手性拆分法同时测定盐酸帕洛诺司琼光学异构体

Simultaneous detemination of optical isomers of palonosetron hydrochloride by chiral separation

目的建立一种快速、高效的同时测定盐酸帕洛诺司琼光学异构体的方法。方法采用CHIRALPAK AD手性色谱柱（250 mm×4.6 mm,5μm）,柱温40℃,乙腈-异丙醇-无水乙醇-二乙胺（75：15：10：0.2）为流动相,流速为1 m L·min^-1,检测波长为254 nm。结果盐酸帕洛诺司琼光学异构体各相邻峰之间的分离度分别为4.0、1.5、8.7,在2.0-100.0μg·L^-1内与峰面积线性关系良好（r=0.999 9、0.999 9、0.999 3）,低、中、高浓度的平均加样回收率分别为100.0%、98.4%、106.7%（n=3,RSD分别为0%、1.4%、10.8%）。结论本法分离度高,精密度、重复性及稳定性好,适用于同时测定盐酸帕洛诺司琼光学异构体。

Objective To develop an HPLC method for simultaneous detemination of optical isomers of palonosetron hydrochloride. Methods The chiral separation was carried out on CHIRALPAK AD（250 mm×4.6 mm, 5 μm） column with acetonitrile, 2-propanol, absolute alcohol and diethylamine（75 ：15 ：10 ：0.2） as the mobile phase; the flow rate was 1 m L·min^- 1 with the column temperature was 40 ℃, and the detection wavelength was 254 nm. Results Good resolution for palonosetron hydrochloride optical isomers were achieved with 4.0, 1.5, and 8.7. The linear calibration was found for palonosetron hydrochloride optical isomers within the range of 2.0 to 100 μg·L^- 1（ r = 0.999 9, 0.999 9, 0.999 3）, the average recoveries were 100.0%, 98.4%, 106.7%, and the RSDs were 0%, 1.4%, and 10.8%, respectively（n = 3）. Conclusion The method with good precision, repeatability and stability for the determination of palonosetron hydrochloride optical isomers.