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

发布时间：2018-06-29 21:02

本文选题：液相色谱-串联质谱 + QuEChERS　；参考：《色谱》2017年06期

【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。
[Abstract]:A QuEChERS- liquid chromatography-tandem mass spectrometry (LC-MS / MS) method was developed for the determination of pyrazolyl ester, methyl thiazolyl and its metabolite carbendazim in soil and citrus. The samples were purified by methanol or acetonitrile, then separated by liquid chromatography, determined by mass spectrometry with electrospray ion multiple reaction monitoring (MRM), and quantified by external standard solution. The quantification limits of pyrazole, methyl thiamyl and carbendazim were 5.8 渭 g / kg and 2.1g / kg 路kg ~ (-1) 路min ~ (-1), respectively. The recoveries of the samples were 75.48 and 109.18, and the relative standard deviation (RSD) was 0.60 卤5.11% (n = 5). The method is rapid, simple and accurate. The preparation of standard solution with matrix can be used to correct the matrix effect of pyrazole, methyl thiamyl and carbendazim residues in soil, orange peel, and to correct accurately the matrix effect of LC-MS / MS for the determination of pyrazole, methyl thiamyl and carbendazim residues. Testing requirements for actual samples of tangerine meat and citrus fruit.
【作者单位】：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;
【基金】：贵州大学研究生创新基金项目(2016077)~~
【分类号】：O657.63;TS255.7;X839.2

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