The present study intended to develop an easy and novel Liquid Chromatography–Mass Spectrometry/Mass spectrometry (LC–MS/MS) method for simultaneous assay of remogliflozin etabonate and vildagliptin, a combined formulation used in treatment of type II diabetes in human plasma. Alogliptin drug was selected as internal standard and the analytes were isolated from the spiked plasma matrix using liquid-liquid extraction procedure and the extracts were chromatographed on Inertsil ODS (4.6 mm×100 mm, 5 μm) C18 column. The mobile phase comprises of methanol, acetonitrile and 0.1 % formic acid in 40:50:10 (v/v) at 0.5 mL/min flow rate and analysis was completed within 6 min run time. The method produces peaks with acceptable symmetry and resolution with acceptable system suitability at 2.6 min for remogliflozin etabonate, 2.7 min for vildagliptin, 1.2 min for alogliptin (internal standard). Multiple Reaction Monitoring (MRM) mode was used for the mass spectral characterization of column eluents using mass detector. In the mass spectral studies confirms the characteristic fragment ion transitions at m/z of 523 to m/z of 247 as MH+ ion for remogliflozin, m/z of 304 to m/z of 180 as MH+ ion for vildagliptin. The method can detect both the analyte up to 1.5 ng/mL and having lower limit of quantification (LLOQ) of 5 ng/mL. The method having broad calibration range of LLOQ to 300 ng/mL and was validated for precision, accuracy, stability studies such as freeze-thaw, short term and long-term stability in LLOQ, MQC (medium quality control concentration) and HQC (high quality control concentration) levels and produce acceptable results. Hence it can be confirmed that the method can be adopted for assay of remogliflozin etabonate and vildagliptin simultaneously in plasma samples.
A simple, specific, accurate and stable reverse phase liquid chromatographic method was developed for the simultaneous determination of ticlopidine and its related impurities A and B in bulk drug and tablet dosage forms. The analysis has been performed on XTerra C18 column (250 mm×4.6 mm; 5 µ id) and mobile phase containing of methanol and pH 6.8 phosphate buffer in the ratio of 80:20 (V/V). The detection was carried at 228 nm with a flow rate of 1.0 mL/min. The retention times were found to be 8.9, 5.98 and 4.62 min for ticlopidine, impurities A and B, respectively. The method was validated according to ICH guidelines. The method was validated for specificity, precision, linearity, accuracy and robustness. The linearity range of 50-200 µg/mL for ticlopidine and 0.5-2.0 µg/mL for impurity A and B. The recoveries of ticlopidine and impurities were found to be within the range of 98-102 and the % RSD in each spiked level was found to be less than 2. The stress degradation studies confirmed that the method was effectively separate the degradation products and impurities formed in the stress studies and hence the method was found to be stability indicating method. The method can effectively quantify the standard drug ticlopidine and its impurities A and B in bulk drug and pharmaceutical formulations.
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