模板法制备大孔硅胶微球及其在高效液相色谱蛋白质分离中的应用

doi:10.3724/SP.J.1123.2017.03018

色谱 ›› 2017, Vol. 35 ›› Issue (6): 565-571.DOI: 10.3724/SP.J.1123.2017.03018

模板法制备大孔硅胶微球及其在高效液相色谱蛋白质分离中的应用

牛梦娜, 马红彦, 胡飞, 王世革, 刘璐, 常海洲, 黄明贤

上海理工大学理学院化学系, 上海 200093

收稿日期:2017-03-17 出版日期:2017-06-08 发布日期:2013-09-29
通讯作者: 黄明贤,E-mail:hmx@usst.edu.cn.
基金资助:
上海市科委项目（14440502300）；上海理工大学沪江基金（D15011）.

Preparation of large-pore silica microspheres using templating method and their applications to protein separation with high performance liquid chromatography

NIU Mengna, MA Hongyan, HU Fei, WANG Shige, LIU Lu, CHANG Haizhou, HUANG Mingxian

Department of Chemistry, College of Science, University of Shanghai for Science and Technology, Shanghai 200093, China

Received:2017-03-17 Online:2017-06-08 Published:2013-09-29
Supported by:
Science and Technology Commission of Shanghai Municipality Project (No. 14440502300); Foundation of Hujiang from University of Shanghai for Science and Technology (No. D15011).

摘要/Abstract

摘要：

以弱阳离子交换聚合物微球（WCX）为模板、N-三甲氧基硅基丙基-N，N，N-三甲基氯化铵（TMSPTMA）为结构导向剂、四乙氧基硅烷（TEOS）为硅胶前驱体，在三乙醇胺弱碱催化作用下，水解缩合形成有机聚合物与二氧化硅复合微球，将此复合微球煅烧后得到大孔二氧化硅微球。探索了不同反应条件对二氧化硅微球的形貌、表面结构和分散性的影响；当TMSPTMA、TEOS与三乙醇胺的体积比为1：2：2时可以得到孔径在50~150 nm之间、粒径在2 μm左右的硅胶微球。对所制备的大孔硅胶微球表面进行C18（十八烷基二甲基氯硅烷）键合修饰，然后将键合的填料装填到50 mm×4.6 mm的色谱柱中，考察了其对常见的几种标准蛋白质和市售大豆分离蛋白质的分离效果，结果显示这种填料在高效液相色谱蛋白质分离中具有一定的潜力。

关键词: 大孔二氧化硅微球, 蛋白质分离, 高效液相色谱, 结构导向剂, 模板法

Abstract:

Large-pore silica microspheres were synthesized by utilizing weak cation exchange polymer beads as templates, N-trimethoxysilylpropyl-N,N,N-trimethylammonium chloride (TMSPTMA) as a structure-directing agent, tetraethoxysilane (TEOS) as a silica precursor, and triethanolamine as a weak base catalyst. The hydrolysis and condensation of the silica precursors occurred inside the templating polymer beads yielded polymer/silica composite microspheres. After the organic polymer templates were removed in the calcination step, large-pore silica microspheres were produced. The effects of different reaction conditions on the morphology, structure and dispersibility of the formed silica microspheres were investigated. It has been shown that when the volume ratio of TMSPTMA, TEOS and triethanolamine was 1:2:2, silica microspheres with pore size range of 50-150 nm and particle size around 2 μm were obtained. The as-prepared silica microspheres were then bonded with chlorodimethyloctadecylsilane (C18), packed into a 50 mm×4.6 mm column, and evaluated for the separations of some common standard proteins and soybean isolation proteins. The results showed that the large-pore silica spheres from this work have potentials for protein separation in HPLC.

Key words: high performance liquid chromatography (HPLC), large-pore silica microspheres, protein separation, structure-directing agent, templating method

中图分类号:

O658

牛梦娜, 马红彦, 胡飞, 王世革, 刘璐, 常海洲, 黄明贤. 模板法制备大孔硅胶微球及其在高效液相色谱蛋白质分离中的应用[J]. 色谱, 2017, 35(6): 565-571.

NIU Mengna, MA Hongyan, HU Fei, WANG Shige, LIU Lu, CHANG Haizhou, HUANG Mingxian. Preparation of large-pore silica microspheres using templating method and their applications to protein separation with high performance liquid chromatography[J]. Chinese Journal of Chromatography, 2017, 35(6): 565-571.

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模板法制备大孔硅胶微球及其在高效液相色谱蛋白质分离中的应用

Preparation of large-pore silica microspheres using templating method and their applications to protein separation with high performance liquid chromatography

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