A Validated LC Method for the Determination of Enantiomeric Purity of Clopidogrel Intermediate Using Amylose-Based Stationary Phase

被引：7
|
作者：
Zacharis, Constantinos K. [1 ]
Vastardi, Elli [1 ]
机构：
[1] Pharmathen SA, R&D API Operat, Analyt Dev Lab, Thessaloniki 57001, Greece
来源：
CHROMATOGRAPHIA | 2015年 / 78卷 / 11-12期
关键词：
Chiral; Enantioseparation; Clopidogrel; Intermediate; HPLC;
D O I：
10.1007/s10337-015-2892-0
中图分类号：
Q5 [生物化学];
学科分类号：
071010 ; 081704 ;
摘要：
A simple chiral liquid chromatographic method for the enantiomeric purity of methyl (2S)-(2-chlorophenyl)-(2-(thiophen-2-yl)ethylamino) acetate-a clopidogrel intermediate-is proposed. Chromatographic separations are carried out isocratically on a chiral amylose-based column (ChiralPAK AD-H) using a mobile phase consisting of hexane/isopropanol/diethylamine, 90/10/0.1, v/v/v. Under the optimum conditions, the resolution between the two isomers was found to be more than 4.5. The method was developed and validated in terms of linearity, precision and accuracy, limit of detection (LOD) and quantitation (LOQ) and robustness. The proposed approach has been successfully applied to bulk samples for evaluating enantiomeric purity.
引用
收藏
页码：819 / 824
页数：6
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