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[目的]建立同时测定西瓜和土壤中戊唑醇、肟菌酯及代谢物肟菌酸残留量的超高效液相色谱串联质谱法(UPLC-MS/MS)。[方法]样品中的待测农药组分采用乙腈-水(体积比4∶1)提取,硅藻土液液萃取小柱净化,采用UPLC-MS/MS法,ESI(+)电离方式,多反应监测(MRM)定量测定。[结果]仪器最低检测量为戊唑醇5.0×10-13g,肟菌酯4.0×10-13g,肟菌酸2.5×10-13g;3种农药的最低检出质量分数均为0.02 mg/kg,在西瓜和土壤中的添加回收率为81.8%~94.2%,变异系数为3.67%~7.04%。[结论]该方法快速、准确、灵敏度高,适合西瓜与土壤样品中戊唑醇、肟菌酯及肟菌酸的残留量测定。
[Objective] The research aimed to establish a simultaneous determination of tebuconazole, trifloxystrobin and trifloxystrobin in watermelon and soil using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). [Method] The pesticide components in the sample were extracted with acetonitrile-water (4: 1 by volume) and cleaned up by liquid-liquid extraction with celite. The UPLC-MS / MS and ESI Response Monitoring (MRM) Quantitation. [Result] The lowest detection limit of the instrument was 5.0 × 10-13g of tebuconazole, 4.0 × 10-13g of trifloxystrobin and 2.5 × 10-13g of trifloxystrobin. The minimum detectable mass fraction of the three pesticides was 0.02 mg / kg , The recoveries of watermelon and soil were 81.8% ~ 94.2%, and the coefficients of variation were 3.67% ~ 7.04%. [Conclusion] The method was rapid, accurate and sensitive and suitable for the determination of tebuconazole, trifloxystrobin and triflumuron in watermelon and soil samples.