Original Articles
F. I. Farooqui* and R. B. Kakd
Abstract
The current work on impurity profiling of Saxagliptin in its bulk drugs, included development of a stabilityindicating reverse-phased liquid chromatographic method and its validation for the estimation of degradation related impurities (DRIs). Saxagliptin was subjected to acid and alkaline hydrolysis, H2O2 oxidation, thermal degradation and photolysis. Acid hydrolysis and base hydrolysis yielded significant degradants, which were isolated on a semi-preparative high performance liquid chromatography (HPLC) and characterized with the help of highresolution mass spectroscopy, and the possible structures of the DRIs were revealed. The chromatographic separations were accomplished on Hypersil BDS C18 column (250 mm x 4.6 mm; 5 μm) using water and acetonitrile as a mobile phase with gradient elution at 1.0 ml/min flow rate, and eluents were detected using photo diode array detector at 213 nm wavelength. The method was validated with respect to accuracy, precision, linearity, robustness, and limits of detection and quantification as per International Conference on Harmonization (ICH) guidelines.