杂化硅胶整体材料研磨法制备混合型高效液相色谱固定相

doi:10.3724/SP.J.1123.2018.11040

色谱 ›› 2019, Vol. 37 ›› Issue (5): 484-490.DOI: 10.3724/SP.J.1123.2018.11040

杂化硅胶整体材料研磨法制备混合型高效液相色谱固定相

王照地, 张璐, 郭丙倩, 王世革, 黄明贤

上海理工大学理学院化学系, 上海 200093

收稿日期:2018-11-28 出版日期:2019-05-08 发布日期:2015-03-23
通讯作者: 黄明贤,Tel:(021)65710384,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 mixed-mode stationary phase for high performance liquid chromatography with ground hybrid silica monolithic material

WANG Zhaodi, ZHANG Lu, GUO Bingqian, WANG Shige, HUANG Mingxian

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

Received:2018-11-28 Online:2019-05-08 Published:2015-03-23
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：

以聚乙二醇（PEG）为致孔剂，四甲氧基硅烷（TMOS）和乙烯基三甲氧基硅烷（VTMS）为杂化硅胶前驱体，在乙酸催化作用下使硅烷发生水解，在尿素加热分解提供的碱性环境下水解的硅烷进一步缩聚得到杂化硅胶整体材料。将此整体材料用球磨机研磨，然后用三羟甲基氨基甲烷处理，并洗涤干燥得到粒径为3 μm左右的硅胶颗粒。探索了不同反应条件对硅胶颗粒的大小、比表面积和孔径、表面形貌和分散性的影响；当TMOS和VTMS体积比为3：1时可以得到孔径为7.5 nm和比表面积为245 m²/g的硅胶颗粒。通过对所制得的硅胶颗粒表面进行C18（十八烷基二甲基氯硅烷）键合修饰和巯基-烯点击反应，得到混合型高效液相色谱固定相。对此固定相的测试结果表明以上硅胶色谱填料的制备方法具有一定的实用性。

关键词: 硅胶整体材料, 混合型固定相, 键合固定相, 巯基-烯点击反应

Abstract:

With polyethylene glycol as a porogen, vinyltrimethoxysilane (VTMS) and tetramethoxysilane (TMOS) as silica precursors, a hybrid silica monolithic material was obtained under the catalysis of acetic acid and thermally decomposed urea. The silica monolithic material was ground by a ballmill, treated with tris(hydroxymethyl)aminomethane (Tris), then washed and dried to obtain silica particles with particle size~3 μm. The effects of different reaction conditions on the particle size, surface morphology and dispersibility of silica particles were investigated. When the volume ratio of TMOS to VTMS was 3:1, it was observed that silica particles with a pore diameter of 7.5 nm and a specific surface area of 245 m²/g were obtained. The resultant silica particles were modified by binding with chlorodimethyloctadecylsilane (C18) and by the thiol-ene click reaction to obtain a mixed-mode type stationary phase. The test results showed that the silica packing materials prepared in this work has certain applicability.

Key words: bonded stationary phase, mixed-mode stationary phase, silica monolith material, thiol-ene click reaction

中图分类号:

O658

王照地, 张璐, 郭丙倩, 王世革, 黄明贤. 杂化硅胶整体材料研磨法制备混合型高效液相色谱固定相[J]. 色谱, 2019, 37(5): 484-490.

WANG Zhaodi, ZHANG Lu, GUO Bingqian, WANG Shige, HUANG Mingxian. Preparation of mixed-mode stationary phase for high performance liquid chromatography with ground hybrid silica monolithic material[J]. Chinese Journal of Chromatography, 2019, 37(5): 484-490.

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杂化硅胶整体材料研磨法制备混合型高效液相色谱固定相

Preparation of mixed-mode stationary phase for high performance liquid chromatography with ground hybrid silica monolithic material

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