聚苯乙烯磺酸钠/氧化锆固相萃取填料的制备及其在农药残留萃取分析中的应用  

Preparation of solid phase extraction packing of poly (sodium styrene sulfonate )/zirconia and its application in the extraction analysis of pesticide residues

作　　者：隋丽丽[1] 隋崴崴[2] 肖晓杏[1] 

机构地区：[1]齐齐哈尔大学化学与化学工程学院,齐齐哈尔161006 [2]河北农业大学海洋学院,秦皇岛066003

出　　处：《分析试验室》2013年第8期11-15,共5页Chinese Journal of Analysis Laboratory

基　　金：黑龙江省自然科学基金项目(B201101);齐齐哈尔大学青年教师科研启动计划项目(060033)资助

摘　　要：采用聚合诱导胶体凝聚法(PICA)制备了ZrO2微球,用钛酸酯偶联剂对微球表面进行改性,再以苯乙烯、二乙烯基苯、苯乙烯磺酸钠,在引发剂偶氮二异丁腈(AIBN)作用下与ZrO2微球表面双键进行聚合,制备了聚苯乙烯磺酸钠/氧化锆固相萃取填料。采用FT-IR、SEM/EDS及N2吸附脱附等手段表征了合成材料的组成与结构。将固相萃取与高效液相色谱联用,测定了除草剂莠去津、异丙甲草胺和二甲戊乐灵。实验结果表明:莠去津、异丙甲草胺和二甲戊乐灵萃取的色谱峰面积与浓度的线性关系良好,相关系数(R2)分别为0.9965,0.9918,0.9934,检出限分别为0.0053,0.0042,0.0084 mg/L。Zirconia microspheres were prepared by the method of PICA.The surfaces of zirconia microspheres were modified by the use of titanate coupling agent.Zirconia microspheres cross-linked polymerized with phenyl ethylene,divinyl benzene and sodium styrene sulfonate,in which AIBN was used as an initiator.The solid phase extraction packing of poly（sodium styrene sulfonate）/zirconia was prepared.The composition and structure of the material were characterized by FT-IR,SEM/EDS and N2 adsorption-desorption.By means of SPE combined with HPLC,the contents of atrazine,metolachlor and pendimethalin in water were determined.The experiment results indicated that the chromatographic peak areas and concentrations of extracted atrazine,metolachlor,pendimethalin had good linearties and the correlation coefficients（R2） were 0.9965,0.9918,and 0.9934.The minimum detection limits for them were 0.0053 mg/L,0.0042 mg/L and 0.0084 mg/L respectively.

关 键 词：固相萃取填料 高效液相色谱 莠去津 异丙甲草胺 二甲戊乐灵 

分 类 号：O657.7[理学—分析化学]