Determination of genotoxic impurities in saxagliptin bulk drug by GC
10.13220/j.cnki.jipr.2016.03.034
- Author:
Fei ZHENG
1
Author Information
1. Department of Pharmacy, Dongfang Hospital, Beijing University of TCM
- Publication Type:Journal Article
- Keywords:
Gas chromatography;
Genotoxic impurities;
Saxagliptin bulk drug
- From:
Journal of International Pharmaceutical Research
2016;43(3):575-577
- CountryChina
- Language:Chinese
-
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.
