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采用溶胶-凝胶法,以四乙氧基硅烷和苯基三乙氧基硅烷作为反应单体,通过酸碱两步催化在毛细管中进行原位缩聚反应,制备了新型有机-无机杂化硅胶基质毛细管整体柱,制备过程简单。整体柱基质中均匀分布的苯基基团可直接用于反相毛细管电色谱的分离,因而不需要对基质再进行衍生化。优化了整体柱的制备条件,采用扫描电镜和压汞法对整体柱的微观结构和孔径分布进行了表征。分别考察了溶胶-凝胶初始反应液中水的用量对柱床结构的影响和两种单体的配比对材料孔径分布的影响。研究了稠环芳烃类化合物在整体柱上的保留行为,用所制备的整体柱分离了7种苯酚类化合物,平均柱效达100 000塔板/m。
A novel organic-inorganic hybrid silica gel was prepared by the sol-gel method using tetraethoxysilane and phenyltriethoxysilane as the reaction monomers and the in-situ polycondensation reaction in the capillary by acid-base two-step catalysis. Matrix capillary monolithic column, the preparation process is simple. Phenyl groups homogeneously distributed throughout the monolith matrix can be used directly for the separation of reversed-phase capillary electrochromatography and thus do not require further derivatization of the matrix. The preparation conditions of monolithic column were optimized. The microstructure and pore size distribution of the monolithic column were characterized by scanning electron microscopy and mercury intrusion porosimetry. The effects of the amount of water in the initial reaction solution of sol-gel on the bed structure and the ratio of two kinds of monomers on the pore size distribution were investigated. The retention behavior of condensed aromatic hydrocarbons on monolithic columns was studied. Seven kinds of phenolic compounds were isolated from the prepared monolithic columns with an average column efficiency of 100 000 plates / m.