超高效液相色谱-串联质谱法分析氟虫双酰胺在稻田生态系统中的消解动态

Residue decline study of flubendiamide in rice ecosyetem by UPLC-MS/MS

应用超高效液相色谱-串联质谱(UPLC-MS/MS)建立了氟虫双酰胺(NNI-0001)及其代谢产物(NNI-des)在土壤和田水中的残留检测方法。样品采用乙腈提取,乙二胺-N-丙基硅烷吸附剂(PSA)净化,UPLC-MS/MS检测。氟虫双酰胺及其代谢产物NNI-des在土壤和田水中的最低检测浓度分别为0.002 mg/kg和0.001 mg/L,最小检出量分别为1.2×10-13和3.1×10-14 g。在土壤和田水中的添加水平为0.001～1 mg/kg(mg/L)条件下,氟虫双酰胺及其代谢产物NNI-des的平均回收率在78.2%～108.2%之间,相对标准偏差在8.2%～15.3%之间。消解动态试验结果表明,氟虫双酰胺在土壤和田水中的半衰期分别为1.0和5.4 d。施药21 d后,消解率均在85%以上,属易降解农药。

A method had been developed to determine flubendiamide（NNI-0001） and its metabolite（NNI-des）residues in soil and water.The samples were extracted by acetonitrile,followed by clean-up on PSA cartridge and analyzed by UPLC-MS/MS.The limit of detection of flubendiamide and its metabolite in soil and water were 0.002 mg/kg and 0.001 mg/L,respectively.The limit of detection was 1.2×10-13 g for flubendiamide and 3.1×10-14 g for NNI-des.External reference method was used for quantitative determination.When the concentration of flubendiamide and its metabolite NNI-des was quantitative from 0.001 to 1 mg/kg（mg/L）,the average recoveries varied from 78.2% to 108.2% with the coefficient of variation of 8.2%-15.3%,respectively.The study indicated that the half-life of flubendiamide in soil and water was 1.0 days and 5.4 days.The rate of decline exceeded 85% 21 days after application.Flubendiamide belongs to the easily degradable pesticide.