A simple, precise, sensitive, rapid and reproducible HPTLC method for the simultaneous estimation of the rabeprazole and itopride hydrochloride in tablets was developed and validated. This method involves separation of the components by TLC on precoated silica gel G60F254 plate with solvent system of n-butanol, toluene and ammonia (8.5:0.5:1 v/v/v) and detection was carried out densitometrically using a UV detector at 288 nm in absorbance mode. This system was found to give compact spots for rabeprazole (Rf value of 0.23 0.02) and for itopride hydrochloride (Rf value of 0.75±0.02). Linearity was found to be in the range of 40-200 ng/spot and 300-1500 ng/spot for rabeprazole and itopride hydrochloride. The limit of detection and limit of quantification for rabeprazole were 10 and 20 ng/spot and for itopride hydrochloride were 50 and 100 ng/spot, respectively. The method was found to be beneficial for the routine analysis of combined dosage form.
A stability-indicating forced-degradation study of valdecoxib was conducted using high performance thin layer chromatography (HPTLC). It was used to analyze valdecoxib as bulk drug and as tablets. Undegraded valdecoxib was eluted with a retardation factor, Rf, of 0.56. Valdecoxib was forcibly degraded by exposure to alkali, acid, oxidation, and light, the greatest degradation occurring under basic conditions. Base-degraded valdecoxib gave an additional peak with an Rf value of 0.76. The calibration curve was linear in the range of 0.2-1 microg/microL with a correlation coefficient of 0.9952. Complete validation was carried out for precision (inter-day, intra-day, repeatability), accuracy, and robustness. All the data were analyzed statistically. This HPTLC procedure shows the reliability needed for use as a stability-indicating method. It can quantify valdecoxib in bulk and in tablets and also resolves the degraded peak of valdecoxib. This method is also useful for studying the degradation pattern and degradation mechanism of valdecoxib.
A simple, precise and rapid RP-HPLC method was developed for the determination of doxazosin mesylate in pharmaceutical formulations. The method was carried out on a Chromolith RP-C18 column using a mixture of potassium phosphate buffer and methanol (40:60 v/v) and detection was done at 251 nm. The linearity range was 1-5 μg/ml. The retention time of the drug was 3.8 min. The LOD and LOQ were found to be 0.1 μg/ml and 0.5 μg/ml, respectively.
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