HPLC测定维格列汀中的2种基因毒性杂质

Determination of Two Genotoxic Impurities in Vildagliptin by HPLC

目的:采用HPLC法测定维格列汀中的两种潜在基因毒性杂质。方法:采用KromasilC18色谱柱(250 mm×4.6 mm,5μm),流动相A为0.21%辛烷磺酸钠溶液(磷酸调节pH值至2.1),流动相B为乙腈,梯度洗脱,流速1.0 mL·min^-1,检测波长210 nm,柱温30℃。结果:维格列汀峰与两个基因毒性杂质峰的分离度均大于3.0,两个基因毒性杂质的线性范围均为0.015~0.9μg·mL^-1(r>0.998),检测限分别为0.091 ng、0.095 ng,平均回收率分别为99.0%、93.2%,RSDA=4.7%、RSDB=5.4%。结论:所用方法专属性强、准确性好、灵敏度高、操作简便,适用于维格列汀基因毒性杂质的测定。

To determine the potential genotoxic impurities in vildagliptin by HPLC.A Kromasil C18 column(250 mm×4.6 mm,5μm) was used in HPLC system;The mobile phase A was 0.21% octane sulfonic acid sodium salt solution(regulated by phosphoric acid to pH of 2.1) and the mobile phase B was acetonitrile in gradient elution at a flow rate of 1.0 mL·min^-1 with 210 nm detection wavelength.The temperature of the column was maintained at 30℃.The Injection volume was 20 μL.The two genotoxic impurities could be well separated from vildagliptin,The linear range of the two genotoxic impurities exhibited a good linear relationship from0.015~0.9 μg·mL^-1(r>0.998),The LOD were 0.091 ng and 0.095 ng.The average recoveries for impurity A and impurity B were 99.0% and 93.2% with RSD of 4.7% and 5.4% respectively.The method is simple,specific,accurate and sensitive. It is applicable to be used for the determination of the potential genotoxic impurities in vildagliptin.