正相高效液相色谱法拆分普拉克索对映异构体  

Chiral separation of pramipexole enantiomers by normal phase high performance liquid chromatography

作　　者：杨庆云[1] 王志鹏[1] 邓愉凤[1] 童元峰[1] 赵同华 吴松[1] 

机构地区：[1]中国医学科学院北京协和医学院药物研究所,北京100050 [2]四川科伦药业股份有限公司,成都610500

出　　处：《药物分析杂志》2014年第11期2005-2009,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：国家"十二五"重大新药创制科技重大专项:治疗帕金森病手性药物盐酸普拉克索原料及片剂开发(2011ZX09202-101-04)

摘　　要：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 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 5μm silica- gel）. The mobile phase was hexane- isopropanol- diethylamine（ 85∶15∶0.1） at a flow rate of 1.0 mL·min^-1.The column temperature was 35℃ and the detection wavelength was 254nm. 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.

关 键 词：盐酸普拉克索 光学纯度分析 对映异构体 手性分离 手性固定相 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]