色谱

色谱 ›› 2014, Vol. 32 ›› Issue (4): 381-387.DOI: 10.3724/SP.J.1123.2013.10038

• 庆祝《色谱》创刊三十周年暨卢佩章院士九十华诞专刊-研究论文 • 上一篇    下一篇

一种混合模式反相弱阳离子交换色谱填料的制备及其保留机理

彭西甜1,2, 冯钰锜1   

  1. 1. 生物医学分析化学教育部重点实验室, 武汉大学化学系, 湖北 武汉 430072;
    2. 湖北省农业科学院农业质量标准与检测技术研究所, 湖北 武汉 430064
  • 收稿日期:2013-10-31 修回日期:2013-12-06 出版日期:2014-04-08 发布日期:2014-03-28
  • 通讯作者: 冯钰锜
  • 基金资助:

    国家自然科学基金项目（91017013）；湖北省农业科学院青年基金（2013NKYJJ18）.

Preparation and retention mechanism of a mixed-mode reversed-phase/weak-cationic-exchange chromatographic packing

PENG Xitian1,2, FENG Yuqi1   

  1. 1. Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China;
    2. Institute of Agricultural Quality Standards and Testing Technology Research, Hubei Academy of Agricultural Science, Wuhan 430064, China
  • Received:2013-10-31 Revised:2013-12-06 Online:2014-04-08 Published:2014-03-28

PDF

437

被引次数

17

摘要：

采用“点击化学”的合成方法制备了一种混合配体的辛基-羧基共同键合硅胶（OCS）材料，经元素分析和红外光谱表征，证明了辛基和羧基官能团均已成功键合到硅胶表面。将其作为混合模式反相弱阳离子交换（RP/WCX）的固定相填料，以3种同系物阳离子表面活性剂作为探针分子，定量研究了该固定相的混合模式保留机理，考察了溶质保留因子与盐浓度和溶质亚甲基数目的关系，验证了混合模式固定相的单点和两点保留机理的数学模型，并进一步将其应用于一系列标准碱性混合物的分离。结果表明：两点保留机理更加符合实验的结果；根据混合模式两点保留机理的数学方程，可以得到单一的疏水或离子交换作用力对总保留的影响，对混合模式色谱的实际分离应用提供了有价值的参考。本文建立了反相弱阳离子交换混合模式OCS固定相的保留机理的定量模型，并证明了该固定相在碱性化合物的分离中具有很大的应用前景。

关键词: 保留机理, 反相弱阳离子交换色谱固定相, 混合模式色谱, 色谱分离, 数学模型

Abstract:

A "mixed ligand" octyl-carboxylic co-bonded silica (OCS) packing was prepared by the method of "click chemistry". The resulting OCS packing was characterized by elemental analysis (EI) and Fourier transform infrared spectroscopy (FT-IR) to prove the successful immobilization of octyl and carboxylic groups on the surface of silica gel. Then the mixed-mode reversed-phase/weak-cationic-exchange (RP/WCX) retention mechanism of the OCS packing was quantitatively probed by studying the retention factors of a homologous series of three cationic surfactants on the mixed-mode stationary phase column as a function of the ammonium concentration in the eluent or the number of methylene groups in the solute. The one-site and two-site mixed-mode retention models of the three cationic surfactants on the OCS phases were studied by investigating the logarithm and reciprocal relationships of retention factors and salt concentrations, demonstrating that the two-site model was more suitable for the description of the retention mechanism of the three cationic surfactants on the OCS phases. Furthermore, the individual RP or WCX contribution to total retention was obtained according to the mathematical equations of two-site retention mechanism, which can provide some valuable guidance for the separation of real samples. This study developed the qualitative model of retention mechanism of the mixed-mode OCS packing, and a series of standard basic mixtures were well separated on the OCS packing, demonstrating the great application potential of OCS packing for the separation of various basic compounds.

Key words: chromatographic separation, mathematic model, mixed-mode chromatography (MMC), retention mechanism, reversed-phase/weak-cationic-exchange (RP/WCX) chromatographic packing

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