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用于亲水相互作用加压毛细管电色谱的甘氨酸键合硅胶整体柱作为两性离子固定相。

Glycin-bonded silica monolithic column as zwitterionic stationary phase for hydrophilic interaction pressurized capillary electrochromatography.

作者信息

Lin Xucong, Zeng Wencan, Wang Xiaochun, Xie Zenghong

机构信息

Department of Chemistry, Fuzhou University, Fuzhou, Fujian, PR China.

出版信息

J Sep Sci. 2009 Aug;32(15-16):2767-75. doi: 10.1002/jssc.200900107.

Abstract

A novel zwitterionic monolith was prepared by in situ covalent attachment of glycin to a gamma-glycidoxypropyltrimethoxysilane-modified silica monolith. The monolith possessing in its structure bonded secondary amine groups and carboxylic acid groups was evaluated in pressurized CEC (pCEC) system using small neutral and charged solutes. Owing to the zwitterionic nature of the resulting stationary phase, the direction and magnitude of EOF in this column could be manipulated by adjusting the pH values of the mobile phase. Typical hydrophilic interaction was observed when the ACN content exceeded 45%. Separations of acidic and basic compounds were performed on the prepared column in weakly anodic and cathodic EOF modes, respectively. The organic solvent composition, the salt concentration, and the pH of the mobile phase have effects on the electrochromatographic retention. Besides the hydrophilic interaction and electrophoretic mechanism, electrostatic interactions are also involved in the separations of acids and bases on the zwitterionic column.

摘要

通过将甘氨酸原位共价连接到γ-缩水甘油氧基丙基三甲氧基硅烷改性的硅胶整体柱上,制备了一种新型两性离子整体柱。使用小分子中性和带电溶质在加压毛细管电色谱(pCEC)系统中对结构中含有键合仲胺基团和羧酸基团的整体柱进行了评估。由于所得固定相的两性离子性质,该柱中电渗流的方向和大小可通过调节流动相的pH值来控制。当乙腈含量超过45%时,观察到典型的亲水相互作用。分别在弱阳极和阴极电渗流模式下,在制备的柱上对酸性和碱性化合物进行分离。流动相的有机溶剂组成、盐浓度和pH值对电色谱保留有影响。除了亲水相互作用和电泳机制外,静电相互作用也参与了两性离子柱上酸碱的分离。

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