[目的]制备3种内吸性农药分子印迹聚合物及固相萃取柱,建立MISPE-LC-MS/MS方法.[方法]应用分子印迹技术制备分子印迹聚合物,通过研究模板分子、功能单体和交联剂的配比关系以及索氏萃取效率,分析该聚合物制备的影响因素;通过吸附试验分析该聚合物特异性;通过研究不同洗脱溶剂、洗脱体积等因素对该萃取柱的使用进行优化,最后通过对黄瓜样品添加回收率测定分析该方法的实用性.[结果]制备出了多目标物特异性分子印迹聚合物,其对嘧菌酯、噻虫啉和吡虫啉具有较高识别能力和快速吸附效果,以此聚合物作为吸附功能原料制备固相萃取柱,建立固相萃取与液质联用检测农药残留的方法.此方法应用在黄瓜的嘧菌酯、噻虫啉和吡虫啉残留检测上,添加回收率在88.5％～94.6％之间,相对标准偏差在1.6％～2.9％之间.[结论]该分子印迹聚合物制备较容易,固相萃取柱前处理过程简单,以其为前处理核心与LC-MS/MS仪器建立的农药残留检测方法特异性较好、检测灵敏度较高,具有一定的实用性.%[Objective] To prepare the three systemic pesticide molecularly imprinted polymers and molecularly imprinted solidphase extraction column,establish the MISPE-LC-MS/MS method.[Methods]The molecular imprinting technique was used to prepare the molecularly imprinted polymers.The factors affecting the preparation of polymers were analyzed through studying the template molecule,ratio of functional monomer to cross-linking agent and Soxhlet extraction efficiency.The adsorption test was performed to analyze the specificity of polymers,the application of extraction column was optimized with studying the different elution solvents or volumes.The fortified recovery in cucumber sample was observed.[Results]The multi-target specific molecularly imprinted polymer was prepared,which was a high recognition capability and rapid adsorption effect on azoxystrobin,thiacloprid and imidacloprid,and this polymer was used as the adsorption raw material to prepare the solid-phase extraction column,and the solid-phase extraction and liquid mass combination method of detecting pesticide residues was established.The recovery by the method was between 88.5 ％ and 94.6 ％,and the relative standard deviation was between 1.6 ％ and 2.9％.[Conclusion] The molecularly imprinted polymer was easily to prepare,the pretreatment process of solid-phase extraction was simple.The specificity and detection sensitivity of the method on pesticide residues with the polymer combined with LC-MS/MS were higher.
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