QuEChERS-液相色谱-串联质谱法同时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残留  

Simultaneous determination of pyraclostrobin and thiophanate-methyl and its metabolite carbendazim residues in soil and citrus by QuEChERS-liquid chromatography-tandem mass spectrometry

作　　者：李福琴[1] 石丽红[1] 王飞[1] 孙财远 康頓 张钰萍[1] 陈泠竹[1] 胡德禹[1] 康頔[1] LI Fuqin;SHI Lihong;WANG Fei;SUN Caiyuan;KANG Di;ZHANG Yuping;CHEN Lingzhu;HU Deyu;KANG Di(Research and Development Center for Fine Chemicals,State Key Laboratory of Green Pesticide and Agricultural Bioengineering,Ministry of Education,Guizhou University,Guiyang 550025,China)

机构地区：[1]贵州大学精细化工研究开发中心,教育部绿色农药与农业生物工程国家重点实验室,贵州贵阳550025

出　　处：《色谱》2017年第6期620-626,共7页Chinese Journal of Chromatography

基　　金：贵州大学研究生创新基金项目(2016077)~~

摘　　要：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5.8~7.0μg/kg、9.3~14.1μg/kg和2.1~2.6μg/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(P S A),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 were5.8-7.0ug/k g,9.3-14.1ug/kg and2.1-2.6ug/k g,respectively.For all the samples,the spiked recoveries ranged from75.48%to109.18%,and the relative standard deviations(RSDs)were0.60%-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,citruspulp and citrus fruits.

关 键 词：液相色谱-串联质谱 QUECHERS 吡唑醚菌酯 甲基硫菌灵 多菌灵 土壤 柑橘 

分 类 号：O658[理学—分析化学]