基于超高效液相色谱-串联质谱的稻田环酰菌胺和噻酰菌胺残留量检测

采用超高效液相色谱-串联质谱(UPLC-MS/MS)建立了环酰菌胺和噻酰菌胺在稻田生态系统中的残留检测方法。样品经乙腈提取,N-丙基乙二胺吸附剂(PSA)净化(稻秆和稻壳样品添加石墨化碳黑(GCB)辅助净化),UPLC-MS/MS测定,基质外标法(ESTD)定量。稻田土、稻田水、稻米、稻壳和稻秆五种基质中环酰菌胺和噻酰菌胺的添加浓度在0.005~2 mg/kg时,平均回收率均为81.9%~107.6%,相对标准偏差为1.4%~9.6%,检出限(LOD)是0.019~0.061μg/kg,定量限(LOQ)是5μg/kg。结果表明本方法灵敏度高、定量准确、测定浓度范围宽,且操作简便;可用于稻田生态系统中同时对环酰菌胺和噻酰菌胺进行残留检测分析。

Determination of Fenhexamid and Tiadinil Residues in Rice Fielde Ecosystem by UPLC-MS/MS

A method for determination of fenhexamid and tiadinil residues in rice field ecosystem was estab-lished based on ultraperformance liquid chromatography-mass spectrometry（ UPLC-MS/MS） . The samples were extracted by acetonitrile and then purified by primary secondary amine （ PSA） and graphitized carbon black （ GCB） . The fenhexamid and tiadinil residues were analyzed by UPLC-MS/MS under multiple reac-tion monitoring mode and quantified with matrix-match external standards. Average recoveries of fenhexamid and tiadinil in rice at three levels （0. 005, 0. 05, 0. 5, 1 and 2 mg/kg） ranged from 81. 9% to 107. 6% with relative standard deviations from 1 . 4% to 9 . 6%. Limits of detections for fenhexamid and tiadinil were 0 . 019~0. 061 μg/kg,while limits of quantifications were 5 μg/kg. The method is simple, rapid, and accurate, and it can meet the requirements of the domestic and international legislation. The method may adapt to detect residues of fenhexamid and tiadinil residues in rice field ecosystem.