Objective: The objective of present work was to develop and validate simple, precise, accurate and specific stability indicating method for determination of acotiamide in presence of its degradation products.Methods: An isocratic RP-HPLC method has been developed using C-8 Thermo Hypersil BDS Column (250 x 4.6 mm i.d., 5µparticle size) with the mobile phase composition of acetonitrile: 0.1 % triethylamine in 0.2% formic acid (30: 70) at column oven temperature of 40 °C. The flow rate was 1.0 ml min-1 and effluent was detected at 282 nm. The method was validated in terms of linearity, accuracy, precision, LOD (Limit of Detection), LOQ (Limit of Quantification) and robustness as per ICH guidelines.Results: The method was found to be linear in the range of 10-60µg/ml. Limit of detection and limit of quantification was found to 0.36µg/ml and 1.10 µg/ml.% Recovery was found to be in the range of 99.45%-99.75%and precision less than 2%. The developed method was successfully applied for estimation of Acotiamide in marketed tablet formulation and percentage assay was found to be 100.45%. Acotiamide was subjected to stress degradation under acid, base, neutral hydrolysis, oxidation, dry heat, photolysis conditions. Significant degradation was observed in acid and base degradation.Conclusion: The developed RP-HPLC method was simple, rapid, accurate, precise and stability indicating for the estimation of Acotiamide in bulk and tablet dosage form.

Aim: The present study reports the degradation behavior of new antihypertensive drug Riociguat under various stress conditions as per International Conference on Harmonization guidelines ICH, Q2(R1). Materials and Methods: Riociguat was subjected to stress degradation under hydrolytic (acidic, alkaline and neutral), oxidative, photolytic and thermal stress conditions to investigate the inherent stability. A rapid, accurate, precise and robust HPLC method was developed on Waters Symmetry C 18 Column (150mm X 4.6 mm, 5µ) using isocratic elution of 10 mm ammonium acetate buffer pH 5.7 and acetonitrile in the ratio of 70:30 with the flow rate at 1.0 mL/min.The detection was performed at 254nm. Results: The drug was found to be degraded in alkaline and oxidative condition whereas it was stable under acidic, neutral hydrolytic, thermal and photolytic conditions. Two degradation products (DP1, DP2) under alkaline condition and one under oxidative condition (DP3) were characterized by LC-HR-MS/MS with accurate mass measurements. Degradation products (DP1, DP2 and DP3) were isolated by preparative HPLC and were characterized by 1 H NMR, 13 C NMR, APT and IR Techniques. Conclusion: Using spectral data analysis, alkaline degradation product DP1 wascharacterized as 2-(1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl)-N5-methylpyrimidine-4,5,6-triamine and DP2 was characterized as 2-(1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl)-6-amino-7-methyl-7H-purin-8(9H)-one while oxidative degradation product DP3was characterized as methyl 2-(1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl)-4,6diaminopyrimidin-5-ylmethylcarbamate-N-oxide.The developed chromatographic method was validated in terms of specificity, linearity, accuracy, precision as per ICH guidelines. The robustness of the method was studied with 2-level fractional factorial design 2^4-1 .

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Objective: To develop and validate stability indicating HPTLC method for determination of clevidipine butyrate in synthetic mixture. Methods:The present study deals with development and validation of stability indicating HPTLC method for estimation of clevidipine butryate. Chromatographic separation was performed on aluminum plate pre coated with Silica Gel 60 F254 using toluene: ethyl acetate (8:2) as mobile phase. TLC scanner was set at wavelength of 370 nm. Results: Retention factor RfConclusion: A new, Simple, Accurate, Precise, Sensitive and economic stability indicating HPTLC method has been developed and validated for the determination of clevidipine and can be employed for stability indicating analysis.of clevidipine was found to be 0.49. The method was validated as per ICH guidelines. Calibration curve was in the range of 1000-6000ng/band. The correlation coefficient was found to be 0.999. The precision expressed by RSD was less than 2%. The accuracy of method was confirmed by recovery studies using standard addition method and recovery was found to be 99.03-99.57%. The drug was subjected to ICH prescribed hydrolytic, oxidative, photolytic and thermal stress conditions. Clevidipine and its degradation products were well resolved under experimental conditions. The method was validated according to ICH guidelines. The drug showed significant degradation in alkaline and acidic condition and slight degradation in oxidative condition. The drug was stable in thermal condition.