霍佳楠,刘欣雨,焦 逊,郑清林.有机磷分子印迹聚合物的制备及其吸附性能评价[J].食品安全质量检测学报,2022,13(3):933-940 |
有机磷分子印迹聚合物的制备及其吸附性能评价 |
Preparation of organophosphorus molecularly imprinted polymers and evaluation of its adsorption performance |
投稿时间:2021-09-09 修订日期:2021-11-08 |
DOI: |
中文关键词: 有机磷 分子印迹聚合物 虚拟模板 农药残留 吸附性能 |
英文关键词:organophosphorus molecularly imprinted polymers virtual template pesticide residues adsorption performance |
基金项目:国家级大学生科研与创新创业项目(G038)、北京工商大学2020年度青年教师科研启动基金项目(QNJJ2020-10) |
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中文摘要: |
目的 制备出有机磷类分子印迹聚合物(molecular imprinted polymers, MIPs)并对其进行吸附性能评价。方法 选用氯代磷酸二苯酯为虚拟模板、以甲基丙烯酸(methacrylic acid, MAA)为功能单体、三羟甲基丙烷三甲基丙烯酸酯(trimethylolpropane trimethacrylate, TMPTMA)为交联剂, 通过沉淀聚合法制备有机磷类农药的分子印迹聚合物, 经过优化合成体系得到最优的MIPs。采用扫描电镜对MIPs进行结构表征, 利用平衡吸附实验对MIPs的吸附性能进行评价。最后将合成的MIPs制备成固相萃取(solid phase extraction, SPE)柱进行样品前处理, 采取氯唑磷作为目标吸附物, 对白菜中氯唑磷残留进行回收率评价实验。结果 有机磷类农药的MIPs最佳合成体系条件为: 模板分子(氯代磷酸二苯酯):功能单体(MAA):交联剂(TMPTMA)的摩尔比为1:3:4、反应温度为60 ℃、引发剂用量为30 mg; 所合成的MIPs能够吸附5种目标有机磷农药, 最大表观结合量达到10.76 mg/g。制备成SPE小柱进行白菜中氯唑磷残留的前处理, 回收率在73%~105%之间, 精密度为7.76%~9.55%。结论 所制备的印迹材料对有机磷类农药具有良好的吸附性能, 可以实现对有机磷类农药的特异吸附。 |
英文摘要: |
Objective To prepare organophosphorus molecular imprinted polymers (MIPs) based on molecular imprinting technology and evaluate its adsorption performance. Methods The molecularly imprinted polymers of organophosphorus pesticides were prepared by precipitation polymerization with diphenyl chlorophosphate as virtual template, methacrylic acid (MAA) as functional monomer and trimethylolpropane trimethylacrylate (TMPTMA) as crosslinking agent. The optimal MIPs were obtained by optimizing the synthesis system. The structure of MIPs was characterized by scanning electron microscope, and the adsorption performance of MIPs was evaluated by equilibrium adsorption experiment. Finally, the synthesized MIPs were prepared into a solid phase extraction (SPE) column for sample pretreatment. Chlorzofos was used as the target adsorbent to evaluate the recovery of chlorzofos residue in Chinese cabbage. Results The optimum synthesis conditions of MIPs for organophosphorus pesticides were as follows: The molar ratio of template molecule (phosphate chloride diphenyl ester), functional monomer (MAA) and cross-linking agent (TMPTMA) was 1:3:4, the reaction temperature was 60 ℃, and the dosage of initiator was 30 mg. The MIPs could adsorb 5 kinds of target organophosphorus pesticides, and the maximum apparent binding amount reached 10.76 mg/g. The SPE column was prepared for the pretreatment of chlorazophos residues in Chinese cabbage. The recoveries were 73%?105%, and the precisions were 7.76%?9.55%. Conclusion The imprinted material has good adsorption performance for organophosphorus pesticides, and can realize the specific adsorption of organophosphorus pesticides. |
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