The current work aims to establish a novel and advanced reverse phase isocratic liquid chromatography system followed by validation and to conduct stability analysis in active pharmaceutical ingredients and formulations for the quantification of Solifenacin Succinate. The optimized elution was achieved with column Sunfire C8 (4.6 x 150mm, 5µm), using the mobile phase of Buffer: Methanol: Acetonitrile in the composition ratio of 45:45:10 v/v. The wavelength of detection was selected as 220nm with 1.0ml/ min flow rate and 30μl injection volume. The retention time of Solifenacin Succinate was found 2.94 min respectively. The method developed has been validated for various analytical parameters according to ICH guidelines. The Linearity was attained at 20 to100 μg/ml of concentration range. The established method was proved as reproducible. The Assay was obtained as 100.40%. The degradation studies were carried out at all degradative conditions and the results of degradation studies denote that the current method was specific, reliable, and economical. Hence, the developed method can be applied for the qualitative and quantitative determination of the selected drug and its commercial formulations.
A simple, effective and reliable UV photolysis digestion (UVPD) method has been developed for the determination of fluoride in pharmaceuticals containing fluorine as one of the constituents. It is based on the use of high intensity UV-irradiation in the presence of a mixture of HNO 3 and methanol. For the optimization of the UVPD procedure, three bulk drug samples namely levofloxacin, nebivolol and efavirenz, were chosen as representatives of three diverse matrices: containing single fluorine, two fluorine atoms and trifluoromethyl groups respectively. Optimization of the procedure involves an initial reaction with nitric acid followed by a UVPD approach for complete mineralization of the sample i.e., conversion of bound fluorine to free fluoride ion followed by determination by fluoride ionselective electrode (F-ISE) and spectrophotometry based methods. Parameters affecting the UVPD method, such as acid concentration, digestion time and sample weight, were optimized to obtain the quantitative recovery (>95%) of fluoride. Quantitative recovery of the fluorine in the samples could be achieved within 20-30 min of UV exposure time for a 50-mg sample. Total digestion of the drug samples was carried out by a closed microwave digestion system and the recoveries of the fluoride were found to be low (<70%) demonstrating the capabilities of the UVPD procedure. The proposed UVPD method was successfully applied to various commercially available fluorine containing drug samples.
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