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No. of bitstreams: 2 license_rdf: 23148 bytes, checksum: 9da0b6dfac957114c6a7714714b86306 (MD5) Dissertação - Rodrigo Gomes de Alencar - 2014.pdf: 13066901 bytes, checksum: 15e26e7a3dde863c6267ef54f83385be (MD5) Previous issue date: 2014-04-25 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / Ketoprofen is a nonsteroidal anti-inflammatory drug used for the treatment of mild to moderate pain in chronic inflammatory conditions. Due to its superior potency ketoprofen can be used in the treatment of inflammatory bowel disease (IBD). The treatment of IBD becomes safer and more effective when the drug is incorporated into colon-specific drug delivery systems. Pellets are multiparticulate solid dosage forms extensively investigated as colon-specific drug delivery systems. Pellets can be introduced into capsules or compressed into tablets. The industrial production of tablets containing pellets has several advantages when compared to the production of capsules. However, the compression of the pellets should not affect the release of the drug and the tablets should quickly disintegrate following administration. Therefore, the aim of this study was to develop tablets containing ketoprofen coated pellets for colon-specific drug release. For this, pellets were produced by extrusion and spheronization technique containing 40% (w / w) ketoprofen. Ketoprofen pellets obtained were coated with two different pH - dependent polymers derived from methacrylic acid (Opadry ® k 94 or Eudragit ® FS 30D) with weight gains of 10 or 20% (w / w). The coated pellets were then compressed under different pellets’ amounts and different compression forces. An extra- granular mixture of lactose and microcrystalline cellulose was used as compression aid. The in vitro release of ketoprofen from the systems obtained was evaluated in Bio Dis ® apparatus. The morphological and physical properties of pellets and tablets were assessed. The Eudragit ® FS 30 D coated pellets with weight gains of 10 or 20% showed higher efficiency of colon-specific delivery (94 %), however, the drug was released slowly and incompletely in conditions mimicking the pH of the colonic region. After compression of the pellets, the efficiency of colon – specific drug delivery was lowered after compression (between 20% and 61%, depending on the formulation). The lowest decrease of colon specific efficiency was observed in formulations containing lower amount of pellets, which also produced disintegrating matrices with potential for use in the topical treatment of IBD. / O cetoprofeno é um antiinflamatório não esteroidal usado para o tratamento de dores leves a moderadas, em condições inflamatórias crônicas. Devido a sua elevada potência antiinflamatória, o cetoprofeno pode ser aproveitado no tratamento das doenças inflamatórias intestinais (DII). O tratamento das DII se torna mais seguro e eficaz quando o fármaco é incorporado em sistemas de liberação cólon-específica. Pellets são formas farmacêuticas multiparticuladas bastante investigadas como sistemas de liberação cólon-específica. Após sua produção, os pellets podem ser inseridos em cápsulas ou comprimidos. A produção industrial de comprimidos contendo pellets apresenta inúmeras vantagens quando comparada ao processo de enchimento de cápsulas. No entanto, a compressão dos pellets não deve afetar as características de liberação do fármaco e os comprimidos formados devem se desintegrar rapidamente. Dessa forma, o objetivo deste trabalho foi desenvolver comprimidos contendo pellets revestidos para liberação cólon-específica de cetoprofeno. Para tanto, foram produzidos pellets contendo 40% (p/p) de cetoprofeno e celulose microcristalina pela técnica de extrusão e esferonização. Os pellets de cetoprofeno obtidos foram revestidos com dois diferentes polímeros pH-dependentes, ambos derivados do ácido metacrílico (Opadry ® 94 k ou Eudragit ® FS 30) com ganhos de massa 10 ou 20% (p/p). Os pellets revestidos foram então comprimidos com diferentes cargas de pellets e submetidos a diferentes forças de compressão, utilizando como adjuvante extra-pellets uma mistura granulada de lactose e celulose microcristalina. A liberação in vitro do cetoprofeno a partir das formas farmacêuticas obtidas foi avaliada em dissolutor Bio Dis aparato III. As caracterizações morfológicas e físicas dos pellets e comprimidos foram conduzidas. Os pellets obtidos por revestimento com Eudragit ® FS 30 D, com ganhos de massa de 10 ou 20%, mostraram elevada eficiência de liberação cólon-específica in vitro (até 94%), no entanto, o fármaco foi liberado de forma lenta e incompleta em meio com pH similar ao encontrado na região colônica. Após a compressão dos pellets, os valores de eficiência de liberação cólon-específica sofreram reduções entre 20% e 61%. A menor diminuição da eficiência de liberação cólon-específica foi observada nas formulações contendo a menor carga de pellets, as quais deram origem à matrizes desintegráveis com potencial para utilização no tratamento tópico das DII.

A importância das restaurações provisórias no tratamento reabilitador oral é inquestionável. Os materiais utilizados para a execução destas restaurações, entretanto, são críticos com relação à resistência e longevidade, principalmente, quando estas são executadas em tratamentos prolongados e/ou em espaços desdentados extensos. A proposta deste trabalho foi determinar o efeito de diversos reforços sobre a resistência flexional, o módulo de elasticidade e o tipo de fratura apresentados por espécimes confeccionados em uma resina poli(metilmetacrilato) (PMMA), quando submetidos a um teste de carga de três pontos. Sete tipos de reforços constituíram os grupos experimentais com dez espécimes cada: um fio de aço com 0,7 mm de diâmetro; um fio de amarrilho trançado; uma fibra de vidro trançada Interlig® (Angelus®); uma fibra de vidro entrelaçada Splint-It!® (Jeneric-ron®); uma fibra de vidro unidirecional Fibrante® (Angelus®); uma fibra de poli(etileno) Connect® (Kerr®) e uma fibra cerâmica flexível GlasSpan® (GlasSpan®). O grupo controle, também com dez amostras, foi composto de espécimes não reforçados. A confecção dos espécimes, o ensaio mecânico e cálculo da resistência flexional e do módulo de elasticidade foram realizados seguindo norma ISO 10477 – modificada. A análise dos resultados (ANOVA, p < 0,05), para ambas as propriedades, mostrou haver diferença estatística entre os grupos. O teste de Tukey encontrou que os grupos reforçados com fio de aço com 0,7 mm; fibra Interlig® e fibra Connect® aumentaram significantemente a resistência flexional, e que os grupos reforçados com fio de aço com 0,7 mm; fibra Interlig®; fibra Splint-It!®; fibra Connect® e fibra GlasSpan®, aumentaram o módulo de elasticidade, em relação ao grupo controle. A análise das fraturas concorreu com a elaboração de um novo sistema de classificação dividindo-as em quatro tipos: Ausente, Parcial, Total Não Separada e Total Separada. As fraturas dos espécimes reforçados foram consideradas mais favoráveis ocorrendo, predominantemente, os tipos Ausente e Parcial. / Provisional restorations are essential components of oral rehabilitation treatment. The strength and durability features are, however, critical whe n long-term treatment is needed. The aim of this work was to measure the flexural strength, the elastic modulus and the type of fracture of poly (methyl methacrylate) (PMMA) resin specimens when submitted to a three-point-bend test. Seven types of reinforcements constituted the experimental groups with ten specimens each: a 0.7 mm of diameter wire; an orthodontic braided wire; a braided fiberglass Interlig® (Angelus®); an woven fiberglass Splint-It!® (Jeneric-Pentron®); a roving fiberglass Fibrante® (Angelus®); a braided poly(ethylene) fiber Connect® (Kerr®) and a flexible ceramic fiber GlasSpan® (GlasSpan®). The control group, also with ten samples, included not reinforced specimens. All specimens were made and test according to modified ISO specification No. 10477. The analysis of the results (ANOVA, p < 0.05), for both properties, showed significant differences between groups. Tukey\'s test detected higher figures for groups reinforced with wire of 0.7 mm of diameter wire; Interlig® and Connect® when flexural strength was concerned. Groups reinforced with a wire 0.7 mm of diameter; Interlig®; Splint-It!®; Connect® and GlasSpan®, increased the elastic modulus, when compared to the control group. The fractures analysis contributed with the elaboration of new index system dividing them in four types: Absent, Partial, Total Not Separated and Total Separated. It was observed that the reinforced specimens fractures were more favorable, occurring, predominantly, in the Absent and Partial types.

O presente trabalho verificou a alteração dimensional dos guias cirúrgicos confeccionados em resina acrílica para cirurgia ortognática quando submetidos à esterilização por meio de plasma de peróxido de hidrogênio. Foram utilizados 15 corpos de prova confeccionados em resina acrílica quimicamente ativada a partir de moldes metálicos em três espessuras: 1,5 mm, 3,0 mm e 5,0 mm, em um total de 45. A imagem de cada corpo de prova foi digitalizada antes e após o processo de esterilização e processada pelo programa Photoshop® CS2. Foi realizada a vetorização das imagens pelo programa Corel Trace ® 12 para mensuração pelo programa Corel Drawn ® 12. Os resultados foram submetidos ao teste estatístico dos postos sinalizados de Wilcoxon, ao nível de significância de 0,05%. Os resultados obtidos foram que nos corpos de prova de 1,5 mm de espessura não houve diferença estatisticamente significante entre as mensurações realizadas antes e após o processo de esterilização (P>0,05), porem, nas espessuras de 3,0 mm e 5,0 mm houve pelo menos uma das medidas estatisticamente diferentes (p=0,011 e p=0,017, respectivamente). Fato este que nos levou a acreditar que o processo de esterilização não leva a alteração dimensional, porem em volumes maiores provavelmente houve uma contração de polimerização diretamente proporcional. / Dimensional alterations in surgical splints made of acrylic resin used in orthognathic surgery were evaluated after hydrogen peroxide gas plasma sterilization. Fifteen specimens of resin acrylic was made by a metal model master with three different thickness: 1,5 mm, 3,0 mm and 5,0 mm, totally 45 specimens. Specimens digital image was acquired before and after sterilization and process by Photoshop® CD2 software. The images were transformed in vector form by Corel Trace® 12 software. The measures were performed by Corel Draw® 12 software. The results were submitted to Wilcoxon statistic method, 0.05 level of confidence. The results showed no statistical differences in 1.5 mm specimens (p0,307) before and after sterilization process but, in 3.0 and 5.0 mm, there was at least one measure statistically different (p=0,011 and p=0,017, respectively). It was possible to conclude that the sterilization process did not lead to dimensional alteration but, in higher thickness probably had happen a proportional polymerization contraction.

O propósito desse trabalho foi o de produzir lentes biconvexas pelo processo de injeção para serem utilizadas no ensino de óptica geométrica e de ciências nos níveis fundamental e médio. A importância de tal trabalho se justifica na carência de material experimental didático produzido no mercado nacional. Para atingir os objetivos propostos, foi necessário estudar o processo de injeção de termoplásticos e adequá-lo à produção de um componente óptico. No desenvolvimento do trabalho, foi projetado e confeccionado um molde para injeção das lentes, segundo especificações técnicas e apoiado em resultados obtidos através de simulações numéricas. Após a realização de testes de injeção, seguiu-se a caracterização das lentes obtidas através de parâmetros ópticos: transparência, birrefrigência, índice de refração, distância focal, raio de curvatura e FTM / The purpose of this work was the development and production of acrylic biconvex lens by injection process to be used in optical and science teaching at elementary and high schools. The importance of such work is based in the deficiency of experimental didactic material made in Brazil. In order to achieve the intended objective it was necessary to study the thermoplastic injection process and adapt it to the fabrication of an optical element. During the development of the work a mold was designed and constructed in according to technical specifications and based on results of numerical simulations. After the injection tests the lens were characterized by theirs optical parameters: transparency, birefringence, refraction index, focal distance, curvature radius and MFT

O objetivo principal deste trabalho foi a formação de um material que possa responder aos estímulos pH e elétrico na liberação controlada de fármaco. Assim, hidrogéis condutores foram obtidos pela combinação do hidrogel de ácido acrílico com o polímero condutor polipirrol. O polipirrol foi eletroquimicamente polimerizado no interior do hidrogel e o material obtido (AA-PPi) conservou a propriedade de intumescimento que é característico dos hidrogéis e a eletroatividade, dos polímeros condutores. Além disso, o grau de intumescimento variou com a força iônica e pH. A liberação da safranina pelo hidrogel de AA-PPi foi estudada combinando os estímulos de pH e potencial e o resultado mais interessante foi a obtenção do perfil cuja velocidade de liberação foi constante, indicando uma cinética de ordem zero. Liberação do tipo liga-desliga foi estudada com o intuito de verificar se o AA-PPi pode ser controlado por pH e/ou potencial elétrico. Foi observado que dependendo da combinação de pH e potencial, o hidrogel pode ser controlado, por variação de pH ou de potencial elétrico. Outro hidrogel sintetizado foi o do hidrogel de AA contendo o poli(3,4-etilenodioxitiofeno):poli(estireno sulfonado), este por sua vez foi polimerizado quimicamente. Porém os resultados preliminares indicaram incompatibilidade entre os dois polímeros / The aim of this work was to obtain a material that can respond to both pH and potential stimuli for drug release. Thus, eletroactive hydrogels were synthesized by the combination of the properties of acrylic acid hydrogels with the conducting polymer polypyrrole. The polypyrrole was electrochemically polymerized into the hydrogel (AA-PPi), and the material retained the swelling properties that is characteristic of hydrogels and electroactivity of conducting polymers. Furthermore, the degree of swelling varied with the ionic strength and pH. The safranin release by AA-PPi was mensured under the combination of pH and potential stimuli and the most interesting result was obtained from the linear profile indicating a zero-order kinetics. On-off release profile was studied in order to verify if the AA-PPi can be controled by pH and/or electric potential. Depending on the combination of pH or electrochemical potential, the hydrogel had pH or electrochemical control. Other hydrogel synthesized was from AA hydrogel containing poly(3,4- ethylenedioxythiophene):polystyrene sulfonate, this, in other hand, was chemically polymerized. However, preliminary results indicate incompatibility between the two polymers

The goal of this master's thesis was to develop a method for gas chromatography using the Controlled Evaporation Mixer (CEM) for gas mixture sampling. Gas mixture contained chemical substances formed during manufacturing of acrylic acid by two-step oxidation of propylene. The analyzed mixture composed of permanent gases, light hydrocarbons and compounds containing oxygen. During the method development several capillary columns with polar and nonpolar stationary phase were used. After selection of the most suitable column (SPB-1 Sulfur, Supelco, USA) the method was further optimized for the maximal possible separation efficiency. However, it was impossible to separate propane and propene on SPB-1 Sulfur column. These gases were possible to determine on TCD detector and separate on respective columns prior to the detector. For that purpose, the optimization of multiple-port valves switching inside the gas chromatograph was performed. The next step was calibration of gas chromatograph for a purpose of quantitative analysis of selected substances. The calibration solution containing solvent and an analyte was evaporated and diluted with nitrogen by CEM to obtain desired analyte concentration. Formaldehyde and propane had a very low response on detectors, acetaldehyde was undetectable in desired...

Différents phosphates ont été préparés et testés pour la déshydratation de l'acide lactique en phase gaz. La sélectivité en acide acrylique dépend fortement de la température de réaction mais peu du temps de contact. A 380°C, des valeurs de sélectivité allant de 19 à 50% ont été mesurées pour des phosphates alcalino-terreux qui sont stables sur au moins 24 h. Des mesures d'acido-basicité ont montré que ces phosphates contiennent une forte proportion de sites de même force faible. De plus, une corrélation entre la sélectivité en acide acrylique et le ratio molaire acide/base a été établie : elle atteint 50% pour un rapport proche de 1 et diminue lorsque ce ratio augmente. L'acide lactique étant thermiquement peu stable (fonction acide très réactive), nous nous sommes tournés vers la conversion du lactate d'éthyle pur. Les sélectivités en produits de déshydratation sont largement favorisées avec une sélectivité maximale de 87% à 15% de conversion. Cependant, les catalyseurs sont moins actifs et se désactivent fortement sur 24 h. La désactivation peut être inhibée par ajout d'eau dans la phase gaz. La caractérisation de surface a montré que les vitesses de réaction augmentent avec le rapport P/M et a révélé la présence d'une phase amorphe hydroxylée correspondant à des mono, dihydrogénophosphates ou des polyphosphates. Les groupements P-OH présents dans cette phase sont consommés ou modifiés en condition de réaction pour les deux réactifs suggérant qu'ils constituent des sites actifs. Enfin, le suivi DRIFT des TPD-NH3 a permis de proposer que des paires acide-base (M2+ et P-O-) sont dosées dans ce cas. Elles constitueraient le site d'adsorption de l'acide lactique conduisant ensuite à un mécanisme de déshydratation de type E2 / Various alkaline-earth phosphates were prepared and evaluated for gas phase dehydration of lactic acid. Selectivity to acrylic acid strongly depends on the reaction temperature but not on the contact time. At 380 °C, values ranging from 19 to 49% were measured for alkaline–earth phosphates catalysts that are stable for at least 24 h. Acid–base properties measurements revealed that such phosphates contain high proportion of acidic and basic sites with same weak strength. Furthermore, correlation between selectivity to acrylic acid and the acid–base balance was clearly established: it was 50% for balance close to 1 and decreased increasing this parameter. Because of poor thermal stability of lactic acid, we then focused on the ethyl lactate conversion. Selectivities in dehydration products were much higher with a maxima of 87% at 15% conversion. However, the catalysts were less active and stable. The deactivation can be inhibited adding water in the gas phase. Surface characterization of catalysts showed that catalytic activities are correlated with the P/M ratio and revealed the presence of an hydroxylated amorphous phase corresponding to mono / dihydrogenophosphates or polyphosphates. The P-OH species present in these phases are consumed or modified for both reactants suggesting that they are active sites. Finally, NH3-TPD measurements followed by DRIFT suggested that acid base pairs (M2+ and P-O-) are then probed. Such pairs would constitute the adsorption site of lactic acid which then dehydrate in acrylic acid by an E2 mechanism

A transmissão de dados e informação na fibra óptica vem aumentando nos últimos anos. O interesse para avaliar melhor a confiabilidade mecânica tomou-se uma necessidade, depois que uma fibra, de um cabo instalado, estava se partindo com muita facilidade. O foco principal deste trabalho foi voltado para estabelecer metodologias para avaliar o estado de degradação dos polímeros usados. Através destas técnicas, buscou-se encontrar parâmetros (E\', E\", tan &#948, Tg, etc.) que pudessem indicar o estado de degradação dos revestimentos. Diferentes técnicas foram empregadas para avaliar o revestimento das fibras tais como: calorimetria exploratória diferencial (DSC), diferencial fotocalorimetria (DPC), análise térmica dinâmico mecânico (DMTA) e espectroscopia na região do infravermelho (FIIR). A partir da técnica desenvolvida, DMTA, esta pode ser empregada para avaliar a confiabilidade mecânica de várias fibras comercias. As técnicas DMTA e FIIR mostraram ser muito promissoras, pois consegue-se, através delas, obter muitos dados a respeito das características dos polímeros. / The datas and information transmission in the optical fiber have been increasing in the last years. The interest to evaluate the mechanical reliability became necessary, after that a optical fiber, from a cable installed, was cracking very easily. The principal aim of this work was establishing methodologies to evaluate the polymer degradation state. Through of this techniques we search to find out parameters (E\', E\", tan &#948, Tg. etc) that could denote the degradation state of the coatings. Different techniques were utilized to evaluate the coating of the optical fibers such as: differential scanning calorimeter (DSC), differential photocalorimeter (DPC), dynamic mechanic thermal analyzer (DMTA) and infrared spectroscopy (FIIR). From the method development (DMTA), it was possible to evaluate the mechanical realiability of many commercial fibers. DMTA and FTIR techniques shown to be very promising to obtain very dates to respect of polymer characteristics.

Rugosidad superficial, acrílico dental, pulido dental, conchas de moluscos. Surface roughness, dental acrylic, dental polish, seashells. / Objetivo: Evaluar in vitro la rugosidad superficial de una pasta experimental de pulido para acrílico a base de conchas de moluscos. Materiales y métodos: Un total de 74 especímenes de acrílico fueron divididos en 2 grupos (n=37). Todos los especímenes fueron confeccionados con una matriz metálica (14x5x6 mm) y pulidos con una pasta experimental a base de Donax Obesulus y piedra pómez con un tamaño de partículas de 15µm, respectivamente para cada grupo. La rugosidad superficial inicial y final fue evaluada con un rugosímetro luego del pulido de los especímenes. Los datos fueron analizados mediante estadística descriptiva (media, mediana, desviación estándar y rango intercuartílico) e inferencial (Prueba de Wilcoxon pareada y Prueba de U de Mann Whitney) (p<0.05). Resultados: Los especímenes pulidos con piedra pómez mostraron mayores valores de rugosidad (0,45±0,12 µm); mientras que los especímenes que fueron pulidos con la pasta experimental tuvieron menores valores de rugosidad (0,50±0,07µm). Pese a ello, no se encontró diferencia estadísticamente significativa entre la rugosidad superficial de la pasta experimental y el grupo control (p = 0.309). Conclusiones: La pasta experimental a base de conchas de moluscos redujo los valores de rugosidad superficial en las superficies del acrílico dental. / Objective: To evaluate in vitro the surface roughness of an experimental polishing paste for acrylic based on seashells. Materials and methods: A total of 74 acrylic specimens were divided into 2 groups (n = 37). All specimens were made with a metal matrix (14x5x6 mm) and then polished with an experimental paste and pumice stone with a particle size of 15 µm, respectively for each group. Initial and final surface roughness was evaluated after polishing the specimens. The data were analyzed using descriptive (mean, median, standard deviation and interquartile range) and inferential statistics (Wilcoxon signed-rank test and Mann Whitney U test) (p<0.05). Results: Specimens polished with pumice had higher roughness values (0.16 ± 0.06 µm), whereas specimens polished with the seashell powder had lower values in their surface roughness (0.09 ± 0.03 µm). Despite this, no statistically significant difference was found between the surface roughness of the experimental paste and the control group (p = 0.309). Conclusions: The experimental paste made of seashells reduced the surface roughness values on dental acrylic surface. / Tesis

The diploma thesis deals with preparation of acrylic copolymers via emulsion polymerization technique. Two sets of copolymer samples were prepared within this thesis, n BA/MMA and 2-EHA/MMA copolymers. n-BA/MMA copolymer sample was used for investigation of effect of surfactant concentration as well as effect of addition of acrylic acid to the feed composition. During all the copolymerizations, conversion was observed via solids content evaluation as the reaction progressed. Copolymerization was lead under inert atmosphere at continuous stirring and 80 °C for 4 hours. Glass transition temperature of samples was determined with DSC and Vicat softening point was measured as well. Data acquired from measurements were compared with values calculated with Fox equation which was used for modelling molar ratio of monomers in initial feed.