HPLC手性固定相法检查苄基依折麦布中的异构体杂质

High-performance liquid chromatography method with chiral stationary phase for the determination of epimer impurity in benzyl ezetimibe

目的建立简便、灵敏的手性高效液相色谱法检查苄基依折麦布中的异构体杂质。方法以Chiralpak IC为固定相,正己烷-异丙醇（体积比90∶10）为流动相,流速为1.0 m L·min-1,检测波长为232 nm。结果通过对分离条件进行优化,苄基依折麦布与其异构体杂质能达到良好分离。苄基依折麦布在质量浓度为1.0～12 mg·L-1内线性关系良好。平均回收率为99.8%,日内与日间精密度均小于3.0%。结论所建立的分析方法灵敏度高、重现性好,适用于苄基依折麦布中异构体杂质的检查。

Objective To establish a simple and sensitive chiral high performance liquid chromatography method for the determination of epimer impurity in benzyl ezetimibe. Methods A Chiralpak IC column was used as chiral stationary phase, and the mobile phase was consisted of n-hexane-isopropanol（ V： V = 90： 10） at a flow rate of 1.0 mL.min-1 ,and the detection wavelength was set at 232 nm. Results Various conditions for separation was optimized and benzyl ezetimibe and its epimer impurity could be separated successfully under the optimum condition. This calibration curve was linear for benzyl ezetimibe in the range of 1.0 - 12 mg.L-1. The average recovery was 99.8%. Both of the intra-day and inter-day precision were less than 3.0%. Conclusions The method is found to be sensitive and precise, and suitable for the determination of epimer impurity in benzyl ezetimibe.