“一锅法”制备C18-硅胶杂化毛细管整体柱及其应用  

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

作　　者：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] 

机构地区：[1]中国科学院分离分析化学重点实验室、中网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

出　　处：《色谱》2011年第9期830-836,共7页Chinese Journal of Chromatography

基　　金：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)

摘　　要：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。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.

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

分 类 号：O658[理学—分析化学]