Simultaneous determination

A novel, simple, precise, rapid, reproducible and cost effective RP-HPLC method was developed and validated for the simultaneous estimation of Nadifloxacin and Clobetasol propionate in its pharmaceutical dosage form. The chromatographic separation was carried out using C18 Shim pack XR ODS II (250 mm × 4.6 mm, 5µm) column with mobile phase comprising of Acetonitrile : Water (50:50)(%v/v). Flow rate was maintained 1.0 mL/min and quantitation was carried out using UV detection at 242nm. Retention time of Nadifloxacin and Clobetasol propionate were found to be 2.64 min and 6.19 min respectively. The method was validated by assessing different parameters such as specificity, linearity, precision, accuracy, robustness, LOD and LOQ for the developed method. The linearity range 20-240 µg/mL and 1-12 µg/mL were selected for Nadifloxacin and Clobetasol propionate respectively. The correlation coefficient (r2) for Nadifloxacin and Clobetasol propionate were found to be 0.9995 and 0.9999 respectively. The limit of detection for Nadifloxacin and Clobetasol propionate were found to be 0.029 µg/mL and 0.21 µg/mL. The limit of quantitation for Nadifloxacin and Clobetasol propionate were found to be 0.089 µg/mL and 0.64 µg/ml respectively. Percentage recovery was found to be 99% to 100.56% for Nadifloxacin and 99.37% to 99.79% for Clobetasol propionate. All the validation parameters were with-in the acceptance limit. The relative standard deviation (%RSD) was found to beless than 2% in all the assessed parameters. The developed HPLC method can successfully used for the quantitative estimation of both the drugs in its formulation.

A simple, precise and sensitive reverse-phase high performance liquid chromatographic method was developed and validated for the simultaneous estimation of Ramipril and Metoprolol tartarate in pharmaceutical formulations. Chromatographic separation was performed on a High performance liquid chromatography equipped with auto sampler and UV detector. Good sensitivity for all analyte was observed with UV detection at wavelength of 218 nm, Separation was performed on a BDS Hypersil C18 (250 X 4.6mm) 5µm, using a mixture of 0.1% Triethylamine buffer pH 3.5 and Acetonitrile in the ratio of (10:90, v/v). The method results in excellent separation with good resolution between the two analytes. The within day variation %RSD values between Ramipril and Metoprolol tartarate were 0.55 and 0.82. The recovery was greater than 98% with %RSD less than 1.00. The method was validated according to ICH guidelines by performing linearity, accuracy, precision, limits of quantitation and selectivity. The results show the method is suitable for its intended use.

A simple, rapid, and precise RP-HPLC method for simultaneous analysis of Amlodipine besylate and Glimepiride in bulk and its pharmaceutical formulations has been developed and validated. Amlodipine besylate was separated from Glimepiride by using Grace Smart Altima C8 column (25 cm × 4.6 mm, 5-μm) with a mobile phase consisting of acetonitrile: 20mM phosphate buffer (55:45 (v/v), pH 3.5) a flow rate of 1 mL/min and detection wavelength at 230 nm.  Amlodipine besylate and Glimepiride were eluted with retention times of 5.47 min and 14.17 min respectively. The method was validated for accuracy, precision, linearity, specificity and sensitivity in accordance with ICH (Q2B) guidelines. The results of all the validation parameters were found to be within the acceptable limits. The calibration plots were linear over the concentration ranges from 70-3000ng/mL for Amlodipine besylate and 100-3000ng/mL for glimepiride. The limit of detection and limit of quantification were found to be 19.4ng/mL and 58.8ng/mL for amlodipine besylate, 25.6ng/mL and 76.2ng/mL for glimepiride respectively for both the drugs. From the results it is suggested that the method is simple, reproducible, accurate and precise. The method was successfully applied for the determination of content and the dissolution profile of the combined bilayer tablet dosage form.