HPLC法测定左舒必利的手性杂质

HPLC determination of chiral impurity in levosulpiride

目的：建立左舒必利原料手性杂质测定方法并检测手性杂质的含量。方法：采用正相高效液相色谱法,使用DAICEL OJ-H手性柱（4.6 mm×250 mm,5μm）,以正己烷-乙醇-二乙胺（90∶10∶0.1）为流动相,流速1.0 m L·min-1,检测波长230nm,柱温30℃,进样量20μL。结果：在本文色谱条件下舒必利的分离度为2.1,线性范围为1.648-16.48μg·m L-1,检测限（S/N=3）为0.099μg·m L-1,定量限（S/N=10）为0.198μg·m L-1,采用该方法检测3批原料手性杂质的结果为0.47%-0.50%。结论：本法经方法学验证可用于左舒必利中手性杂质含量的分析测定。

Objective： To establish a method for assay of the chiral impurity in levosulpiride and determine the chiral impurity. Methods： Normal phase high performance liquid chromatography was adopted. The DAICEL OJ- H chiral column（ 4. 6 mm × 250 mm,5 μm） was adopted with n- hexane- alcohol- diethylamine（ 90∶ 10∶ 0. 1） as the mobile phase at the flow rate of 1. 0 m L·min- 1. The wavelength was set at 230 nm,the column degree was 30 ℃,and the injection volume was 20 μL. Results： The resolution of sulpiride enantiomers was 2. 1 under the condition in this paper. The linearity range of levosulpiride was 1. 648- 16. 48 μg·m L- 1; the detection limit（ S /N = 3） was0. 099 μg·m L- 1,and the quantification limit（ S /N = 10） was 0. 198 μg·m L- 1. The results of three batches of raw materials were 0. 47%- 0. 50% when this method was adopted to determine the contents of the impurity chiral.Conclusion： The methodology verification shows that this method can be used to determine the related chiral substance in levosulpiride.