一种新型萃取柱的制备及在盐酸克伦特罗富集中的应用研究

A strong cation-exchange polymer silica-Microspheres-encapsulated monolithic column for microextraction

利用3-磺酸丙基甲基丙烯酸酯钾盐为单体,乙二醇二甲基丙烯酸酯为交联剂,正丙醇、1,4-丁二醇和水为三元致孔剂,通过在装满硅球的250μm内径的石英毛细管内原位聚合制备了1种强阳离子交换有机聚合物包覆硅球整体柱.通过对单体总浓度、聚合反应温度和聚合反应时间的调节来控制有机聚合物对硅球的包覆,确定了整体柱的最佳制备条件.最佳条件:单体总浓度T=30%,C=50%;反应温度60℃;反应时间3h.在优化了影响萃取效率的参数(洗脱液组成,萃取柱的吸附容量,进样速度,样品的pH)后,测得该整体柱对盐酸克伦特罗的富集倍率高达535.

A strong cation-exchange polymer silica-microspheres-encapsulated monolithic column was prepared by in-situ polymerization of 3-sulfopropyl methacrylate potassium salt and ethylene dime- thacrylate in the presence of ternary porogens consisting of n-propanol,l,4-butanediol and water in a 250μm i. d. fused silica capillary prepacked with silica-microspheres for microextraction. The total concentration of the monomers, temperature and time were investigated, and the optimal conditions for preparation of the column were established. The optimized concentration, temperature and time are T=30% （C=50%）,60℃ and 3 h,respectively. After several parameters including composition of desorption solution, adsorption capacity of extraction column, sample flow rate and pH value of the sample matrix were optimized, an about 500 times high enhancement factor was obtained.