色谱

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“一锅法”制备C18-硅胶杂化毛细管整体柱及其应用

张振宾1,2, 欧俊杰1*, 董靖1, 王方军1, 吴明火1, 林辉1,2, 邹汉法1*   

  1. 1. 中国科学院分离分析化学重点实验室, 中国科学院大连化学物理研究所, 国家色谱研究分析中心, 辽宁 大连 116023; 2. 中国科学院研究生院, 北京 100039
  • 收稿日期:2011-08-03 修回日期:2011-08-17 出版日期:2011-09-28 发布日期:2011-10-28
  • 通讯作者: 邹汉法,博士,研究员,博士生导师,主要从事生物分离分析新材料与新技术等相关研究工作. Tel: (0411)84379610,.欧俊杰,博士,副研究员,主要从事整体材料的制备及应用研究工作.
  • 基金资助:

    国家自然科学基金项目(20735004, 20975101)和国家自然科学基金创新研究群体项目(21021004)

Preparation of C18-silica hybrid monolithic capillary column by “one-pot” process and its application

ZHANG Zhenbin1,2, OU Junjie1*, DONG Jing1, WANG Fangjun1, WU Minghuo1, LIN Hui1,2, ZOU Hanfa1*   

  1. 1. CAS Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, National Chromatographic R.& A. Center, Dalian 116023, China; 2. Graduate University of Chinese Academy of Sciences, Beijing 100039, China
  • Received:2011-08-03 Revised:2011-08-17 Online:2011-09-28 Published:2011-10-28

摘要: 本文发展了一种“一锅法”制备C18-硅胶杂化毛细管整体柱的方法。发展了一种“一锅法”制备有机-无机杂化毛细管整体柱的方法。首先将四甲氧基硅烷、乙烯基三甲氧基硅烷在弱酸条件下水解,然后加入有机单体(甲基丙烯酸-N,N-二甲基十八烷基溴化铵乙酯)及自由基聚合引发剂,同步原位完成硅羟基间的缩聚反应及双键间的自由基聚合反应,从而制成C18-硅胶杂化整体柱;同时用毛细管电色谱(CEC)和毛细管液相色谱(CLC)对其柱效和分离能力进行了初步评价,并将其应用到微柱液相色谱-串联质谱对牛血清白蛋白酶解液的分离分析。结果表明,该C18-硅胶杂化整体柱具有较高的柱效和较好的重现性,在分离分析复杂生物样品方面具有较大的应用前景。此外,本文所发展的方法在制备杂化整体柱的过程中不借助相应的硅烷试剂,为杂化整体柱的制备提供了一种新的思路。

关键词: 蛋白质组分析, 毛细管电色谱, 毛细管液相色谱, 一锅法, 有机-无机杂化, 整体材料

Abstract: A “one-pot” process for the preparation of organic-silica hybrid capillary monolithic column by concurrently using tetramethoxysilane (TMOS), vinyltrimethoxysilane (VTMS) and the organic monomer, N-(2-(methacryloyloxy)ethyl)dimethyl-octadecylammonium bromide (MDOAB), is described. The polycondensation of alkoxysilanes and the copolymerization of MDOAB and VTMS were subsequently carried out within the confines of a capillary under the proper reaction conditions. The performance of the C18-silica hybrid monolithic column was investigated by capillary electrochromatography and capillary liquid chromatography. In addition, the C18-silica hybrid capillary monolithic column was also applied in the analysis of tryptic digests of bovine serum albumin by capillary liquid chromatography/tandem mass spectrometry (CLC-MS/MS) for demonstrating its potential in proteome analysis. This in situ process of incorporating functional groups into silica monolith provides a new way for the preparation of the organic-silica hybrid monolithic column.

Key words: capillary electrochromatography (CEC), capillary liquid chromatography (CLC), one-pot, proteome analysis, monolith, organic-inorganic hybrid