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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 the determination of chiral impurities in raw materials of Zu-Sulpiride and to determine the content of chiral impurities. Methods: The mobile phase was consisted of n-hexane-ethanol-diethylamine (90:10:0.1) using DAICEL OJ-H chiral column (4.6 mm × 250 mm, 5 μm) 1.0 m L · min-1, detection wavelength 230nm, column temperature 30 ℃, injection volume 20μL. Results: Under the chromatographic conditions, the resolution of sulpiride was 2.1, the linear range was 1.648-16.48μg · m L-1, the limit of detection (S / N = 3) was 0.099μg · m L-1, N = 10) was 0.198μg · m L-1. The results of three methods for the determination of chiral impurities in raw materials ranged from 0.47% to 0.50%. Conclusion: This method is validated by methodology for the analysis of the content of chiral impurities in Zuvalipide.