以衍生化聚硅氧烷为固定相的开管毛细管电色谱柱的研制

建立了一种简单可行的制备衍生化聚硅氧烷开管毛细管电色谱柱的方法,石英毛细管无需浸蚀,直接键合上大分子的聚硅氧烷,用异丁烯酸丁酯和乙烯基磺酸衍生化时对苯的同系物有很好的分离能力,对甲苯柱效可达1.52×10⁵N/m(N为理论塔板数),柱效稳定;当用烯丙基全甲基β-环糊精和乙烯基磺酸衍生化时,石英毛细管先经溶胶-凝胶处理后,所制得的柱子对萘普生对映体的分离度可达0.81.

Preparation and Evaluation of Open Tubular Electrochromatography Column with Derivated Polysiloxane as Stationary Phase

A simple and valid procedure for the preparation of open tubular electrochromatography column with derivated polysiloxane as stationary phase was established. When using polysiloxane derivated with butyl methacrylate and vinylsulfonic acid as stationary phase, the column has a strong ability for separation of the series of benzene. The separation efficiency of tuluene was 1.52×10⁵ theoretical plates/meter and the retention factors of the series of benzene were larger than 2.40 After two months, there was no obvious difference in the separation ability of the column. In this method, the polymer was directly bonded in 50 μm i.d. fused silica capillary without pre etching. When using polysiloxane derivated with allyl-permethyl-β-cyclodextrin and vinylsulfonic acid as chiral stationary phase, naproxen could be enantiomeric separated with resolution of 0.81. In this method, the 50 μm i.d. fuse-silica capillary was primarily treated with Sol-Gel technology to increase the area of inner wall and the density of Si-OH.