正相高效液相色谱法拆分普拉克索对映异构体

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 mL·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 an HPLC method to separate pramipexole enantiomers for optical purity detection of pramipexole dihydrochloride monohydrate. Methods: The method was carried out on a Chiralpak AY-H chiral column(amylose tris-(5-chloro-2-methylphenylcarbamate)coated on 5 (] 15:0.1)at a flow rate of 1.0 mL·min^-1.The column temperature was 35 ℃ and the detection wavelength was 254 nm. Results: Pramipexole enantiomers were separated under the above conditions,the resolution between S-and R-pramipexole was 6.0.This method was used for the optical purity detection of pramipexole dihydrochloride monohydrate obtained by chiral separation.No enantiomer impurities were detected in each batch of test samples.The enantiomeric excess(ee)of pramipexole dihydrochloride monohydrate was 100%. Conclusion: With good resolution and repeatability,the method could be reliably used for chiral separation of pramipexole dihydrochloride monohydrate,and determination of the optical purity of S-and R-pramipexole samples.

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