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建立了基于分子印迹聚合物(MIPs)为固相萃取填料的固相萃取技术结合超高效液相色谱串联质谱法(MISPE-UPLC-MS/MS)检测猪肉中磺胺二甲氧嗪。以磺胺二甲氧嗪为模板分子,三氟甲基丙烯酸为功能单体,采用沉淀聚合法制备了分子印迹固相萃取填料,并对萃取净化条件进行了优化。在优化的提取条件和分析条件下,对猪肉肌肉样品中磺胺二甲氧嗪进行分析,其检出限为1.225μg/kg;定量限为4.083μg/kg;双水平回收率在81.4%~106.9%;RSD为3.7%和12%。与M CX柱净化相比,分子印迹固相萃取柱能够有效去除基质效应,分离待测物与杂质。
The detection of sulfamethazine in pork by solid phase extraction (SPE) coupled with MIPs (solid-phase extraction) and ultra-high performance liquid chromatography tandem mass spectrometry (MISPE-UPLC-MS / MS) Using sulfadimethoxine as the template molecule and trifluoromethacrylate as the functional monomer, the molecularly imprinted solid-phase extraction packing was prepared by precipitation polymerization method, and the extraction and purification conditions were optimized. Under the optimal conditions of extraction and analysis, the detection limit of sulfadimethoxine in pork muscle samples was 1.225μg / kg, the limit of quantification was 4.083μg / kg, and the bi-level recoveries ranged from 81.4% to 106.9 %; RSD 3.7% and 12%. Compared with the M CX column purification, molecularly imprinted SPE columns can effectively remove matrix effects and separate analytes and impurities.