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Determina??o da energia de ativa??o e pureza de medicamentos de refer?ncia, gen?rico e similar utilizando t?cnicas termoanal?ticasPaula, Sueilha Ferreira de Andrade de 28 August 2014 (has links)
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Previous issue date: 2014-08-28 / Neste trabalho, os medicamentos de refer?ncia, gen?rico e similar com os princ?pios ativos ?cido Acetil Salic?lico, Paracetamol, captopril, hidroclorotiazida e mebendazol foram adquiridos em farm?cias locais e estudados por Termogravimetria (TG) e Calorimetria Explorat?ria Diferencial (DSC). A decomposi??o t?rmica foi avaliada objetivando obter a partir do M?todo de Ozawa a energia de ativa??o, em atmosfera inerte (de nitrog?nio), utilizando tr?s raz?es de aquecimento distintas (5, 10 e 20 oC min-1). A formula??o farmac?utica do AAS de refer?ncia foi o ?nico que apresentou perfil termogravim?trico diferente dos demais (gen?rico e similar) indicando, provavelmente intera??o entre os excipientes e o princ?pio ativo. Foi observado no gr?fico do log da raz?o de aquecimento pelo inverso da temperatura que n?o houve linearidade dos dados, isto ?, n?o houve correla??o entre os percentuais de perda de massa e a energia de ativa??o envolvida na decomposi??o t?rmica da formula??o farmac?utica do AAS de refer?ncia. A an?lise por calorimetria explorat?ria diferencial foi realizada em atmosfera de nitrog?nio, com raz?o de aquecimento de 10?C min-1. Na an?lise destes mesmos medicamentos, os dados das curvas encontradas sobre o ponto de fus?o foram, exceto para a hidroclorotiazida, s?o condizentes com a literatura. A hidroclorotiazida apresentou um ponto de fus?o bastante inferior ao encontrado na literatura, o que pode ser justificado devido ? intera??o do princ?pio ativo com o excipiente lactose. No estudo da pureza, utilizando a equa??o de Van?t Hoff , os medicamentos de hidroclorotiazida de refer?ncia e mebendazol de refer?ncia, gen?rico e similar apresentaram teor de impureza acima do limite estabelecido nesta equa??o que deve ser superior a 2,5 % mol. / In this work, the reference drugs, generic and similar to the active ingredients acetylsalicylic
acid, paracetamol, captopril, hydrochlorothiazide and mebendazole were purchased from local
pharmacies and studied by thermogravimetry (TG) and Differential Scanning Calorimetry
(DSC). Thermal decomposition was assessed to obtain from the Ozawa method the activation
energy in inert atmosphere (nitrogen), using three different heating ratios (5, 10 and 20 o
C
min-1). The pharmaceutical formulation of the AAS reference was the one who presented
different from the others (generic and similar) Thermogravimetric profile indicating likely
interaction between the active ingredient and excipients. Was observed at the heating rate of
the inverse temperature that no linearity of the data, ie, there was no correlation between the
percentage of mass loss and the activation energy involved in the thermal decomposition of
the pharmaceutical formulation of the AAS reference log graph. The analysis by differential
scanning calorimetry was performed in nitrogen atmosphere with a heating rate of 10 ? C
min-1. In the analysis of these same drugs, the data curves found on the melting point were,
except for hydrochlorothiazide, are consistent with the literature. Hydrochlorothiazide
presented a melting point well below that found in the literature, which may be justified due
to the interaction of the active ingredient with the excipient lactose. In the study of purity,
using the Van't Hoff equation, the reference drugs hydrochlorothiazide and mebendazole
reference generic and showed similar impurity content below the limit established that this
equation must be greater than 2.5 mol%
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Avalia??o da estabilidade t?rmica e oxidativa dos biodieseis de algod?o, girassol, dend? e sebo bovinoSantos, Anne Gabriella Dias 26 February 2010 (has links)
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Previous issue date: 2010-02-26 / The search for new sources of environmentally friendly energy is growing every day. Among these alternative energies, biodiesel is a biofuel that has had prominence in world production. In Brazil, law 11.097, determine that all diesel sold in the country must be made by mixing diesel/biodiesel. The latter called BX, , where X represents the percent volume of biodiesel in the diesel oil, as specified by the ANP. In order to guarantee the quality of biodiesel and its mixtures, the main properties which should be controlled are the thermal and oxidative stability. These properties depend mainly of the chemical composition on the raw materials used to prepare the biodiesel. This dissertation aims to study the overall thermal and oxidative stability of biodiesel derived from cotton seed oil, sunflower oil, palm oil and beef tallow, as well as analyze the properties of the blends made from mineral oil and biodiesel in proportion B10. The main physical-chemical properties of oils and animal fat, their respective B100 and blends were determined. The samples were characterized by infrared and gas chromatography (GC). The study of thermal and oxidative stability were performed by thermogravimetry (TG), pressure differential scanning calorimeter (PDSC) and Rancimat. The obtained biodiesel samples are within the specifications established by ANP Resolution number 7/2008. In addition, all the blends and mineral diesel analyzed presented in conformed withthe ANP Regularion specifications number 15/2006. The obtained results from TG curves data indicated that the cotton biodiesel is the more stable combustible. In the kinetic study, we
obtained the following order of apparent activation energy for the samples: biodiesel from palm oil > sunflower biodiesel > tallow biodiesel > cotton biodiesel. In terms of the oxidative
stability, the two methods studied showed that biodiesel from palm oil is more stable then the tallow. Within the B100 samples studied only the latter were tound to be within the standard
required by ANP resolution N? 7. Testing was carried out according to the EN14112. This higher stability its chemical composition / A busca por novas fontes de energia, que sejam ecologicamente corretas, cresce a cada dia. Dentre essas energias alternativas, o biodiesel ? um dos biocombust?veis que vem tendo destaque na produ??o mundial. No Brasil, a Lei n? 11.097, determina que todo diesel vendido no pa?s, deve ser constitu?do pela mistura de ?leo diesel/biodiesel, denominado BX, onde X representa o percentual em volume de biodiesel no ?leo diesel, conforme especifica??o da Ag?ncia Nacional do Petr?leo (ANP). Entre as principais propriedades que devem ser
controladas para garantir a qualidade do biodiesel est?o as estabilidades t?rmica e oxidativa, as quais dependem, basicamente, da composi??o da mat?ria prima utilizada. Este trabalho tem como objetivo estudar a estabilidade t?rmica e oxidativa de biodieseis provenientes dos ?leos de algod?o, girassol, dend? e do sebo bovino, assim como analisar as propriedades das blendas feitas do ?leo mineral com biodiesel, na propor??o B10. Foram determinadas as principais propriedades f?sico-qu?micas dos ?leos vegetais e gordura animal, das respectivas amostras de B100 e suas misturas, al?m de caracteriza??es atrav?s de infravermelho e cromatografia a g?s. O estudo das estabilidades t?rmica e oxidativa foram realizados atrav?s de Termogravimetria (TG), Calorimetria Explorat?ria Diferencial sob Press?o (PDSC) e Rancimat. As amostras de biodiesel obtidas est?o dentro das especifica??es estabelecidas pela Resolu??o da ANP No7/2008. As misturas analisadas e o diesel mineral apresentaram todos os
resultados em conformidade com as especifica??es da Portaria da ANP N?15/2006. Os resultados obtidos via TG apontam o biodiesel de algod?o como o mais est?vel. No estudo cin?tico, obteve-se a seguinte ordem de energia de ativa??o aparente: biodiesel de dend? > biodiesel de girassol > biodiesel de sebo > biodiesel de algod?o. Em rela??o ? estabilidade oxidativa os resultados obtidos via PDSC e Rancimat indicaram que o biodiesel de dend? foi o mais est?vel, e em seguida o de sebo. Dentre os B100 estudados, o de dend? e sebo bovino, se encontraram dentro dos padr?es exigidos na Resolu??o ANP N?7 (tempo de indu??o 6h), os ensaios foram realizados de acordo com a norma Europ?ia EN14112, a temperatura de 110?C. A maior estabilidade do biodiesel de dend? pode ser atribu?do ? sua composi??o qu?mica
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