Abstract: 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.