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作为手性固定相的马来海松酸酐键合硅胶整体柱用于 CEC 拆分苯硫基碳酰氨氨基酸。

Maleopimaric acid anhydride-bonded silica monolith as chiral stationary phase for separations of phenylthiocarbamyl amino acids by CEC.

机构信息

Key Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources (Ministry of Education of China), School of Chemistry and Chemical Engineering of Guangxi Normal University, Guilin, PR China.

出版信息

Electrophoresis. 2010 May;31(9):1488-92. doi: 10.1002/elps.200900716.

Abstract

A new type of chiral silica monolith was successfully developed for the enantioseparation of phenylthiocarbamyl amino acids (PTC-(D/L)-AAs) by CEC. The bare monolithic silica column was prepared by a sol-gel process and has been modified chemically with aminopropyltrimethoxysilane, followed by immobilization of a chiral selector maleopimaric acid anhydride. Eight pairs of tested amino acids enantiomers including PTC-(D/L)-arginine, PTC-(D/L)-valine, PTC-(D/L)-leucine, PTC-(D/L)-4-methylphenylalanine, PTC-(D/L)-phenylalanine, PTC-(D/L)-beta-phenylalanine, PTC-(D/L)-tryptophan and PTC-(D/L)-kynurenine were well resolved with high column efficiencies. The influences of organic modifier in mobile phase on apparent retention factor, enantioselectivity factor and resolution were also investigated.

摘要

一种新型手性硅胶整体柱被成功开发出来,用于通过 CEC 对手性苯硫基碳酰氨氨基酸(PTC-(D/L)-AAs)进行对映体分离。裸硅胶整体柱是通过溶胶-凝胶工艺制备的,并用氨丙基三甲氧基硅烷进行化学修饰,然后固定手性选择剂马来海松酸酐。测试的八种对映体氨基酸对包括 PTC-(D/L)-精氨酸、PTC-(D/L)-缬氨酸、PTC-(D/L)-亮氨酸、PTC-(D/L)-4-甲基苯丙氨酸、PTC-(D/L)-苯丙氨酸、PTC-(D/L)-β-苯丙氨酸、PTC-(D/L)-色氨酸和 PTC-(D/L)-犬尿氨酸都得到了很好的分离,柱效很高。还研究了流动相中有机改性剂对表观保留因子、对映体选择性因子和分辨率的影响。

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