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用于毛细管电色谱手性分离的、涂覆有三(3,5-二甲基苯基氨基甲酸酯)纤维素的光接枝甲基丙烯酸酯基整体柱。

Photografted methacrylate-based monolithic columns coated with cellulose tris(3,5-dimethylphenylcarbamate) for chiral separation in CEC.

作者信息

Noel Echevarria Romina, Carrasco-Correa Enrique Javier, Keunchkarian Sonia, Reta Mario, Herrero-Martinez José Manuel

机构信息

Laboratorio de Investigación y Desarrollo en Métodos Analíticos (LIDMA), Facultad de Ciencias Exactas, Universidad Nacional de La Plata (UNLP), La Plata, Bs. As., Argentina.

Department of Analytical Chemistry, University of Valencia, Burjassot, Valencia, Spain.

出版信息

J Sep Sci. 2018 Mar;41(6):1424-1432. doi: 10.1002/jssc.201701234. Epub 2018 Mar 9.

Abstract

A chiral capillary monolithic column for enantiomer separation in capillary electrochromatography was prepared by coating cellulose tris(3,5-dimethylphenylcarbamate) on porous glycidyl methacrylate-co-ethylene dimethacrylate monolith in capillary format grafted with chains of [2(methacryloyloxy)ethyl] trimethylammonium chloride. The surface modification of the monolith by the photografting of [2(methacryloyloxy)ethyl] trimethylammonium chloride monomer as well as the coating conditions of cellulose tris(3,5-dimethylphenylcarbamate) onto the grafted monolithic scaffold were optimized to obtain a stable and reproducible chiral stationary phase for capillary electrochromatography. The effect of organic modifier (acetonitrile) in aqueous mobile phase for the enantiomer separation by capillary electrochromatography was also investigated. Several pairs of enantiomers including acidic, neutral, and basic analytes were tested and most of them were partially or completely resolved under aqueous mobile phases. The prepared monolithic chiral stationary phases exhibited a good stability, repeatability, and column-to-column reproducibility, with relative standard deviations below 11% in the studied electrochromatographic parameters.

摘要

通过将三(3,5-二甲基苯基氨基甲酸酯)纤维素涂覆在以毛细管形式存在的、接枝了[2-(甲基丙烯酰氧基)乙基]三甲基氯化铵链的多孔甲基丙烯酸缩水甘油酯-二甲基丙烯酸乙烯酯整体柱上,制备了一种用于毛细管电色谱中对映体分离的手性毛细管整体柱。对[2-(甲基丙烯酰氧基)乙基]三甲基氯化铵单体的光接枝对整体柱进行表面改性,以及将三(3,5-二甲基苯基氨基甲酸酯)涂覆到接枝的整体柱支架上的条件进行了优化,以获得用于毛细管电色谱的稳定且可重现的手性固定相。还研究了水相流动相中有机改性剂(乙腈)对毛细管电色谱分离对映体的影响。测试了包括酸性、中性和碱性分析物在内的几对对映体,它们中的大多数在水相流动相下部分或完全分离。所制备的整体手性固定相表现出良好的稳定性、重复性和柱间重现性,在所研究的电色谱参数中相对标准偏差低于11%。

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