RESUMO
Simple, sensitive, precise, and specific high-performance liquid chromategraphic (HPLC) and high-performance thin-layer chromatographic (HPTLC) methods for the determination of dolutegravir sodium in bulk drug and pharmaceutical dosage form were developed and validated. In the HPLC method, analysis of the drug was carried out on the ODS C18 column (150 × 4.6 mm, 5 µm particle size) using a mixture of acetonitrile: water (pH 7.5) in the ratio of 80:20 v/v as the mobile phase at the flow rate 1 mL/min at 260 nm. This method was found to be linear in the concentration range of 5-35 µg/mL. The peak for dolutegravir sodium was observed at 3.0 ± 0.1 minutes. In the HPTLC method, analysis was performed on aluminum-backed plates pre-coated with silica gel G60 F254 using methanol: chloroform: formic acid in the proportion of 8:2:0.5 v/v/v as the mobile phase. This solvent system was found to give compact spots for dolutegravir sodium with the Rf value 0.77 ± 0.01. Densitometric analysis of dolutegravir sodium was carried out in the absorbance mode at 265 nm. Linear regression analysis showed good linearity with respect to peak area in the concentration range of 200-900 ng/spot. The methods were validated for precision, limit of detection (LOD), limit of quantitation (LOQ), accuracy, and specificity. Statistical analysis showed that both of the methods are repeatable and specific for the estimation of the said drug. The methods can be used for routine quality control analysis of dolutegravir sodium.
RESUMO
AIM: A simple, rapid, precise, and economical spectrophotometric method has been developed for quantitative analysis of zaltoprofen (ZLT) in pharmaceutical formulations. MATERIALS AND METHODS: A mixture of methanol and water was used as a solvent. Initial stock solution of ZLT was prepared in methanol and subsequent dilution was done in water. The standard solution of ZLT in water showed two absorption maxima, one at 243.5 nm and another at 338.0 nm. RESULTS: The drug obeyed Beer-Lambert's law in the concentration range of 1-40 µg/mL with regression 0.9999 at 243.5 nm and 5-100 µg/mL with regression 0.9999 at 338.0 nm. The overall % recovery was found to be 99.53% and 99.77% at 243.5 nm and 338.0 nm, respectively, which reflect that the method is free from interference of the impurities and other additives used in tablet formulation. Relative standard deviations of absorbance from six measurements were always less than 2%. CONCLUSIONS: The results of analysis have been validated as per ICH guidelines. Both the wavelengths can be adopted in routine analysis of ZLT in tablet dosage form.
RESUMO
Quinapril hydrochloride and hydrochlorothiazide were simultaneously determined by HPTLC in pharmaceutical formulations. The drugs were separated on silica gel 60 F(254) plates using suitable combination of solvents as mobile phase. The validation parameters, tested in accordance with the requirements of ICH guidelines, prove the suitability of methods.