环糊精修饰的胶束电动色谱法手性拆分雷替曲塞

Chiral separation of raltitrexed by cyclodextrin-modified micellar electrokinetic chromatography.

作者信息

Liu Yi, Fu Xiaofang, Ma Chao, Zhong Jiasheng, Liao Yiping, Liu Huwei

机构信息

Institute of Analytical Chemistry, Key Laboratory of Bioorganic Chemistry and Molecular Engineering of the Ministry of Education, College of Chemistry and Molecular Engineering, Peking University, Beijing, 100871, China.

出版信息

Anal Bioanal Chem. 2009 Jan;393(1):321-6. doi: 10.1007/s00216-008-2444-7. Epub 2008 Oct 19.

DOI:10.1007/s00216-008-2444-7

PMID:18931995

Abstract

A rapid and effective method was developed for the chiral separation of raltitrexed (RD) enantiomers by carboxymethyl-beta-cyclodextrin (CM-beta-CD)-modified micellar electrokinetic chromatography (MEKC). Optimization of conditions including the type and concentration of the chiral selector, concentration of sodium dodecyl sulfate (SDS), pH and concentration of the background electrolyte (BGE), capillary temperature, and applied voltage was investigated. The enantiomers of raltitrexed could be separated with satisfactory resolution and linear response by using 75 mM Tris-phosphate at pH 8.0 containing 30 mM SDS and 8 mM CM-beta-CD as buffer system. Furthermore, the usefulness of this method was demonstrated in a purity test of a real synthetic drug sample.

摘要

开发了一种通过羧甲基-β-环糊精（CM-β-CD）修饰的胶束电动色谱（MEKC）对手性雷替曲塞（RD）对映体进行快速有效分离的方法。研究了包括手性选择剂的类型和浓度、十二烷基硫酸钠（SDS）浓度、背景电解质（BGE）的pH值和浓度、毛细管温度以及施加电压等条件的优化。通过使用pH 8.0的75 mM磷酸三乙胺缓冲液，其中含有30 mM SDS和8 mM CM-β-CD作为缓冲体系，雷替曲塞对映体能够以令人满意的分辨率和线性响应进行分离。此外，该方法的实用性在一个实际合成药物样品的纯度测试中得到了证明。