[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0.02mg/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。
[Aims] A method was developed for the simultaneous determination of tebuconazole, trifloxystrobin and its metabolite trifloxystrobin acid in watermelon and soil by ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) detection. [Methods] The pesticides were extracted using mixed solvent of acetonitrile and water (4 : 1, by vol), and were separated and purified with column of diatomite liquid liquid phase extraction. The pesticides were finally detected by UPLC-MS/MS-ESI(+), quantified with multiple reaction monitoring(MRM) mode. [Results] The limit of detection (LOD) was 5.0×10^-13g for tebuconazole, 4.0×10^-13g for trifloxystrobin, 2.5×10^-13 g for trifloxystrobin acid, while the quantification limit (LOQ) was 0.02 mg/kg for three compounds. The average recoveries of tebuconazole, trifloxystrobin and trifloxystrobin acid were 81.8-94.2%, with relative standard deviation (RSD) of 3.67-7.04% in watermelon and soil. [Conclusions] It is an effective method which attained the pesticide residue analysis demands in sensitivity, accuracy and precision for detecting residues of tebuconazole, trifloxystrobin and trifloxystrobin acid in watermelon and soil.