建立了QuEChERS-液相色谱-串联质谱法(LC-MS/MS)检测土壤和柑橘中吡唑醚菌酯、甲基硫菌灵及其代谢物多菌灵的分析方法.样品经甲醇或乙腈提取,N-丙基乙二胺(PSA)净化后,用液相色谱分离,电喷雾正离子多反应监测(MRM)模式进行质谱测定,以基质匹配标准溶液进行外标法定量.吡唑醚菌酯、甲基硫菌灵和多菌灵的定量限(LOQ,S/N=10)分别为5.8~7.0 μg/kg、9.3~14.1 μg/kg和2.1~2.6 μg/kg.样品的加标回收率为75.48%~109.18%,相对标准偏差(RSD)为0.60%~5.11%(n=5).该法快速简便,定量准确,用基质配制标准溶液能够有效、准确地校正LC-MS/MS测定吡唑醚菌酯、甲基硫菌灵和多菌灵残留的基质效应,满足土壤、橘皮、橘肉和柑橘全果实际样品的检测需求.
A QuEChERS-liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of pyraclostrobin,thiophanate-methyl and its metabolite carbendazim in soil and citrus.The samples were extracted with methanol or acetonitrile,purified by primary secondary amine (PSA),then separated by LC,detected in multiple reaction monitoring (MRM) mass spectrometry mode via positive electrospray ionization.The analytes were quantified by matrix-matched standard solutions with external standard method.The limits of quantification (LOQs) of pyraclostrobin,thiophanate-methyl and carbendazim in different matrices were 5.8-7.0 μg/kg,9.3-14.1 μg/kg and 2.1-2.6 μg/kg,respectively.For all the samples,the spiked recoveries ranged from 75.48% to 109.18%,and the relative standard deviations (RSDs) were 0.60%-5.11% (n=5).The method is quick,easy,effective,sensitive and accurate.The matrix-matched calibration solutions can efficiently compensate matrix effects of the pyraclostrobin,thiophanate-methyl and carbendazim in LC-MS/MS analysis.The established method can be applied to the residue analysis of the real samples of soil,citrus peel,citrus pulp and citrus fruits.
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