Aim and Backrgound:A stability-indicating LC method was developed for the simultaneous determination of Ibuprofen and Famotidine in pharmaceutical dosage forms.Materials and Methods:The chromatographic separation was achieved on Acquity UPLC BEH C-18,50 mm × 2.1 mm and 1.7 μm column with gradient elution. The mobile phase A contains a mixture of 50 mM sodium acetate buffer (pH 5.5): methanol (85:15, v/v), and the mobile phase B contains a mixture of 50 mM sodium acetate buffer (pH 5.5): methanol (25:75, v/v). The flow rate was 0.3 mL min-1, and the detection wavelength was 260 nm.Results:The limit of detection for Ibuprofen and Famotidine was 1.6 and 1.2 μg mL-1, respectively. The limit of quantification (LOQ) for Ibuprofen and Famotidine was 5.1 and 4.3 μg mL-1, respectively.Conclusion:This method was validated for accuracy, precision, and linearity. The method was also found to be stability indicating.

A stability-indicating ultra perfomance liquid chromatography (UPLC) method was developed for the simultaneous determination of sumatriptan succinate and Naproxen sodium in pharmaceutical dosage forms. The chromatographic separation was achieved on C18, 50 mm × 4.8 mm, 1.8-µm particle size column. The mobile phase contains a mixture of 0.2% ortho phosphoric acid and acetonitrile as the mobile phase in gradient elution technique. The retention time of Sumatriptan and Naproxen was found to be 1.7 and 2.7 min respectively. The total runtime was 5 min within which two active compounds and degradation products were separated. This method allows the determination of 850-2565 µg mL -1 of sumatriptan succinate and 5000-15000 µg mL -1 of Naproxen sodium. The flow rate was 1.0 mL min -1 and the detection wavelength was 225 nm. The limit of detection (LOD) for sumatriptan succinate and Naproxen sodium was 1.9 and 1.5 µg mL -1 , respectively. The limit of quantification (LOQ) for sumatriptan succinate and Naproxen sodium was 6.3 and 4.8 µg mL -1 , respectively. This method was validated for accuracy, precision, linearity and robustness. sumatriptan succinate and Naproxen sodium were subjected to different ICH prescribed stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation and the method was also found to be stability indicating. Ultra performance liquid chromatography (UPLC) is a recent technique in liquid chromatography, which enables significant reductions in separation time and solvent consumption. Literature indicates that UPLC system allows about ninefold decrease in analysis time as compared to the conventional HPLC system using 5μm particle size analytical columns, and about threefold decrease in analysis time in comparison with 3μm particle size analytical columns without compromise on overall separation [23][24][25][26][27]. Rapid Simultaneous Determination of SumatriptanHence, a rapid, accurate stability indicating UPLC method for the simultaneous determination of SS and NS from combined dosage form was developed and validated. Experimental Instrumentation and chromatographic conditionsThe Waters UPLC Acquity system we used consists of a binary solvent manager, a sample manager and a UV detector. Zorbax SB C-18, 50 mm x 4.6 mm i.d with 1.8µm particles was used as stationary phase. 0.2% ortho phosphoric acid in water (pH 2.2) as solvent A and acetonitrile and water in the ratio 90:10; v/v, was as solvent B used for mobile phase. Prior to use, the mobile phase was mixed thoroughly and degassed. ReagentsStandards were supplied by D.C.O. Hyderabad, India. HPLC grade acetonitrile, analytical grade ortho phosphoric acids were purchased from Merck (Mumbai, India). Water was prepared by Millipore MilliQ Plus water purification system. Commercial pharmaceutical preparation of Triximet combined tablets were purchased from the market. The declared content of tablets was Sumatriptan 85 mg and Naproxen 500 mg per tablet. Preparation of solutionsStandard solutions: A standard so...

The present paper describes stability indicating reverse phase Ultra performance liquid chromatographic (RPLC) assay method for Atrovastatin Calcium in bulk drugs. The developed method is also applicable for the related substance determination and degradation products generated from forced decomposition studies. The drug substance was subjected to stress conditions of acid hydrolysis, base hydrolysis, oxidation, photolysis and thermal degradation. The degradation of Atrovastatin was observed under acid hydrolysis, base hydrolysis and peroxide hydrolysis. The drug was found to be stable to other stress conditions attempted. Successful separation of the drug from synthetic impurities and degradation product formed under stress conditions was achieved on a C18 column using buffer 0.02 M phosphoric acid and acetonitrile. The developed UPLC method was validated with respect to linearity, accuracy, precision, specificity and ro-bustness. The developed UPLC method to determine the related substances and assay determination of Atrovastatin can be used to evaluate the quality of regular production samples. It can be also used to test the stability sample of Atrovastatin Calcium

A simple, precise and rapid stability-indicating ultra-performance liquid chromatography (UPLC) method was developed for the simultaneous quantitative determination of Olmesartan, Amlodipine and Hydrochlorothiazide from their innovative Pharmaceutical combination drug product, with the presence of degradation products. It involved a 50 mm × 2.1 mm, 1.8 µm Phenyl column. The separation was achieved on simple gradient method. The mobile phase A contains a mixture of sodium perchlorate buffer pH 3.2(0.053M): acetonitrile in the ratio 90:10, v/v, and mobile phase B contains a mixture of sodium perchlorate buffer pH 3.2(0.053M): acetonitrile in the ratio 10:90, v/v. The flow rate was 0.7 mL•min-1 and column temperature was maintained at 55˚C.The gradient program (T/%B) was set as 0/10, 2/50, 4/80, and 6.0/10. The detector wavelength was 271 nm for Hydrochlorothiazide, 215 for Olmesartan and 237 nm for Amlodipine. The retention times of Olmesartan, Amlodipine, and Hydrochlorothiazide are 3.5, 3.3 and 0.9 minutes; respectively. The total runtime was 6.0 minutes within which three active compounds and their degradation products were separated. The described method was validated with respect to system suitability, specificity, linearity, precision and accuracy. The precision of the assay method was evaluated by carrying out six independent assays of Olmesartan, Amlodipine, and Hydrochlorothiazide (0.004 mg•mL-1 , 0.001 mg•mL-1 , 0.0025 mg•mL-1). The accuracy of the method was evaluated in triplicate at three concentration levels, i.e. 50%, 100%, and 150% of target test concentration. The described method was linear over the range, 2 to 6 µg•mL-1 for Olmesartan, 0.5 to 1.5 µg•mL-1 Amlodipine and 1.25 to 3.75 µg•mL-1 for Hydrochlorothiazide. The method is fast and is suitable for high-throughput analysis of the drug and one can analyze about 240 samples per working day, facilitating the processing of large-number batch samples.

A simple, sensitive gradient rapid resolution liquid chromatographic assay method has been developed for the quantitative determination of Candesartan Cilexetil in bulk active pharmaceutical ingredient, used for the treatment of hypertension. The developed method is also applicable for the process related impurities determination. Efficient chromatographic separation was achieved on a C18 stationary phase with simple mobile phase combination delivered in a gradient mode and quantification was by ultraviolet detection at 210 nm at a flow rate of 0.4 mL·min −1. In the developed UPLC method the resolution between Candesartan Cilexetil and its two potential impurities was found to be greater than 2.0. Regression analysis showed an r value (correlation coefficient) greater than 0.99 for Candesartan Cilexetil and its two impurities. This method was capable to detect two impurities of Candesartan Cilexetil at a level of 0.003% with respect to test concentration of 1.0 mg·mL −1 for a 2 μL injection volume. The bulk active pharmaceutical ingredient was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. Considerable degradation was found to occur in oxidative stress conditions. The stress samples were assayed against a qualified reference standard and the mass balance was found close to 99.5%. The developed RP-LC method was validated with respect to linearity, accuracy, precision and robustness.