last 5 decades, the retrospective pretest has been used in behavioral science research to battle key threats to the internal validity of posttest-only control-group and pretest-posttest only designs. The purpose of this study was to compare outcome measures resulting from four research design implementations incorporating the retrospective pretest: (a) pre-post-then, (b) pre-post/then, (c) post-then, and (d) post/then. The study analyzed the interaction effect of pretest sensitization and post-intervention survey order on two subjective measures: (a) a control measure not related to the intervention and (b) an experimental measure consistent with the intervention. Validity of subjective measurement outcomes were assessed by correlating resulting to objective performance measurement outcomes. A Situational Leadership® II (SLII) training workshop served as the intervention. The Work Involvement Scale of the self version of the Survey of Management Practices Survey served as the subjective control measure. The Clarification of Goals and Objectives Scale of the self version of the Survey of Management Practices Survey served as the subjective experimental measure. The Effectiveness Scale of the self version of the Leader Behavior Analysis II® served as the objective performance measure. This study detected differences in measurement outcomes from SLII participant responses to an experimental and a control measure. In the case of the experimental measure, differences were found in the magnitude and direction of the validity coefficients. In the case of the control measure, differences were found in the magnitude of the treatment effect between groups. These differences indicate that, for this study, the pre-post-then design produced the most valid results for the experimental measure. For the control measure in this study, the pre-post/then design produced the most valid results. Across both measures, the post/then design produced the least valid results.
324

Réalisation de liaisons céramique-métal par brasage dans une cellule prototype d’électrolyse de la vapeur d’eau à haute température pour la production d’hydrogène / Ceramic to metal assemblies by brazing within a steam electrolysis prototype cell under pressure at high temperature for hydrogen production

Loricourt, Johan 19 April 2011 (has links)
L'électrolyse de la vapeur d'eau à haute température et sous pression avec des électrolytes à conduction protonique est un moyen envisagé pour produire massivement de l'hydrogène à un coût compétitif. Pour être fonctionnelle, une cellule d'électrolyse doit être hermétique vis-à-vis de l'extérieur et entre le compartiment anodique (O2 et H2O) et le compartiment cathodique (H2). Ainsi, la réalisation de liaisons céramique-métal est nécessaire, soit pour l'intégration de l'électrolyte (liaison perovskite-métal), soit pour l'intégration d'alimentations électriques (liaison alumine-métal). Compte-tenu des conditions de fonctionnement de la cellule (600°C, 50 bars, vapeur d'eau), seul un procédé de brasage est envisageable pour réaliser des jonctions résistantes mécaniquement et hermétiques. L'expertise des processus de corrosion sous vapeur d'eau a permis de définir la partie métallique et la brasure pour cette application et a montré que des alliages spécifiques étaient requis. L'étude de métallisation des céramiques par PVD pour permettre le mouillage de la brasure au moment du brasage a montré que la présence d'une barrière de diffusion était nécessaire, pour éviter la dissolution du dépôt lors du passage à l'état liquide de la brasure. Après une étude de mouillabilité à chaud de la brasure sélectionnée sur les céramiques métallisées et les substrats métalliques, les liaisons ont été optimisées en appliquant la méthodologie des plans d'expériences sur des éprouvettes normalisées. L'ensemble des résultats a ainsi conduit au développement de liaisons céramique-métal possédant de bonnes propriétés mécaniques (Rm = 60 MPa à 20°C) et hermétiques. / Steam electrolysis at high temperature and under pressure with protonic conduction electrolyte is a way to produce hydrogen massively at low cost. To operate, an electrolysis cell must be hermetic especially between the anodic compartment (O2 and H2O) and the cathodic one (H2). Thus, ceramic to metal assemblies are needed, either to insert the electrolyte (perovskite-metal junction) or to realize power supply (alumina-metal junction).Considering the operating conditions (873°K, 725 PSI, steam), only a brazing process is possible to realize strong and hermetic junctions.The evaluation of corrosion process under steam pressure has enabled to select a metallic component and a brazing alloy for this application, and has shown that specific alloys are needed.The studies of ceramics metallization by PVD to assure the brazing alloy wetting throughout the brazing process have shown that a barrier diffusion was necessary to avoid the dissolution of coatings when the brazing alloy become liquid.After wetting experimentations of the chosen brazing alloy over the metalized ceramics and the metallic substrate, ceramic to metal assemblies have been optimized in applying the experimental design methodology on standard samples (ASTM).The whole results have enabled to develop hermetic ceramic to metal assemblies having good mechanical properties (Rm = 8700 PSI at 300°K).
325

Integration of Simulation into Healthcare Education through Applied Constructivism: A Randomized, Switching Replications Experiment

Yoders, Samuel A. 01 January 2017 (has links)
This report describes the development, deployment, and analysis of an experimental instructional unit using applied constructivism instructional design (ID). The ID template was used to integrate a high-fidelity simulator into an undergraduate health care degree curriculum in a private, not-for-profit university. A switching-replications experimental design was used with random assignment of volunteer participants to initial treatment and control groups. Quantitative analysis of learning outcomes using standardized assessments was performed, including correlational analysis for knowledge transfer of simulator skills to clinical skills. Statistically significant positive effects were found for the educational outcomes of participants when measuring both the knowledge and application of heart anatomical structures and views for examination of the heart with ultrasound. Mild positive correlations were found between performance on the simulator and performance in an actual clinical setting, with limited predictive value between the two. The switching-replications experimental design helped to control for potentially strong social effects that could have endangered internal validity and to maximize the data available for analysis. Many of the constructivist-based ID features of the educational unit resulted in positive feedback and participation from participants. However, cautionary findings relating to the ID features included the need to carefully evaluate their use, as there was a tendency for participants to not value the performance of certain features if they were not going to be graded, despite their likely educational benefit. Future research suggested includes repetition across similar institutions with disparate student populations, and use of the educational unit ID template to implement simulation technology in other educational realms. Other possibilities include determining the effects on learning outcomes of a more-realistic user interface (UI) design and/or increased realism (difficulty) in the simulation itself. Related qualitative-based research could include structured interviews to determine participant satisfaction and learning outlooks, and investigation of the learners’ thoughts and perceptions as they use actual ultrasound machines after practicing on the simulator through think-aloud and active interview techniques.
326

Etude cinétique et optimisation multicritères du couplage déshydratation imprégnation par immersion : séchage convectif de la poire, la pomme et l'abricot / Kinetic investigation and multicriteria optimization of dehydration impregnation : by soaking combined to convective drying of pear, apple and apricot

Djendoubi Mrad, Nadia 20 December 2012 (has links)
Ce travail avait pour objectif l'étude de l'impact des deux procédés : la déshydratation imprégnation par immersion (DII) et le séchage convectif menés séparément ou combinés sur les transferts couplés d'eau et de saccharose et les principaux critères de qualité de fruit (écart de couleur, teneur en phénols totaux (PT), teneur en acide ascorbique (AA), retrait volumique, activité de l'eau) en prenant la poire Conférences comme modèle. L'effet des procédés sur les morceaux de poire a été appréhendé selon deux approches : (i) une étude globale de l'impact des variables de commandes sur la qualité du produit fini et (ii) une étude cinétique des composés d'intérêt nutritionnel et de la qualité (couleur, retrait, activité de l'eau).Un plan d'expériences composite centré à quatre facteurs et cinq niveaux a été établi (concentration en saccharose de la solution osmotique : 25-65%, température de DII : 20-60 °C, durée de la DII : 0,5-6,5 h, température du séchage convectif : 30-70 °C) pour étudier l'effet global des procédés sur le produit fini. En DII, les paramètres « °Brix, « durée » et « la température de la solution » ont un effet significatif (p < 0,01) sur les pertes en eau, le gain en soluté et les attributs de qualité de morceaux de poire. Les pertes en AA sont plus élevées que les pertes en PT et sont essentiellement dues à l'oxydation et à l'entraînement par l'eau. Durant le séchage convectif, les pertes en PT et en AA dépendent plus de la durée du procédé que de la température d'exposition. Elles atteignent respectivement 80% et 34% après 10 h de séchage à 30 °C. Le changement de couleur de morceaux de poire dépend de la durée et de la température de traitement et est plus prononcé en fin de séchage. Des modèles quadratiques prédictifs ont été proposés pour relier les variables de réponse (aw, différence de couleur, perte en PT et durée totale de traitement) aux paramètres opératoires des deux procédés étudiés. Cependant, la perte en AA décroit linéairement avec la durée de DII. Une optimisation multicritères en utilisant la méthodologie des surfaces de réponse (MSR) a été proposée (pertes minimales en PT et en AA, durée totale du traitement et différence de couleur réduites et une aw inférieure à 0,6) pour la combinaison DII/séchage. Les conditions optimales sont : solution osmotique à 28°C et 25°Brix, une durée de DII de 30 min et un séchage convectif à 60 °C. Par ailleurs, les effets de la température (30, 45 et 60 °C) et de l'imprégnation en saccharose par DII (10 et 65 min, 70°Brix, 30 °C) sur les isothermes de désorption et sur la température de transition vitreuse (Tg) de morceaux de poires, de pommes et d'abricots ont été déterminés. L'imprégnation en saccharose du tissu végétal atténue l'influence de la température sur sa capacité de sorption. Elle engendre un effet dépresseur de l'activité de l'eau et une augmentation de l'hygroscopicité de la poire, la pomme et l'abricot à température élevée. Les isothermes de désorption des abricots frais et enrichis en saccharose présentent un croisement des courbes marquant l'inversement de l'effet de la température sur les isothermes. La Tg dépend de la température, de la teneur en saccharose et de la teneur en eau des fruits. Pour une teneur en eau constante, l'augmentation de la température et la durée de DII se traduisent par l'augmentation de la Tg. Les digrammes de phase (Tg=f(X) et Tg=f(aw)) des fruits ont été établis à 30, 45 et 60°C et les teneurs en eau critiques ainsi que les activités d'eau critiques ont été déterminées. Une teneur en eau en fin de séchage inférieure ou égale à 0,02 g/g M.S. est recommandée pour l'obtention de morceaux de fruit stables aux niveaux microbiologique, physicochimique et rhéologique. / The aim of this work was the study of the impact of both drying processes: dehydration-impregnation by soaking (DIS) and convective drying performed separately or in combination on mass transfers of water and sucrose and on the main quality characteristics of the fruit (total difference of colour, total phenols (TP) and ascorbic acid (AA) contents, shrinking, water activity) by taking the pear Conference as a model. The processes effect on the pieces of pear was apprehended according two approaches: (i) a global study of the impact of the variables of commands on the quality of finished product and (ii) a kinetic study of nutritional compounds and the quality (colour, shrinkage, and water activity). Central Composite Design with four factors (sucrose concentration: 25-65 %, temperature: 20-60 °C, immersion time: 0.5-6.5 hr and drying temperature: 30-70 °C) at five levels each was used for pears processing. During DIS, the variables: immersion time, temperature and concentration of sucrose solution had a significant effect (p<0.01) in the loss of water, the solid gain and the quality attributes of pears. The losses in AA are higher than those in TP and are essentially due to the oxidation and the leaching with water. During the convective drying, the losses in TP and in AA depend more on the time of the process rather than the temperature of exposition. They reach respectively 80% and 34% after 10 h of drying at 30 °C. The color change of pear depends on the time and temperature of treatment and is more pronounced at the end of drying. Predictive and quadratic models were suggested to link the responses variables (aw, total colour difference, TP loss and total time treatment) to operational parameters of both studied processes. The losses in AA decrease linearly with the duration of DIS. A multicriteria optimization using response surface methodology (RSM) was proposed (minimal losses in TP and in AA, reduced total processing time and total difference in colour and an aw inferior to 0.6) for the combination DIS/convective drying. The optimal conditions are: osmotic solution at 28°C and 25°Brix, a DIS lasting 30 min and a convective drying at 60 °C. Otherwise, the temperature effects (30, 45 and 60 °C) and the sucrose impregnation by DIS (10 and 65 min, 70°Brix, 30 °C) upon the desorption isotherms and the transition temperature (Tg) of pears, apples and apricots were determined. The sucrose impregnation diminishes the influence of temperature on its sorption ability. It generates a depressing effect on water activity and a rise of pear hygroscopicity, apple and apricot at a high temperature. The desorption isotherms of fresh and sucrose impregnated apricot present a crossing of curves which mark the inverse of the effect of temperature on isotherms. The Tg depends on the temperature, the sucrose content and the fruit water content (X). For constant water content, the rise of temperature and of the duration de DIS result in the increase of Tg. The phase diagrams (Tg=f(X) et Tg=f(aw)) of fruits were established at 30, 45 and 60°C and the critical water content as well as the critical water activities were determined. Water content at the end of drying inferior or equal to 0.02 g/g d.b. is recommended to obtain stable fruit pieces at microbiological, physiochemical and rheological levels.
327

Desenvolvimento e validação da microextração líquido-líquido dispersiva com líquido iônico para determinação de omeprazol em plasma humano por cromatografia líquida de alta eficiência / Development and validation of an ionic liquid dispersive liquid-liquid microextration method for determination of omeprazole in human plasma by high performance liquid chromatography

Dias, Larissa Alves dos Reis 28 September 2018 (has links)
O OME é empregado no tratamento de curto e longo prazo em diferentes desordens gastrointestinais. É um inibidor da bomba de prótons, que atua seletivamente na enzima H+/K+ ATPase. É completamente metabolizado pelas enzimas do citocromo P450 gerando três metabólitos principais: HOME, OMES e OS. É utilizado no tratamento de refluxo gastroesofágico em pacientes que sofrem de obesidade e sobrepeso no período anterior e posterior à cirurgia bariátrica. Entretanto, a realização deste procedimento cirúrgico pode prejudicar a absorção de nutrientes e medicamentos. Assim, a determinação das concentrações plasmáticas do OME é de grande importância clínica para o ajuste de dose evitando-se o comprometimento do tratamento. Portanto, foram desenvolvidos e validados dois métodos para quantificação do OME e metabólitos em amostras de plasma: LLE, método padrão e OS-DLLME e avaliada a IL-DLLME como método alternativo de extração. O método padrão, LLE, foi desenvolvido para quantificação do OME e metabólitos em amostras de plasma por HPLC-UV. A análise foi feita em uma coluna cromatográfica Zorbax Eclipse XDB - C18 (25 cm x 4,6 mm, partículas de 5 ?m) (Agilent Technologies, Palo Alto, CA, EUA) e coluna de guarda Zorbax Eclipse XDB - C18 (12,5 mm x 4,6 mm, partículas de 5 ?m) e FM composta por ACN: água (30:70, v/v), na vazão de 1 mL/min, detecção em 302 nm. Nestas condições foi possível a separação do OME e metabólitos em menos de 20 minutos. O método apresentou-se linear no intervalo de concentração plasmática de 20- 1000 ng/mL (r>0,99). Os parâmetros de precisão, exatidão, efeito carry-over e estabilidade estão em conformidade com o guia de validação da ANVISA (2012). O método foi satisfatoriamente aplicado em amostras de plasma de 20 pacientes submetidos à cirurgia bariátrica, no período pré e pós-cirúrgico. Outros dois métodos foram avaliados utilizando a técnica de microextração em fase líquida (DLLME). O método de OS-DLLME foi desenvolvido e validado para quantificação do OME e metabólitos em amostras de plasma por LCMS/ MS. A análise foi realizada na mesma coluna cromatográfica descrita anteriormente com FM composta por ACN:tampão formiato de amônio 10 mM pH 8,5 (50:50, v/v) vazão de 0,4 mL/min. Foram monitorados os íons precursores do OME, HOME, OMES e PI. As amostras de plasma foram pré-tratadas com ISO e com sobrenadante foi desenvolvida a OS-DLLME. Os parâmetros da OS-DLLME (tipo e volume de solvente extrator e dispersor, pH, força iônica do meio, tempo de agitação, tempo de centrifugação, volume de diluição da amostra e volume de amostra) foram otimizados com o auxílio de um delineamento experimental Plackett Burmann seguido por um CCD. Ao final uma metodologia de superfície de resposta facilitou a determinação da condição ótima de extração utilizando a ferramenta desejabilidade (D) na qual as condições otimizadas foram: 400?L de plasma, 2,5 mL de solução tampão tetraborato de sódio 0,1 mM pH 9,5, 120 ?L de CHCl3, 500 ?L de ISO, 0% de NaCl, 5 minutos de centrifugação, sem agitação das amostras. Posteriormente, o método foi aplicado com sucesso para análise de amostras de plasma de 5 pacientes submetidos à cirurgia bariátrica, no período pré e pós-cirúrgico.A IL-DLLME foi avaliada como técnica de extração utilizando ILs como solventes extratores alternativos. A análise foi realizada na mesma coluna cromatográfica com fase móvel no modo eluição por gradiente composta por ACN:água: 0-10 min, 5:95; 10,0-15 min, 10:90; 15,01-40 min, 30:70, v/v, vazão de 1 mL/min e detecção em 302 nm. Foram avaliados três ILs comerciais e oito ILs sintetizados no laboratório (NPPNS). Foram avaliados os parâmetros da IL-DLLME: solvente dispersor, IL extrator, pH e composição da solução tampão. Também foi realizada a avaliação por RMN dos IL utilizados. Dentre os ILs comerciais foi selecionado o OMImPF6, e dentre os ILs sintetizados foi selecionado o C8PF6. Entretanto, não foi possível o desenvolvimento do método devido a escassa quantidade de IL comercial. Em relação aos ILs sintetizados foram observados problemas na síntese e purificação, como presença de interferentes que coeluiam juntamente com os analitos avaliados. Entretanto, apesar deste método não ter sido validado foi possível obter valores de recuperação, para ambos os IL selecionados, superiores a 40%. / OME is used in the short- and long-term treatment of different gastrointestinal disorders. It is a proton pump inhibitor, which selectively acts on the enzyme H + / K + ATPase. It is completely metabolized by the cytochrome P450 enzymes generating three main metabolites: HOME, OMES and OS. It is used in the treatment of gastroesophageal reflux in patients who are obese and overweight in the period before and after bariatric surgery. However, performing this surgical procedure may impair the absorption of nutrients and medications. Thus, the determination of plasma concentrations of OME is of great clinical importance for dose adjustment, avoiding compromised treatment. Thus, two methods were developed for the quantification of OME and metabolites in plasma samples: LLE, standard method and OS-DLLME and IL-DLLME as an alternative method of extraction. The standard method, LLE, was developed for quantification of OME and metabolites in plasma samples by HPLC-UV. The analysis was done on a Zorbax Eclipse XDB-C18 (25 cm x 4.6 mm, 5 ?m particles) (Agilent Technologies, Palo Alto, CA, USA) and Zorbax Eclipse XDB-C18 (12, 5 mm x 4.6 mm, 5 ?m particles) and mobile phase composed of ACN: water (30:70, v / v) at the flow rate of 1 mL / min, detection at 302 nm. Under these conditions it was possible to separate OME and metabolites in less than 20 minutes. The method was linear in the plasma concentration range of 20-1000 ng / mL (r> 0.99). The parameters of accuracy, accuracy, carry-over effect and stability are in accordance with ANVISA\'s validation guide (2012). The method was satisfactorily applied in plasma samples from 20 patients submitted to bariatric surgery in the pre- and post-surgery period. Two other methods were evaluated using the liquid phase microextraction technique (DLLME). The OS-DLLME method was developed and validated for quantification of OME and metabolites in plasma samples by LC-MS / MS. The analysis was performed in the same chromatographic column described above with mobile phase composed of ACN: 10 mM ammonium formate buffer pH 8.5 (50:50, v / v) flow rate of 0.4 mL / min. The precursor ions of OME, HOME, OMES and PI were monitored. Plasma samples were pre-treated with ISO and the supernatant was grown to OS-DLLME. The parameters of OS-DLLME (type and volume of solvent extractor and dispersant, pH, ionic strength of medium, agitation time, centrifugation time, sample dilution volume and sample volume) were optimized with the aid of an experimental design Plackett Burmann followed by a central composite outline. At the end, a response surface methodology facilitated the determination of the optimal extraction condition using the desirability tool (D) in which optimized conditions were: 400?L of plasma, 2.5 mL of buffer solution 0.1 mM sodium tetraborate pH 9,5, 120 ?L CHCl3, 500 ?l ISO, 0% NaCl, 5 minutes centrifugation, without sample shaking. Subsequently, the method was validated and successfully applied for analysis of plasma samples from 5 patients submitted to bariatric surgery in the pre and post-surgical period. IL-DLLME was evaluated as an extraction technique using ILs as alternative extractive solvents. The analysis was performed on the iv same mobile phase chromatographic column in the gradient elution mode composed of ACN: water: 0-10 min, 5:95; 10.0-15 min, 10:90; 15.01 - 40 min, 30:70, v/v, flow rate of 1 mL / min and detection at 302 nm. Three commercial ILs and eight ILs synthesized in the laboratory (NPPNS) were evaluated. The parameters of IL-DLLME were evaluated: dispersing solvent, IL extractor, pH and buffer composition. NMR evaluation of the ILs used was also performed. Among the commercial ILs, OMImPF6 was selected, and C8PF6 was selected among the ILs synthesized. However, the development of the method was not possible due to the small amount of commercial IL. Concerning ILs synthesized, problems were observed in the synthesis and purification, as presence of interfering factors that coeluted together with the analyzed analytes. Thus, although this method was not validated, it was possible to obtain recovery values, for both ILs selected, higher than 40%.
328

Process parameter optimisation of steel components laser forming using a Taguchi design of experiments approach

Sobetwa, Siyasanga January 2017 (has links)
A research report submitted to the Faculty of Engineering and the Built Environment, University of the Witwatersrand, Johannesburg, in partial fulfilment of the requirements for the degree of Master of Science in Engineering. Date: September 2017, Johannesburg / The focus in this research investigation is to investigate the Process Parameter Optimisation in Laser Beam Forming (LBF) process using the 4.4 kW Nd: YAG laser system – Rofin DY 044 to form 200 x 50 x 3 mm3 mild steel - AISI 1008 samples. The laser power P, beam diameter B, scan velocity V, number of scans N, and cooling flow C were the five input parameters of interest in the investigation because of their influence in the final formed product. Taguchi Design of Experiment (DoE) was used for the selection and combination of input parameters for LBF process. The investigation was done experimentally and computationally. Laser Beam Forming (LBF) input parameters were categorised to three different levels, low (L), medium (M), and high (H) laser forming (LBF) parameters to evaluate parameters that yield maximum bending and better surface finish/quality. The conclusion drawn from LBF process is that samples which are LBFormed using low parameter settings had unnoticeable bending and good material surface finishing. On the other hand, samples LBFormed using medium parameters yielded visible bending and non-smooth surface finishing, while samples processed using high LBF parameters yielded maximum bending and more surface roughness than the other two process parameters. / MT2018
329

Otimização da liberação de difosfato de primaquina em comprimidos de liberação controlada / Optimization of controlled release primaquine diphosphate tablets

Duque, Marcelo Dutra 11 December 2009 (has links)
O presente trabalho teve como objetivo produzir comprimidos de liberação controlada de difosfato de primaquina baseados em polímeros hidrofílicos e otimizar a liberação do fármaco por meio do planejamento estatístico de mistura (DOE). Na seleção dos componentes da formulação foram realizados estudos de calorimetria exploratória diferencial (DSC) para verificar a compatibilidade entre o fármaco/excipientes e avaliação do fluxo dos pós das formulações por meio da determinação do ângulo de repouso. As 20 formulações obtidas no planejamento experimental continham misturas de hidroxipropilmetilcelulose de diferentes graus de viscosidade (K15M, K4M e K100LV) e polietilenoglicol 4000 como polímeros para controle da liberação. Os comprimidos de 30 mg de primaquina foram produzidos por compressão direta em máquina de punção simples de 9 mm e foram avaliados quanto à dureza, friabilidade, peso médio, teor do fármaco e dissolução. A cinética de liberação do fármaco foi estudada segundo os modelos de ordem zero, Higuchi e Korsmeyer-Peppas. Os ensaios de DSC permitiram verificar algum tipo de interação entre o fármaco e os excipientes lactose e estearato de magnésio. Os pós das formulações demonstraram boas propriedades de fluxo de acordo com os valores de ângulo de repouso. Os dados de regressão obtidos pelos modelos matemáticos aplicados com o DOE não permitiram verificar se a mistura de polímeros influenciou no ângulo de repouso dos pós e nas características físicas como dureza, friabilidade e peso médio dos comprimidos. No entanto, foi observada influência significativa da composição polimérica na dissolução dos comprimidos nos intervalos de 2, 4, 6 e 8 horas de ensaio. A partir desses dados e dos gráficos de superfície de resposta gerados pelo programa Design Expert® 6.0, foi possível otimizar as formulações restringindo a quantidade de cada polímero de forma a obter uma formulação com mecanismo de liberação duplo, por difusão e relaxamento das cadeias de polímero. O transporte anômalo foi o mecanismo de liberação de fármaco apresentado pela maioria das formulações, inclusive da formulação otimizada. / The objective of the present work was to produce primaquine diphosphate controlled release tablets based on hydrophilic polymers and use the mixture statistical experimental design (DOE) to optimize drug release. In selecting the components of the formulations, differential scanning calorimetry (DSC) were carried out to verify the compatibility between drug/excipients and evaluating flow properties of the powders by determining the angle of repose. The 20 formulations obtained in the experimental design contained mixtures of hydroxylpropylmethylcellulose of different degrees of viscosity (K15M, K4M and K100LV) and polyethylene glycol 4000 as polymers to control drug release. Tablets containing 30 mg of primaquine were produced by direct compression in a 9 mm single punch tablet press and were evaluated for hardness, friability, average weight, drug content and dissolution. The kinetics of drug release was studied applying Zero Order, Higuchi and Korsmeyer-Peppas models. DSC tests allowed verifying some kind of interaction between the drug and the excipients lactose and magnesium stearate. The values of angle of repose obtained demonstrated that the powders of the formulations presented good flow properties. The regression data obtained by the mathematical models failed to verify the influence of the mixture of polymers in the angle of repose of the powders and physical characteristics such as hardness, friability and average weight of the tablets. However, there was a significant influence of polymers composition in the dissolution of the tablets at intervals of 2, 4, 6 and 8 hours of testing. Most formulations showed anomalous transport as the mechanism of drug release. From these data and response surface plots generated by Design Expert® 6.0 software, it was possible to optimize the formulations by restricting the amount of each polymer to obtain a formulation with a double release mechanism, diffusion and relaxation of the hydrated matrix chains.
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Obtenção de cerveja usando banana como adjunto e aromatizante / Beer obtaining using banana as an adjunct and a flavouring agent

Carvalho, Giovani Brandão Mafra de 20 July 2009 (has links)
Nos últimos anos, duas tendências tem se destacado no universo cervejeiro: a obtenção de cervejas a partir de mostos concentrados e a elaboração de cervejas utilizando adjuntos especiais, os quais podem aromatizar ou não as mesmas. Visando um aumento da produtividade juntamente com uma menor necessidade de investimentos na capacidade produtiva, algumas cervejarias vêm optando pelo aumento do extrato inicial de fermentação para valores superiores aos tradicionais (10-15 0P). A elaboração de cervejas utilizando adjuntos especiais vem se tornando uma solução de barateamento na obtenção de cerveja devido à substituição de parte do malte, acrescentando ainda, atributos sensoriais característicos nos produtos obtidos. A banana constitui-se em matéria-prima bastante favorável à fermentação alcoólica por ser rica em carboidratos, minerais e apresentar baixa acidez. O principal objetivo desta pesquisa foi utilizar a banana como um adjunto do malte e como um aromatizante natural e sutil das cervejas obtidas. A quantificação dos carboidratos presentes na banana prata em diferentes graus de maturação revelou que a condição \"muito-madura\", apresentou o mais alto teor de carboidratos totais solúveis (15,65 %) e o mais baixo teor de amido (0,48 %). Após a etapa quantificação dos carboidratos fez-se um estudo da extração aquosa a quente dos sólidos solúveis da banana com a metodologia de superfície de resposta a partir de um planejamento fatorial 22 onde se obteve um modelo matemático empírico quadrático (Y = 5.58 + 1.25 X1 - 0.26 X2 - 0.37 X22). Os valores que otimizaram esta extração (Y) foram 38,5 g de purê de banana (X1) e tempo de extração de 39,7 minutos. Utilizando um planejamento fatorial 22 fez-se um estudo da fermentação do mosto com adjunto de banana, na planta piloto da microcervejaria da EEL - USP em diferentes concentrações e temperaturas. Observou-se que a 12 0P e a 15 0C obteve-se uma Qp de 0,58 g/L.h em 72 h de fermentação e apenas 6,07 % do açúcar metabolizado pela levedura cervejeira foi desviado para a geração de produtos secundários, garantindo um Yp/s real de 0,48 g/g. Dentro destas condições de estudo investigou-se o comportamento cinético da levedura cervejeira Saccharomyces cerevisiae 308 de baixa fermentação (tipo lager) nestes mostos com banana, de densidade tradicional. Pôde-se observar que o máximo valor de ?x (0,114 h-1) foi alcançado com a fermentação a 12 0P e 15 0C. O valores máximos de ?s e ?p (1,128 e 0,585 g/g.h, respectivamente) foram conseguidos com a fermentação a 15 0P e 15 0C. Em seguida, fez-se um estudo com o propósito de aumentar a produtividade volumétrica de etanol em mostos com banana de alta densidade. Para isto, realizou-se fermentações com a adição de diferentes nutrientes, em mini-bioreatores cilindrocônicos de 0,9 L da Uminho - Portugal. Verificou-se que apenas a adição de MgSO4 foi significativa estatisticamente para o aumento da Qp. Observou-se também que o melhor valor de Qp (0,68 g.L/h) foi alcançado em 64 h de fermentação após suplementação com 420 mg/L de MgSO4. Em seguida, fez-se a caracterização físicoquímica da cerveja obtida com a reprodução do experimento otimizado em mini-bioreator cilindrocônico de 0,9 L da Uminho - Portugal no fermentador de 180 L da EEL - USP, verificando-se que a cerveja com banana de 4,8 % v/v apresentou uma elevada concentração de potássio (600,68 mg/L) e de acetato de isoamila (1,20 mg/L). Das cervejas otimizadas elaboradas na planta piloto da USP, fez-se uma avaliação sensorial comparando-as com cervejas do mercado brasileiro. Observou-se que em relação aos testes de preferência, as cervejas com banana foram estatisticamente preferidas em relação às amostras do mercado. Já os testes de aceitação demonstraram que não houve diferença significativa (p >= 0,05) quanto ao grau de aceitação entre os produtos correspondentes às amostras experimentais otimizadas e as amostras do mercado. Ou seja, as amostras de cerveja com banana foram tão aceitas pelo consumidor quanto às amostras de cerveja do mercado. Por fim foi realizado um estudo econômico preliminar, dentro de uma estimativa de produção de 875 L/mês de cerveja com banana em microcervejaria. Verificou-se que o custo inicial do processo foi 204,76 % superior a de uma cerveja comercial. Todavia, o custo direto variável de produção desta cerveja foi de R$ 0,94/L contra R$ 1,10/L de uma cerveja puro malte produzida nas mesmas condições de processo. / In the past years, two tendencies have been revealed in the universe of brewing: beer production using concentrated wort and its elaboration using special adjunct, which might supply or not a special flavour to the beer. Aiming to increase the process productivity along with decreasing the necessity of further production investments, some breweries have adapted to increase the initial fermentation extract concentration to values superior to the traditional ones (10-15 oP). The elaboration of beer using special adjunct is considered a solution to turn cheap beer production by not only by substituting part of the malt but also in adding characteristic sensorial attributes in the obtained products. Banana is constituted of raw materials suitable for alcoholic fermentation for being rich in carbohydrates and minerals and present law acidity. The principal objective of this research is to utilize the banana as an adjunct for malt and also as a natural and a tenuous flavouring agent for the obtained beer. The quantification of the carbohydrates present in the banana prata in different maturation grade, has revealed that the condition of \"very mature\" represented the highest content in total soluble carbohydrates (15.65%) and the lowest content in starch (0.48%). After the quantification stage of the carbohydrates, a study was done on the hot aqueous extraction of the soluble solids found in the banana using the response-surface method obtained by a complete 22 factorial design. The obtained mathematical empirical quadratic model was (Y = 5.58 + 1.25 X1 - 0.26 X2 - 0.37 X22). The values of the optimized extraction (Y) was 38.5 g of banana pulp (X1) and an extraction time of 39.7 minutes. It was done a study on the fermentation wort with banana adjunct using a factorial design 22, in the micro-brewery pilot plant located in the EEL - USP, at different concentrations and process temperatures. It was observed that at 12 0P and at 15 0C, it was obtained a Qp of 0.58 g/L.h in 72 h of fermentation and only 6.07 % of the sugar metabolized by the alcoholic-yeast was deviated for the production of secondary products, which guaranteed a real Yp/s of 0.48 g/g. Using these conditions in study, it was investigated the kinetic behavior of the alcoholic-yeast Saccharomyces cerevisiae 308 of law fermentation (lager type) in these wort using banana, of conventional gravity. It can be observed that the maximum value of ?x (0.114 h-1) was achieved with fermentation at 12 0P and 150C. The maximum values of ?s and ?p (1.128 e 0.585 g/g.h, respectively) was obtained at fermentation of 15 0P and 15 0C. It was also done studies with the objective of increasing the volumetric productivity of ethanol in worts with banana at high gravity. For this reason, it was done several fermentations with the addition of different nutrients, in mini-bioreactors cylindrical-conical de 0.9 L from UMinho-Portugal. It was verified that the addition of MgSO4 was statistically significant for the increase in Qp. It was also verified that the best value of Qp (0.68 g.L/h) was achieved in 64 h of fermentation after being supplemented with 420 mg/L of MgSO4. It was also done a physical-chemical characterization of the beer obtained from the reproduction of the optimized experiment obtained using the cylindrical-conical bioreactor de 0.9 L from UMinho- Portugal in the bioreactor of 180 L of working volume located in the EEL - USP, verifying that the beer with banana (4.8 % v/v) have presented a high concentrations of potassium (600.68 mg/L) and isomile acetate (1.20 mg/L). It was done a sensorial evaluation of the elaborated beer in the pilot-plant in the USP, comparing it with the other beers found in the Brazilian market. It was observed that in relation to the preference test, beers with banana were statistically preferred in relation to the other samples. Acceptance tests demonstrated that there has been no significant difference (p>= 0.05) in relation to the grade of acceptance between the products corresponding to the samples taken from the optimized experiments and the samples taken from the market. In other words, the samples with banana were acceptable by the consumer as much as the samples taken from common beers found in the market. Finally, it was done a preliminary economical evaluation of the process, considering as production capacity the value of 875 L/month of beer with banana. It was calculated the initial cost of the process was of 204.76% superior than the commercial draft beer. On the other hand, the direct cost of production of this draft beer was of R$ 0.94/L against R$ 1.10/L of draft beer made from pure malt using the same process conditions.

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