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A novel RP-HPLC method was developed and validated for the determination of compounds in an oral solution. The method describes the determination of domperidone along with sodium methylparaben, sodium propylparaben and sodium benzoate in liquid oral formulation. The chromatographic separations were performed using BDS Hypersil 5 µm C18 column and gradient elution (solvent A: phosphate buffer, pH 3.5 and solvent B: methanol) keeping a flow rate of 1.5 mL/min. Detection was done at dual wavelength (232 nm for domperidone and sodium benzoate, and 257 nm for sodium methylparaben and sodium propylparaben). Analysis time was <17 min. The retention times for domperidone, sodium benzoate, sodium methylparaben and sodium propylparaben were found to be 10.0, 6.5, 8.0, and 13.5 min, the calibration curves for domperidone, sodium benzoate, sodium methylparaben and sodium propylparaben were found to be linear in the range of 250-750, 50-150, 50-150, and 5-15 µg/mL, respectively. [ABSTRACT FROM AUTHOR]

A derivative UV spectrophotometric and a reversed phase high-performance liquid chromatographic method for determination of ciprofibrate in tablets was developed. The first-order derivative UV spectrophotometric method found to be accurate with 100.57±0.97 recovery and precise with a coefficient of variation of 1.44. These results were compared to those obtained by reference methods, zero-order UV spectrophotometric method and a reversed-phase high-performance liquid chromatography method. A reversed-phase C8 column with methanol:water (90:10, pH 3.7) mobile phase was used and the detector wavelength was set at 232 nm. Calibration solutions used in HPLC were ranging from 2 to 12 µg/ml. An ANOVA test (P = 0.0226, F = 4.935) showed that the results obtained with the derivative UV spectrophotometric method were comparable to those obtained using reference methods. [ABSTRACT FROM AUTHOR]

A simple, selective, precise high-performance thin-layer chromatographic method for simultaneous determination of amlodipine besylate and metoprolol succinate in bulk and pharmaceutical combined dosage form was developed and validated. The method employed HPTLC aluminum plates precoated with silica gel 60F-254 (10x10) as the stationary phase. The solvent system consisted of toluene:ethyl acetate:methanol:triethylamine (4:1:1:0.4 v/v/v). The system was found to give a compact spot for amlodipine besylate (Rf = 0.39±0.02) and metoprolol succinate (Rf = 0.59±0.02). Densitometric analysis of amlodipine besylate and metoprolol succinate was carried out in the absorbance mode at 254 nm. Linear regression analysis data for the calibration plots showed good linear relationship with r² = 0.9990±0.0013 with respect to peak area in the concentration range 400-1400 ng per spot for amlodipine besylate and r² = 0.9993±0.0013 with respect to peak area in the concentration range 3800-13300 ng per spot for metoprolol succinate. The method was validated for precision, recovery and robustness. The limits of detection and quantitation were 39.99 and 121.20 ng per spot for amlodipine besylate and 234.31 and 710.03 ng per spot for metoprolol succinate, respectively. Statistical analysis proved that the method is selective, precise and accurate for the estimation of amlodipine and metoprolol. [ABSTRACT FROM AUTHOR]

A new simple, precise, accurate and selective RP-HPLC method has been developed and validated for estimation of Ethacridine lactate in pharmaceutical formulation. The method was carried out on a Qualisil RP C-18 (250 mm x 4.6 mm, 5 µm) column with a mobile phase consisting of methanol: water (60:40 v/v), pH adjusted to 2.8 with orthophosphoric acid and low rate of 1.0 mL/min. Detection was carried out at 271 nm. The retention time for ethacridine lactate was found to be 4.41 min. The ethacridine lactate followed linearity in the concentration range of 2- 12 µg/mL (r² = 0.9980). The amount of the drug estimated by proposed method was found to be in good agreement with label claim. The developed method was validated for sensitivity, accuracy, precision, ruggedness and robustness. The LOD and LOQ were found to be 0.11 and 0.33 µg. The proposed method can be used for routine analysis of ethacridine lactate in bulk drug and pharmaceutical formulation. [ABSTRACT FROM AUTHOR]

Quinapril hydrochloride and hydrochlorothiazide were simultaneously determined by HPTLC in pharmaceutical formulations. The drugs were separated on silica gel 60 F254 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. [ABSTRACT FROM AUTHOR]

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]