Development of Sensitive and Specific Analysis of Vildagliptin in Pharmaceutical Formulation by Gas Chromatography-Mass Spectrometry

A sensitive and selective gas chromatography-mass spectrometry (gc-ms) method was developed and fully validated for the determination of vildagliptin (vil) in pharmaceutical formulation. prior to gc-ms analysis,vil was efficiently derivatized with mstfa/nh/β-mercaptoethanol at 60°c for 30 min. the obtained o-tms derivative of vil was detected by selected ion monitoring mode using the diagnostic ions m/z 223 and 252. nandrolone was chosen as internal standard. the gc-ms method was fully validated by the following validation parameters: limit of detection (lod) and quantitation (loq),linearity,precision,accuracy,specificity,stability,robustness,and ruggedness. lod and loq were found to be 1.5 and 3.5 ng ml-1,respectively. the gc-ms method is linear in the range of 3.5-300 ng ml-1. the intra- and interday precision values were less than ≤3.62%. the intra- and interday accuracy values were found in the range of -0.26-2.06%. finally,the gc-ms method was successfully applied to determine vil in pharmaceutical formulation. © 2015 ebru uçaktürk.