脱氢枞基异硫氰酸酯柱前衍生化结合紫外可见检测法对氨己烯酸对映体进行毛细管电泳手性分离

Capillary electrophoresis enantioselective separation of vigabatrin enantiomers by precolumn derivatization with dehydroabietylisothiocyante and UV-vis detection.

作者信息

Zhao Shulin, Zhang Rongcan, Wang Hengshan, Tang Lidong, Pan Yinming

机构信息

College of Chemistry and Chemical Engineering, Guangxi Normal University, Guilin 541004, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Apr 3;833(2):186-90. doi: 10.1016/j.jchromb.2006.01.018. Epub 2006 Feb 20.

DOI:10.1016/j.jchromb.2006.01.018

PMID:16488672

Abstract

A simple and reliable capillary electrophoresis (CE) method with UV-vis detection is presented for the enantioselective separation and determination of vigabatrin enantiomers. Dehydroabietylisothiocyante (DHAIC), a novel chiral derivatizing reagent, was used for precolumn derivatization of vigabatrin enantiomers. Optimal separation was obtained with a running buffer consisting of 50 mM Na2HPO4 (pH 9.0), 17 mM sodium dodecyl sulfate (SDS) and 25% acetonitrile. The enantiomeric separation of vigabatrin derivatives was achieved within 25 min, and the resolution was found to be 2.1. Detection was followed by direct UV absorptiometric measurements at 202 nm. A calibration curve ranging from 0.3 to 6.0 microg/ml was shown to be linear, and the limit of detection was 0.15 microg/ml. The developed method has been applied to the determination of vigabatrin enantiomers spiked in human plasma, no interferences were found from endogenous amino acids.

摘要

本文介绍了一种采用紫外可见检测的简单可靠的毛细管电泳（CE）方法，用于对氨己烯酸对映体进行对映选择性分离和测定。新型手性衍生试剂脱氢枞基异硫氰酸酯（DHAIC）用于氨己烯酸对映体的柱前衍生。使用由50 mM磷酸氢二钠（pH 9.0）、17 mM十二烷基硫酸钠（SDS）和25%乙腈组成的运行缓冲液可获得最佳分离效果。氨己烯酸衍生物的对映体分离在25分钟内完成，分离度为2.1。通过在202 nm处直接进行紫外吸收测量进行检测。结果表明，校准曲线在0.3至6.0 μg/ml范围内呈线性，检测限为0.15 μg/ml。所建立的方法已应用于测定加标于人体血浆中的氨己烯酸对映体，未发现内源性氨基酸的干扰。