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

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3μm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 m^2/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。

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 μ m.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.