色谱

色谱 ›› 2013, Vol. 31 ›› Issue (4): 329-334.DOI: 10.3724/SP.J.1123.2012.11009

• 特别策划：色谱固定相专栏 • 上一篇    下一篇

一种混合模式反相强阳离子交换色谱固定相的制备及其保留机理的考察

彭西甜1,2,王珏1,3,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;
    3. 华东师范大学上海分子治疗与新药创新工程技术研究中心, 上海 200062
  • 收稿日期:2012-11-20 出版日期:2013-04-22 发布日期:2013-04-24
  • 通讯作者: Tel:(027)68755595,E-mail:yqfeng@whu.edu.cn
  • 基金资助:

    国家自然科学基金项目(91019013,31070327).

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

PENG Xitian1,2, WANG Jue1,3, 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; 3. Shanghai Engineering Research Center of Molecular Therapeutics and New Drug Development, East China Normal University, Shanghai 200062, China
  • Received:2012-11-20 Online:2013-04-22 Published:2013-04-24

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摘要：

采用一种简单的“混合配体”方法将辛基和磺酸基键合到硅胶表面,制备了辛基-磺酸基共同键合硅胶(OSS)材料。通过元素分析和吸附容量检测对OSS材料进行表征,证明辛基和磺酸基已成功键合到硅胶表面上。将该OSS硅胶材料作为混合模式反相强阳离子交换(RP/SCX)色谱固定相,在反相液相色谱(RPLC)流动相条件下,采用几种碱性探针分子定量地考察了该固定相的混合模式RP/SCX保留机理。通过改变流动相中缓冲盐的浓度,考察了溶质保留因子和盐浓度的对数和倒数的关系,得到了几种碱性探针分子在该混合模式OSS固定相上的单点和两点保留机理的数学模型。对两种数学模型的方程进行了线性拟合,结果表明两点保留机理更加符合实验的结果。此外,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可提供有价值的参考。

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

Abstract:

A simple and efficient method has been proposed for the preparation of octyl-sulfonic co-bonded silica (OSS) packing by the method of “mixed ligand”. The resulting OSS packing was characterized by elemental analysis and ion-exchange capacity to prove the successful immobilization of octyl and sulfonic groups on the surface of silica gel. Then the retention mechanism of several basic analytes on the developed OSS phases was evaluated under the conditions of reversed-phase liquid chromatography (RPLC) mobile phase. The results indicated that the OSS stationary phases demonstrated a mixed-mode reversed-phase/strong-cationic-exchange (RP/SCX) retention mechanism and ion-exchange interaction maybe dominate the retention of the basic analytes. By changing the salt concentration of mobile phase, the one-site and two-site mixed-mode retention models of the several basic analytes on the OSS phases were obtained by investigating the logarithm and reciprocal relationships of retention factor and salt concentration. On the basis of the linear fitting of the two mathematical equations of the retention models, the experimental results demonstrated that the two-site model was more suitable for the description of the retention mechanism of the basic analytes on the OSS phases. Furthermore, the individual RP or SCX contribution to total retention was obtained according to the mathematical equations of the two-site retention mechanism, which can provide some valuable guidance for the separation of complex samples.

Key words: mathematical model, mixed-mode chromatography (MMC), retention mechanism, reversed-phase/strong-cationic-exchange (RP/SCX) chromatographic packing

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