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通过共聚反应制备带正电荷的纤维素衍生物手性固定相用于毛细管电色谱法分离对映体。

Preparation of a positively charged cellulose derivative chiral stationary phase with copolymerization reaction for capillary electrochromatographic separation of enantiomers.

作者信息

Chen Xiaoming, Qin Feng, Liu Yueqi, Kong Liang, Zou Hanfa

机构信息

National Chromatographic Research & Analysis Center, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian, China.

出版信息

Electrophoresis. 2004 Aug;25(16):2817-24. doi: 10.1002/elps.200405904.

DOI:10.1002/elps.200405904
PMID:15352014
Abstract

A positively charged chiral stationary phase (CSP) was prepared by chemically immobilizing cellulose 3,5-dimethylphenylcarbamate onto methacryloyldiethylenetriaminopropylated silica (MCDEAPS) via a radical copolymerization reaction. The prepared CSP was evaluated for enantiomer separation in nonaqueous capillary electrochromatography (CEC). Electroosmotic flow (EOF) generated on the prepared CSP could be significantly improved with introduction of positive charges into the CSP, and separation of enantiomers in CEC has been achieved with mobile phases of ethanol and hexane-ethanol, respectively. In addition, we investigated the solvent versatility of the immobilized CSP on enantioseparations in CEC and capillary liquid chromatography (CLC) due to the elimination of dissolution of chiral selector in a number of solvents. Chiral resolution of some enantiomers was improved by adopting tetrahydrofuran (THF) and chloroform as mobile-phase modifiers, respectively.

摘要

通过自由基共聚反应将纤维素3,5-二甲基苯基氨基甲酸酯化学固定在甲基丙烯酰二乙烯三胺丙基化硅胶(MCDEAPS)上,制备了带正电荷的手性固定相(CSP)。对制备的CSP进行了非水毛细管电色谱(CEC)对映体分离评价。通过向CSP引入正电荷,可显著改善制备的CSP上产生的电渗流(EOF),并且分别使用乙醇和己烷 - 乙醇流动相在CEC中实现了对映体的分离。此外,由于消除了手性选择剂在多种溶剂中的溶解,我们研究了固定化CSP在CEC和毛细管液相色谱(CLC)对映体分离中的溶剂通用性。分别采用四氢呋喃(THF)和氯仿作为流动相改性剂,提高了一些对映体的手性拆分效果。

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引用本文的文献

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High Throughput Analysis of Chiral Compounds Using Capillary Electrochromatography (CEC) and CEC-Mass Spectrometry with Cellulose Based Stationary Phases.使用基于纤维素的固定相通过毛细管电色谱(CEC)和CEC-质谱联用对手性化合物进行高通量分析。
Sep Sci Technol. 2013;48(17):2589-2599. doi: 10.1080/01496395.2012.719984.
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Sulfated and sulfonated polysaccharide as chiral stationary phases for capillary electrochromatography and capillary electrochromatography-mass spectrometry.硫酸化和磺化多糖作为毛细管电色谱及毛细管电色谱-质谱联用的手性固定相。
J Chromatogr A. 2009 Jan 30;1216(5):857-72. doi: 10.1016/j.chroma.2008.11.082. Epub 2008 Dec 6.