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 1:10. 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.
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 programmed:the 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.