CAJ | 학술논문

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。
채용초고효액상색보-천련질보( UPLC-MS/MS)건립료배선균알화새선균알재도전생태계통중적잔류검측방법。양품경을정제취,N-병기을이알흡부제( PSA)정화(도간화도각양품첨가석묵화탄흑( GCB)보조정화),UPLC-MS/MS측정,기질외표법( ESTD)정량。도전토、도전수、도미、도각화도간오충기질중배선균알화새선균알적첨가농도재0.005~2 mg/kg시,평균회수솔균위81.9%~107.6%,상대표준편차위1.4%~9.6%,검출한(LOD)시0.019~0.061μg/kg,정량한(LOQ)시5μg/kg。결과표명본방법령민도고、정량준학、측정농도범위관,차조작간편；가용우도전생태계통중동시대배선균알화새선균알진행잔류검측분석。
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.