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℃. The injection volume was 5μl and separation ratio was 1∶10. The column temperature was programmedthe initial temperature was 70℃,maintained for 1 min, raised to 190℃with a rate of 16℃/min,and then maintained for another 5 min. The detector was flame ionization detector(FID),with temperature of 250℃. 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 2.46-36.9μg/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.