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Olmesartan medoxomil (OLME) belongs to a group of angiotensin II receptor blockers used as an antihypertensive agent and is currently being used for prevention of hypertension. This paper describes the validation and development of stability indicating RP-HPLC method for the determination of OLME in the presence of its degradation products generated from forced degradation study and characterization of degradation product (impurity). The assay involved gradient elution of OLME and an LC GC BDS C18 column (250 mmx4.5 mm, 5 μm particle size) was employed for loading the sample. The mobile phase A consisted of 7 ml triethylamine in 1000 ml water (pH adjusted to 3.0 with orthophosphoric acid) and B contained acetonitrile. Quantification was achieved with photodiode array detection at 257 nm. The chromatographic separation was obtained with a retention time of 6.72 min, and the method was linear in the range 50-150 µg/ml. The method was validated according to the ICH guidelines with respect to linearity, precision, accuracy, limit of detection (LOD), limit of quantification (LOQ), specificity and robustness. Impurity found in stressed and stability studies of olmesartan medoxomil in both drug substance and drug product are described. This degradation product is identified as 1-(biphenyl-4-ylmethyl)-1H-imidazole-5-carboxylic acid. An alkaline degradation pathway of Olmesartan Medoxomil, for the formation of this degradation product, has been proposed and the degradation product was characterized. [ABSTRACT FROM AUTHOR]

A dissolution method with high performance liquid chromatography (HPLC) analysis was validated for perindopril erbumine and indapamide in combination tablet formulation. The method was validated to meet requirements for a global regulatory filing and this validation included specificity, linearity, accuracy, precision, range, robustness and solution stability studies. The dissolution method, which uses a USP apparatus 1 with basket rotating at 100 rpm, 1000 ml of phosphate buffer, pH 6.8, as the dissolution medium, and reversed-phased HPLC was carried out at 50 °C on a 4.6 mmx250 mmx5 µm cyano column that contained USP packing L1 with acetonitrile:buffer 40:60 (v/v), pH 2.8, as mobile phase. UV detector was set at 225 nm. The method was found to be selective, linear, accurate and precise in the specified ranges. Intra-day and inter--day variability for method was <2% RSD. This method was successfully used for quantification of perindopril erbumine and indapamide combination tablet formulations. [ABSTRACT FROM AUTHOR]

A novel stability-indicating high-performance liquid chromatographic assay method was developed and validated for quantitative determination of ciprofibrate in bulk drugs and in pharmaceutical dosage form in the presence of degradation products. An isocratic, reversed phase HPLC method was developed to separate the drug from the degradation products, using an Ace5-C18 (250 mmx4.6 mm, 5 µm) advanced chromatography column, and methanol and water (90:10 v/v) as a mobile phase. The detection was carried out at a wavelength of 232 nm. The ciprofibrate was subjected to stress conditions of hydrolysis (acid and base), oxidation, photolysis and thermal degradation. Degradation was observed for ciprofibrate in base, in acid and in 30% H2O2. The drug was found to be stable in the other stress conditions attempted. The degradation products were well resolved from the main peak. The percentage recovery of ciprofibrate was from (98.65 to 100.01%) in the pharmaceutical dosage form. The developed method was validated with respect to linearity, accuracy (recovery), precision, system suitability, specificity and robustness. The forced degradation studies prove the stability indicating power of the method. [ABSTRACT FROM AUTHOR]