Method Development and Validation of Canagliflozin by using RP-HPLC in Pure and Tablet Dosage Form

A new method was established for simultaneous estimation of Canagliflozin by RP-HPLC method. The chromatographic conditions were successfully developed for the separation of Canagliflozin by using INERTSIL column, C18 (150x4.6)5µm column, flow rate was 1ml/min, mobile phase ratio was Water: Acetonitrile (70:30), detection wavelength was 264nm. The instrument used was Hitachi HPLC Auto Sampler, Separation module 1575. The analytical method was validated according to ICH guidelines (ICH, Q2 (R1)). The linearity study for Canagliflozin was found in concentration range of 1μg-5μg and 100μg-500μg and correlation coefficient (r2) was found to be 0.999 and 0.999, %mean recovery was found to be 100% and 100.5%, %RSD for repeatability was 0.2 and 0.4, %RSD for intermediate precision was 0.5 and 0.1 respectively.

Simultaneous estimation of telmisartan and atorvastatin calcium in API and tablet dosage form

A new method has been established for the simultaneous estimation of Telmisartan and Atorvastatin calcium by RP-HPLC method. The chromatographic conditions were successfully developed for the separation of Telmisartan and Atorvastatin calcium by using boston ODS C18 column, flow rate was 1.0ml/min, mobile Phase consists of methanol:Acetonitrile:buffer in ratio of 35:25:40. Detection wave length was 235nm.The instrument used was SHIMADZU HPLC auto sampler. The retention time of Atorvastatin calcium and Telmisartan was found to be 2.350 and 3.490 minutes respectively. The analytical method was validated according to ICH guidelines (ICH Q2b). The correlation coefficient (r2) was found to be 0.997 and 0.999 for Telmisartan and Atorvastatin calcium respectively. % mean recovery was found to be 100.943% and 100.576% for Telmisartan and Atorvastatin calcium respectively. %RSD for precision on replicate injection was 0.46 and 0.70 for Telmisartan and Atorvastatin calcium respectively. The validation study was found to be precise, robust, and repeatable. Keywords: Telmisartan, Atorvastatin calcium, ICH guidelines, Validation.

Improved Gas Chromatographic Analysisof Organophosphorus Pesticides with Pulsed Splitless Injectiony

Gas chromatographic (GC) analysis of 6 organo-phosphorus pesticides (methamidophos, acephate, omethoate, diazinon, dimethoate, and chlorpyrifos) was performed with cool on-column, splitless, and pulsed splitless injections and with nitrogen–phos phorus or mass-selective detection. The pulsed splitless technique uses a high column flow rate during injection to sweep the sample out of the inlet rapidly, reducing analyte loss due to adsorption or thermal decomposition. After injection, the column flow rate is automatically reduced to normal values for chromatographic analysis. Pesticide recoveries for splitless and pulsed splitless injections were determined by comparison of GC peak areas with those obtained with cool on-column injection. With conventional splitless injection at a column flow rate of 5 mL/min, recoveries of acephate, omethoate, and methamidophos were only 57, 63, and 71 %, respectively. Pulsed splitless methods with very fast injection flow rates dramatically improved recoveries, with all 6 pesticides falling in the 97–102% range. Because column flow rates are much less for GC with mass spectral detection (GC/MS), recoveries with splitless injection were lower and improvements with pulsed splitless injection were less dramatic for GC/MS. When splitless injection was used, recoveries of the 6 pesticides spiked into a green bean matrix were better than those of pesticides dissolved in pure solvent, presumably because matrix compounds compete with pesticides for active sites in the inlet. By using pulsed splitless injection of solvent standards with very fast initial column flow rates, systematic analyte losses in the inlet were eliminated, making recoveries of pesticides from solvent and green bean matrix very similar.

Simplex Optimization of the Alternating-Current Plasma Detector for Gas Chromatography

Several operating parameters for the alternating-current plasma detector for gas chromatography were optimized on the basis of maximization of the peak area response of the detector towards ethylmerctiry (II) chloride by the modified simplex algorithm. The parameters included in the study were the ac power output, helium make-up flow rate, column flow rate, PMT voltage, and slit width. Univariant values of the optimum were equivalent to most simplex optimum values in this study. Detector evaluation was based on the new optimized response and a new detector interface design and is compared to previous values obtained for this detector. Lower detection limits of 1.10 pg/s were realized, coupled with a relative standard deviation between 1 and 5%. Detector linearity extended over three orders of magnitude.