101 resultados para Method of analysis
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Introduction: Alkalinization potential is a fundamental property of endodontic epoxy-based cements containing calcium hydroxide. Studies have shown discrepant pH results for same materials at different evaluation periods. A possible reason accounting for these differences may be the assessment procedures. Objective: To evaluate the pH value of an epoxy-based cement (Sealer 26) in different periods of analysis, using two assessment methods. Material and methods: Sealer 26 was manipulated and immediately placed into polyethylene tubes (n=10, each group) and immersed in distilled water. In G1, the tubes were kept in the same water during all experiment; and in G2, the tubes were removed and placed into another flask with an equal amount of water after the pH evaluation. The pH of these solutions was measured at 24 hours, 7, 14 and 28 days. Analysis were made within the same group according to the experimental periods and between groups in each experimental period. Data were submitted to ANOVA (α = 5%) and t test, respectively. Results: For G1 and G2, all periods showed different pH values (p < 0.05), except between 14 and 28 days (p > 0.05) and between 7 and 14 days (p > 0.05), respectively. In each period, no significant differences were observed between the groups. Conclusion: The method to obtain the pH values in different experimental periods no interfered in the final results. However, difference was observed when the results were analyzed at same group.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Darunavir (DRV) is a protease inhibitor used in the treatment of HIV infection, which constitutes a keystone in the therapy of patients infected with this virus. There is no monograph described in official compendia. The literature provides few methods of analysis for the determination of DRV in pharmaceuticals which include TLC, IR, UPLC, HPLC, HPLC-MS, HPLC-MS/MS, but there are no reports of the use of capillary electrophoresis (CE) for the determination of this drug. Thus, this research proposed the development and validation of a CE method for the determination of DRV in tablets. The method was completely validated according to the International Conference on Harmonization guidelines, showing linearity, selectivity, precision, accuracy and robustness. The migration was achieved in less than 1 minute using fused-silica uncoated capillary with an id of 50 μm and total length of 21 cm and voltage of +20 kV. The sample injection was performed in the hydrodynamic mode. The method was linear over the concentration range of 50-200 μg mL-1 with correlation coefficient 0.9998 and limits of detection and quantification of 7.29 and 22.09 μg mL-1, respectively. The drug was subjected to acid, base, oxidation and photolysis degradation. Degradation products were found interfering with the assay of DRV, therefore the method can be regarded as stability indicating. The validated method is useful and appropriate for the routine quality control of DRV in tablets.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)