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为建立分子印迹固相萃取-高效液相色谱法检测食品中3种三唑类杀菌剂残留的方法,分别以联苯三唑醇、烯唑醇和腈菌唑为模板分子,α-甲基丙烯酸(MAA)和丙烯酰胺(AM)为功能单体,乙二醇二甲基丙烯酸酯(EDMA)为交联剂,采用本体聚合法合成分子印迹聚合物。将制得的联苯三唑醇、烯唑醇和腈菌唑聚合物按质量比1∶1∶1混合,制成固相萃取柱,用于样品的前处理,采用高效液相色谱法检测。结果表明,联苯三唑醇、烯唑醇和腈菌唑在5 min内实现基线分离。在低和高浓度添加水平下,平均回收率在90.6%~92.7%之间,RSD在1.2%~3.3%之间(n=5),联苯三唑醇的检测限为0.1μg/g,烯唑醇和腈菌唑的检测限为0.2μg/g。该方法分析速度快,灵敏度高,精密度好,适合于同时检测食品中联苯三唑醇、腈菌唑和烯唑醇3种三唑类杀菌剂残留。
To establish a method for the determination of three triazole fungicide residues in food by molecularly imprinted solid-phase extraction and high performance liquid chromatography (HPLC), respectively, and using tribenzotriazole, diniconazole and myclobutanil as template molecules, α-methacrylic acid (MAA) and acrylamide (AM) as functional monomers, and ethylene glycol dimethacrylate (EDMA) as crosslinking agents. The molecularly imprinted polymers were synthesized by bulk polymerization. The prepared biphenyl triadimenol, diniconazole and myclobutanil polymer were mixed at a mass ratio of 1: 1: 1 to prepare a solid phase extraction column for pretreatment of the sample and detected by high performance liquid chromatography. The results showed that the baseline separation of bitertanol, diniconazole and myclobutanil within 5 min. The average recoveries were between 90.6% and 92.7% with RSD between 1.2% and 3.3% (n = 5) at the low and high level of addition, the detection limit of 0.1μg / g for benzotriazole, The detection limit of diniconazole and myclobutanil was 0.2 μg / g. The method has the advantages of fast analysis, high sensitivity and good precision, and is suitable for simultaneous detection of triazole fungicide residues of benzotriazole, myclobutan and diniconazole in food.