无机硅胶-有机聚合物混合基质C_(16)毛细管整体柱的制备和性能研究  

Preparation and Performance of Inorganic Silica Gel-organic Polymer Mixture Based C_(16) Capillary Monolithic Column

作　　者：王园朝[1] 吴琼[1] 金瑛芝[1] 刘金华[1] 

机构地区：[1]杭州师范大学材料与化学化工学院,有机硅化学与材料技术教育部重点实验室,杭州310036

出　　处：《分析化学》2010年第6期828-832,共5页Chinese Journal of Analytical Chemistry

基　　金：浙江省自然科学基金(No.Y406237)资助项目

摘　　要：利用具有双功能基团的3-(三甲氧基硅烷)丙基甲基丙烯酸酯在酸性水溶液中硅氧烷水解缩聚后,再在热引发条件下与甲基丙烯酸十六酯进行双键聚合反应,制备了一类新型的无机硅胶-有机聚合混合基质毛细管电色谱整体柱,实现了硅胶基质整体柱和有机聚合基质整体柱制柱方法合二为一。提出了吸汞法控制溶胶混合溶液引入毛细管适当位置,以获得平整的整体柱固定相界面的简易操作方法。优化了整体柱制备条件,采用扫描电镜和氮吸附比表面仪对整体柱材料的结构特征进行了表征,材料平均比表面积为103.4m2/g,中孔孔径主要分布在3～7nm范围。探讨了运行电压、缓冲液浓度、pH值和有机改性剂含量等因素对电渗流流速的影响。利用制备柱基线分离了7种中性芳香烃类物质。对萘的柱效达54000塔板数/m;连续运行5次的保留时间的RSD为0.9%,容量因子的RSD为0.6%;连续运行3d,保留时间的RSD为1.2%,容量因子的RSD为0.8%;不同批次3支整体柱,保留时间的RSD为8.7%,容量因子的RSD为5.7%。A novel type of inorganic silica gel-organic polymer mixture based capillary monolithic column was prepared using methacryloxypropyltrimethoxysilane hydrolyzing and co-condensation polymerization in the presence of an acid solution, and the product reacted with hexadecyl methacrylcetyl ester by double bond polymerization in the presence of a heat initiator. The method proposed combined of the preparation of silica-based monolithic column with organic polymer-based monolithic column. A technique introducing sol mixture into capillary by suction mercury was carried out to obtain a flat and orderly interface of stationary phase. The influences of running voltage, organic additive, concentration and pH of buffer on electroosmotic flow（EOF） were investigated respectively. The structure and pore size distribution of the monolithic material were characterized by scanning electronmicroscopy and nitrogen adsorption method. The pore size distribution profile of mesopores of the material was around 3-7 nm with average specific surface area of material was 103.4 M2/g. Chromatographic characteristics of the monolithic column prepared with the optimized fabrication condition were studied. Seven neutral hydrocarbon, such as alkylbenzenes and polycyclic aromatic hydrocarbons （PAHs）, were baselinely separated using the mixture based monolithic column. For naphthalene, the separation efficiency of 54000 theoretical plates/m was achieved, the RSD values of retention times and capacity factor were 0.9% and 0.6% for five consecutive runs, 1.2% and 0.8% for day-to-day（n=3）, 8.7% and 5.7% for column-to-column（n=3）, respectively.

关 键 词：整体柱 毛细管电色谱 无机硅胶-有机聚合物混合基质 制备 

分 类 号：O657.8[理学—分析化学]