Development and Validation of an Stability Indicating RP-LC Method for Determination of Imatinib Mesylate

A new, sensitive and stability indicating liquid chromatographic method has been developed for the determination of imatinib mesylate (IM). Efficient chromatographic separation was achieved using a C₁₈ column with simple mobile phase combination delivered in an isocratic mode and quantitation was carried out using ultraviolet detection. For the first time, a novel microwave assisted degradation procedure was employed for stress testing studies. In addition, orthogonal separation technique was applied to demonstrate selectivity of the proposed method. The method has demonstrated excellent linearity over the range of 25–1,600 ng mL⁻¹. Moreover, the method was found to be sensitive with a low limit of detection (3.35 ng mL⁻¹) and limit of quantitation (10.16 ng mL⁻¹). The method has shown good and consistent recoveries (99.35–100.69%) with low intra- and inter-day relative standard deviation (RSD) (<2.5%). Experimental design confirmed that peak area was unaffected by small changes in critical factors, in robustness study. The validated method was successfully applied for determination of IM in pharmaceutical formulations.

     

Development and validation of an ion-pairing RP-HPLC method for the estimation of gatifloxacin in bulk and formulations

A new, simple, and sensitive ion-pair reverse-phase liquid chromatographic method is developed and validated for the estimation of 1-cyclopropyl-6-fluoro-8-methoxy-7-(3-methylpiperazin-1-yl)-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid (gatifloxacin) in bulk and formulations using a UV detector under isocratic conditions. The selected mobile phase consists of the aqueous phase (a 25 mM citrate buffer comprising of 10mM cationic and anionic pairing agents, pH adjusted to 3.5) and acetonitrile (52:48%, v/v). The selected wavelength is 292 nm. Retention time of gatifloxacin is 5.2 min. The linearity range is found to be 50 to 1000 ng/mL (the regression equation is area = 105.5 x concentration in ng/mL--695.8), and the regression coefficient is 0.9996. Validation results demonstrate accuracy, precision, and reproducibility (relative standard deviation < 3%) of the method. The detection and quantitation limits are found to be 6.50 and 17.38 ng/mL, respectively. The method is successfully used for the estimation of gatifloxacin in a variety of dosage forms, and the results are in good agreement with the label claims.     

Development and Validation of an Stability Indicating RP-LC Method for Determination of Imatinib Mesylate

A new, sensitive and stability indicating liquid chromatographic method has been developed for the determination of imatinib mesylate (IM). Efficient chromatographic separation was achieved using a C₁₈ column with simple mobile phase combination delivered in an isocratic mode and quantitation was carried out using ultraviolet detection. For the first time, a novel microwave assisted degradation procedure was employed for stress testing studies. In addition, orthogonal separation technique was applied to demonstrate selectivity of the proposed method. The method has demonstrated excellent linearity over the range of 25–1,600 ng mL^?1. Moreover, the method was found to be sensitive with a low limit of detection (3.35 ng mL^?1) and limit of quantitation (10.16 ng mL^?1). The method has shown good and consistent recoveries (99.35–100.69%) with low intra- and inter-day relative standard deviation (RSD) (<2.5%). Experimental design confirmed that peak area was unaffected by small changes in critical factors, in robustness study. The validated method was successfully applied for determination of IM in pharmaceutical formulations.