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在单(6A - n - 烯丙基氨基 - 6A - 脱氧)全甲基化3 - 环糊精共价键合硅胶上的对映体拆分

Enantioseparation on mono(6A-n-allylamino-6A-deoxy)permethylated 3-cyclodextrin covalently bonded silica gel.

作者信息

Lai Xiang-Hua, Ng Siu-Choon

机构信息

Department of Chemistry, National University of Singapore, 10 Kent Ridge Crescent, Singapore 119260, Singapore.

出版信息

J Chromatogr A. 2004 Dec 3;1059(1-2):53-9. doi: 10.1016/j.chroma.2004.07.018.

DOI:10.1016/j.chroma.2004.07.018
PMID:15628124
Abstract

A chiral selector, mono(6A-N-allylamino-6A-deoxy)permethylated beta-cyclodextrin, was synthesized through a facile synthetic route and chemically immobilized onto porous silica gel via hydrosilylation to afford a cyclodextrin based chiral stationary phase MeCD-CSP. This chiral stationary phase exhibited good enantioselectivity under standard HPLC conditions. The optimal resolution of 1-(p-bromophenyl)ethanol and bromopheniramine was achieved under normal-phase conditions using a mobile phase comprising n-hexane (hexane) and 2-propanol (IPA). The enantioseparation of warfarin, suprofen and a series of flavanones under reversed-phase conditions were optimized and efficient enantioseparations for these analytes were obtained.

摘要

通过简便的合成路线合成了一种手性选择剂,单(6A-N-烯丙基氨基-6A-脱氧)全甲基化β-环糊精,并通过硅氢化反应将其化学固定在多孔硅胶上,得到基于环糊精的手性固定相MeCD-CSP。该手性固定相在标准高效液相色谱条件下表现出良好的对映体选择性。在正相条件下,使用由正己烷(己烷)和2-丙醇(异丙醇)组成的流动相,实现了1-(对溴苯基)乙醇和溴苯那敏的最佳分离度。优化了华法林、舒洛芬和一系列黄烷酮在反相条件下的对映体分离,并获得了这些分析物的高效对映体分离。

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