Determination of genotoxic impurities in saxagliptin bulk drug by GC / 国际药学研究杂志

ABSTRACT

Objective To establish a method to determine genotoxic impurities in saxagliptin bulk drug. Methods The gas chromatography(GC) was carried out with INNOWAX capillary column. The inlet temperature was 120°C. The injection volume was 5 µl and separation ratio was 110. The column temperature was programmed the initial temperature was 70°C, maintained for 1 min, raised to 190°C with a rate of 16 °C/min, and then maintained for another 5 min. The detector was flame ionization detector(FID), with temperature of 250°C. The carrying gas was N2 with the flow rate of 1 ml/min. Methanol was used as solvent for saxagliptin. Results Methyl mesylate, ethyl mesylate and isopropyl mesylate could be separated completely with good linear relationship between 2.44- 36.6, 2.38-35.7 and 2.46-36.9 µg/ml, respectively. The average recovery was 96.94%, 95.96% and 105.47%(n=9), respectively. Conclusion This method is simple, reproducible and accurate enough for the determination of genotoxic impurities in saxagliptin bulk drug.