以阿散酸为虚拟模板分子,2-乙烯吡啶为功能单体,乙二醇二甲基丙烯酸酯为交联剂,合成了对洛克沙胂具有高选择性的分子印迹聚合物。通过考察致孔剂、单体及交联剂等因素对合成聚合物性能的影响,获得优化聚合配方为:阿散酸、2-乙烯吡啶、乙二醇二甲基丙烯酸酯、甲醇-乙腈(1∶1,V/V)及偶氮二异丁腈之比为1 mmol∶4 mmol∶20 mmol∶6 mL∶60 mg。合成印迹聚合物对洛克沙胂的最大吸附量为0.93 mg/g,作为固相萃取填料分离、富集洛克沙胂的优化萃取条件为:水和乙腈活化平衡,乙腈上样,水和甲醇依次淋洗,5%甲酸甲醇溶液洗脱。洛克沙胂在分子印迹固相萃取柱上的回收率达到95%以上,而非分子印迹固相萃取柱的回收率仅为43.1%。制备小柱应用于池塘水中洛克沙胂的净化富集,检测限可达0.05 mg/L。
Molecularly imprinted polymers(MIP) with high selectivity to roxarsone(ROX) were prepared using arsanilic acid(ASA) as dummy template,2-Vinylpyridine(2-VP) as monomer,ethylene glycol dimethacrylate(EGDMA) as cross-linker.The effects of porogen,monomer and cross-linker on the recognition capability of MIP were investigated.The optimal ratio of ASA,2-VP,EGDMA,methanol-acetonitrile(1 ∶ 1,V/V) and azobisisobutyronitrile was 1 mmol ∶ 4 mmol ∶ 20 mmol ∶ 6 mL ∶ 60 mg,respectively.The maximum adsorption of MIP to ROX was 0.93 mg/g.The optimal conditions of solid phase extraction of MIP as adsorptive material for selective extraction and enrichment of ROX were: conditioning with water and acetonitrile,loading ROX in acetonitrile,washing with water and methanol,and eluting with methanol-formic acid(95 ∶ 5,V/V).The recovery of ROX on MIP cartridge was above 95% and that on NIP cartridge was only 43.1%.The prepared MIP cartridge was applied to extract and enrich ROX in pond water,and the limit of detection of ROX was 0.05 mg/L.