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Journal of Analytical Methods in Chemistry
Volume 2015, Article ID 707414, 7 pages
http://dx.doi.org/10.1155/2015/707414
Research Article

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

Faculty of Pharmacy, Department of Analytical Chemistry, Hacettepe University, Sıhhıye, 06100 Ankara, Turkey

Received 2 September 2015; Accepted 19 October 2015

Academic Editor: Miguel de la Guardia

Copyright © 2015 Ebru Uçaktürk. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

Abstract

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/NH4I/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.