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2μm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。
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.Af^er 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 was1:2:2,silica microspheres with pore size range of50-150nm and particle size around2^m were obtained.The as-prepared silica microspheres were then bonded with chlorodimethyloctadecylsilane(C18),packed into a50mmx4.6mm 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.
作者
牛梦娜
马红彦
胡飞
王世革
刘璐
常海洲
黄明贤
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)
出处
《色谱》
CAS
CSCD
北大核心
2017年第6期565-571,共7页
Chinese Journal of Chromatography
基金
上海市科委项目(14440502300)
上海理工大学沪江基金(D15011)~~
关键词
模板法
结构导向剂
大孔二氧化硅微球
高效液相色谱
蛋白质分离
templating method
structure-directing agent
large-pore silica microspheres
high performance liquid chromatography (HPLC)
protein separation