HPLC测定奥格列汀中基因毒性杂质残留量

Determination of Genotoxic Impurities in Omarigliptin by HPLC

关键词:  奥格列汀  原料药  基因毒性杂质  苯磺酸异丙酯  高效液相色谱法

Key words:  omarigliptin  bulk drug  genotoxic impurities  isopropyl benzenesulfonate  HPLC

摘要:

目的 建立奥格列汀原料药中基因毒性杂质的HPLC测定方法。方法 采用Zorbax SB-C₁₈色谱柱（250 mm×4.6 mm，5μm），进样量：20 μl；流动相为0.1%乙酸水-乙腈（65：35）；流速为1mL·min^-1；紫外检测器，检测波长为220 nm；柱温为25℃，色谱乙腈为溶剂。结果 该方法专属性良好，测得苯磺酸异丙酯在4~60 μg·mL^-1内线性关系良好，平均回收率为98.56%（n=9，RSD=3.78%），溶液在8 h内稳定。结论 该法操作简便，重复性好，结果准确可靠，可用于奥格列汀原料药中基因毒性杂质的测定。

Abstract:

OBJECTIVE To establish an HPLC method to determine genotoxic impurities in omarigliptin bulk drug. METHODS The HPLC was carried out with Zorbax SB-C₁₈ column with the column temperature of 25℃. The injection volume was 20 μL. The mobile phase was 0.1% acetic acid water solutiom-acetonitrile (65:35) with the flow rate of 1 ml·min^-1. The detector was UVD with the detection wave of 220 nm. Acetonitrile was used as solvent for omarigliptin. RESULTS Isopropyl benzenesulfonate could be separated completely with good linear relationship in 4-60 μg·mL^-1. The average recovery of isopropyl benzenesulfonate was 98.56%(n=9, RSD=3.78%). CONCLUSION This method is simple, reproducible and accurate for determination of genotoxic impurities in omarigliptin bulk drug.