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目的:建立普拉克索对映异构体的HPLC手性拆分分析方法,用于S-盐酸普拉克索光学纯度的分析测定。方法:选用三-(5-氯-2-甲基苯基氨基甲酸酯)-直链淀粉修饰的正相硅胶(Chiralpak AY-H)为手性固定相,以正己烷-异丙醇-二乙胺(85∶15∶0.1)为流动相,流速1.0 m L·min-1,检测波长254 nm,柱温35℃,拆分普拉克索对映异构体。结果:普拉克索消旋体在此条件下的分离度为6.0。将该方法应用于手性拆分反应得到的盐酸普拉克索的光学纯度测定,各批供试样品中均未检出对映异构体杂质,对映体过量(enantiomeric excess,ee)值为100%。结论:本文建立的方法经方法学验证,可用于盐酸普拉克索光学纯度的分析测定。
OBJECTIVE: To establish a HPLC chiral resolution method for enantiomers of pramipexole, which is used for the determination of pramipexole hydrochloride in optical purity. Methods: The chiral stationary phase of Chiralpak AY-H modified with tris- (5-chloro-2-methylphenylcarbamate) -amylase was prepared. The mobile phase was diethylamine (85:15:0.1), the flow rate was 1.0 m L · min-1, the detection wavelength was 254 nm and the column temperature was 35 ℃. The enantiomers of pramipexole were resolved. Results: The resolution of pramipexole under this condition was 6.0. The method was applied to the optical purity determination of pramipexole hydrochloride obtained by chiral resolution. No enantiomer impurity was detected in each batch of samples. The enantiomeric excess (ee) was 100%. Conclusion: The method established in this paper is validated by methodology and can be used for the analysis and determination of pramipexole hydrochloride optical purity.