乙烯基功能化聚甲基倍半硅氧烷色谱填料的制备与评价

Preparation and evaluation of vinyl-functionalized polymethylsilsesquioxane chromatography stationary phase

以乙烯基三甲氧基硅烷(VTMS)和甲基三甲氧基硅烷(MTMS)为前体,通过酸碱催化水解共缩聚的方法制备得到单分散多孔乙烯基功能化聚甲基倍半硅氧烷(V-PMSQ)微球。当前体混合物中VTMS的摩尔分数从0增加到100%时,微球的比表面,孔容和孔径均单调减小,孔隙率从65%降低至12%。微球的碳含量在16.6%~25.7%的范围内,与十八烷基键合硅胶填料相当。在进行色谱评价时,碱性药物阿米替林表现出对称的峰型,表明微球的硅羟基活性较低。在高p H流动相的条件下,30%和50%VTMS含量的填料可以实现4种碱性药物的基线分离。具有较大p H使用范围的乙烯基功能化聚甲基倍半硅氧烷色谱填料在分离碱性化合物方面具有较大的优势。

The monodispersed porous vinyl-functionalized polymethylsilsesquioxane （V-PMSQ） microspheres were prepared by acid-base catalytic hydrolysis and co-condensation of vinyltrimethoxylsilane （ VTMS ） and methyltrimethoxylsilane （ MTMS ） precursors. With VTMS increased from 0 to 100% in the precursor mixture, the surface area, pore volume and pore size all decreased monotonically with porosity reduced from 65% to 12%. The carbon contents were in the range from 16. 6% to 25.7%, comparable to those typical for octadecyl bonded silica packings. Symmetric peaks were observed for basic drug amitriptyline used in a column evaluation procedure, confirming reduced silanol activity of these materials. Baseline separations of four basic pharmaceuticals were achieved on packings with 30% and 50% VTMS with high pH mobile phases. It could be seen that vinyl-functionalized organosilica packings with broad usable pH range had a greater advantage in basic compounds separation.