分散固相萃取-超高效液相色谱-串联质谱法测定农产品中螺虫乙酯及其3种代谢产物残留量

Determination of spirotetramat and its 3 metabolites in agriculture products by ultra performance liquid chromatography-tandem mass spectrometry combined with dispersive solid phase extraction

目的建立农产品中螺虫乙酯及其3种代谢产物的超高效液相色谱-串联质谱检测方法。方法样品经乙腈涡旋提取,采用乙二胺-N-丙基硅烷(primary secondary amine,PSA)和HC-C_(18)分散固相萃取剂净化,经超高效液相色谱串联质谱仪多反应监测模式检测,外标法定量。结果螺虫乙酯及其3种代谢产物在0.1~100μg/L质量浓度范围内与其呈良好的线性关系(r^2>0.999),检出限为0.1μg/kg,螺虫乙酯代谢产物S1定量限为1.0μg/kg,其余为0.2μg/kg,在添加水平为1.0、25、50μg/kg时,平均回收率为82.5%~99.1%,测定结果的相对标准偏差为1.3%~8.4%(n=6)。结论该方法简单、快速,重复性好,灵敏度和准确度均能满足农产品中螺虫乙酯残留量的测定。

Objective To develop a method for the determination of spirotetramat and its 3 metabolites in agriculture products by ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） combined with dispersive solid phase extraction.Methods The samples were extracted with acetonitrile,cleaned up by a mixture of primary secondary amine（PSA） and HC-C18 sorbents,and then detected by UPLC-MS/MS with multiple reaction monitoring mode,and quantified by external standard method.Results Spirotetramat and its 3 metabolites showed good linearities in the range of 0.1-100 μg/L,and the correlation coefficients were more then 0.999.The limits of detection were 0.1 μg/kg for spirotetramat and its 3 metabolites.The limit of quantitative of S1 for metabolite of spirotetramat was 1.0 μg/kg while the rests were 0.2 μg/kg.The average recoveries were in the range of 82.5%-99.1% at the spiked levels of 1.0,25,and 50 μg/kg,and the relative standard deviations（RSDs） were 1.3%-8.4%（n=6）.Conclusion The method is simple,rapid,accurate,reproducible,sensitive and accurate,which can be used to determine the residue of spirotetramat in agricultural products.