QuEChERS-液相色譜-串聯(lián)質(zhì)譜法同時(shí)檢測(cè)土壤和柑橘中吡唑醚菌酯、甲基硫菌靈及其代謝物多菌靈的殘留
本文選題:液相色譜-串聯(lián)質(zhì)譜 + QuEChERS; 參考:《色譜》2017年06期
【摘要】:建立了QuEChERS-液相色譜-串聯(lián)質(zhì)譜法(LC-MS/MS)檢測(cè)土壤和柑橘中吡唑醚菌酯、甲基硫菌靈及其代謝物多菌靈的分析方法。樣品經(jīng)甲醇或乙腈提取,N-丙基乙二胺(PSA)凈化后,用液相色譜分離,電噴霧正離子多反應(yīng)監(jiān)測(cè)(MRM)模式進(jìn)行質(zhì)譜測(cè)定,以基質(zhì)匹配標(biāo)準(zhǔn)溶液進(jìn)行外標(biāo)法定量。吡唑醚菌酯、甲基硫菌靈和多菌靈的定量限(LOQ,S/N=10)分別為5.8~7.0μg/kg、9.3~14.1μg/kg和2.1~2.6μg/kg。樣品的加標(biāo)回收率為75.48%~109.18%,相對(duì)標(biāo)準(zhǔn)偏差(RSD)為0.60%~5.11%(n=5)。該法快速簡(jiǎn)便,定量準(zhǔn)確,用基質(zhì)配制標(biāo)準(zhǔn)溶液能夠有效、準(zhǔn)確地校正LC-MS/MS測(cè)定吡唑醚菌酯、甲基硫菌靈和多菌靈殘留的基質(zhì)效應(yīng),滿足土壤、橘皮、橘肉和柑橘全果實(shí)際樣品的檢測(cè)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 鹵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.
【作者單位】: 貴州大學(xué)精細(xì)化工研究開(kāi)發(fā)中心教育部綠色農(nóng)藥與農(nóng)業(yè)生物工程國(guó)家重點(diǎn)實(shí)驗(yàn)室;
【基金】:貴州大學(xué)研究生創(chuàng)新基金項(xiàng)目(2016077)~~
【分類號(hào)】:O657.63;TS255.7;X839.2
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