以苯乙烯、二乙烯苯和甲基丙烯酸为原料,聚乙烯醇为分散剂,过氧化苯甲酰为引发剂,采用悬浮聚合法制备了具有亲脂和弱阳离子交换性能的球形固相萃取填料,并确定了最佳的聚合反应条件。采用红外光谱和扫描电子显微镜表征了聚合物结构和微球的形貌,通过氮气吸附法测定了填料的比表面积和孔径分布。以氰草津、西玛津、阿特拉津和特丁津4种三嗪类除草剂为目标化合物,通过固相萃取-液相色谱联用技术,考察了样品溶液的酸度、过柱流量及洗脱剂的体积对萃取回收率的影响,确定了最佳固相萃取条件。测定了制备的固相萃取填料的吸附容量和小柱的穿透体积。氰草津、西玛津、阿特拉津和特丁津的检出限分别为0.26,0.63,0.42,0.31 μg·L-1。

The polymer microspheres with lipotropy and weak cation exchange performance, for using as filler in solid phase extraction, were prepared through suspension polymerization method using styrene, divinyl benzene and methyl acrylate as monomers, PVA as dispersant, benzoyl peroxide as the initiator, and the optimum polymerization conditions were defined. The structure and morphology of the polymer microspheres were characterized by IR and SEM, and the specific surface area and pore size distribution of the polymer microspheres was examined by nitrogen adsorption method. With four kinds of triazine herbicides (cyanazine, simazine, atrazine and terbuthylazine) as target compounds, the influence of the acidity of the sample solution, the volume of eluant and the velocity of flow on extraction rate were investigated by the means of solid phase extraction-liquid chromatography technology, and the optimum conditions for solid phase extraction were determined. The adsorption capacity and penetration volume of SPE colunm were determind. The detection limits of cyanazine, simazine, atrazine and terbuthylazine were 0.26, 0.63, 0.42, 0.31 μg·L-1, respectively.