聚苯乙烯-二乙烯基苯-甲基丙烯酸甲酯固相萃取填料的制备及其应用

Preparation and application of polystyrene-divinylbenzene-methyl methacrylate solid phase extraction packing

以苯乙烯、甲基丙烯酸甲酯为单体,二乙烯基苯为交联剂,偶氮二异丁腈为引发剂,在乙腈溶剂中采用回流沉淀法制备单分散的聚苯乙烯-二乙烯基苯-甲基丙烯酸甲酯微球.考察单体体积分数、引发剂用量、交联剂体积分数以及反应时间对聚合物微球粒径大小及形貌的影响.采用红外光谱和扫描电镜对微球官能团种类、形貌及粒径大小进行了表征,确定了合成微球的最佳条件.以聚苯乙烯-二乙烯基苯-甲基丙烯酸甲酯微球为固相萃取填料,对茶叶中的甲氰菊酯进行吸附,利用超高效液相色谱对其含量进行测定.在质量浓度为0.05~5 mg/mL范围内,甲氰菊酯的峰面积与质量浓度呈良好的线性关系,相关系数(R^2)为0.999 9;检出限为0.05 mg/L.

Using styrene and methyl methacrylate as monomers,divinylbenzene as a cross-linker,azobisisobutyronitrile as an initiator,monodisperse polystyrene-divinylbenzene-methyl-methacrylate microsphere(P(St-co-DVBco-MMA))was prepared by distillation precipitation method.The effect of the monomer volume fraction,the amount of initiator,the cross-linker volume fraction,and the reaction time on the size and morphology of the polymer microspheres was investigated.FT-IR and scanning electron microscopy(SEM)were used to characterize the type of the functional groups,morphology and particle size of microspheres.P(St-co-DVB-co-MMA)was used as the solid-phase extraction filler for adsorbing fenpropathrin in tea and the content was determined by ultra-performance liquid chromatography(UPLC).In the range of 0.05~5 mg/mL,the peak area and concentration of fenpropathrin showed a good linear relationship,and the correlation coefficient(R2)was 0.999 9.The detection limit of the method was 0.05 mg/L.