摘要
目的建立测定维格列汀原料药中对映异构体的HPLC测定方法。方法采用Chirapak IC-3手性色谱柱(250 mm×4.6 mm,3μm);流动相:正己烷–乙醇–三乙胺(150∶750∶1);检测波长:210 nm;体积流量:0.6 mL/min;进样量:20μL;柱温:35℃。结果在上述色谱条件下,维格列汀与其对映异构体的分离度大于5;最低定量限为1.2μg/mL,最低检测限为0.3μg/mL;维格列汀和对映异构体在1.2~30.0μg/mL与峰面积呈良好的线性关系。对映异构体的加样回收率为99.67%,RSD值为2.1%;色谱参数变动对对映异构体的检测没有影响。结论本方法灵敏度高,重现性好,适用于维格列汀中对映异构体杂质的检查。
Objective To establish an HPLC method for determination of enantiomer in vildagliptin API. Methods Chirapak IC-3 column(250 mm × 4.6 mm, 3 μm) was used. The mobile phase consisted of hexane-ethanol-triethylamine(150∶750∶1). The detection wavelengths were set at 281 nm. The flow rate was 0.6 mL/min, volume of injection was 20 μL, and temperature of column was set at 35 ℃. Results The resolution of vildagliptin and enantiomer was good with R > 5. The LOQ was 1.2 μg/mL, and the LOD was 0.3 μg/mL. The linear relationship was good in the range of 1.2 - 30.0 μg/mL. The recovery of enantiomer was 99.67% with RSD 2.1%. The change of chromatographic parameters had no effect on the detection of enantiomer. Conclusion This method has high sensitivity and good reproducibility, and is suitable for the detection of enantiomer impurities in vildagliptin.
作者
王丽红
刘均洪
WANG Li-hong;LIU Jun-hong(Department of Pharmaceutical Engineering,Qingdao University of Science&Technology,Qingdao 266042,China)
出处
《现代药物与临床》
CAS
2019年第11期3215-3217,共3页
Drugs & Clinic
