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1、貴州農(nóng)業(yè)科學(xué)2014，42(4)：1O9～112GuizhouAgriculturalSciences[文章編號]1001—3601(2014)04—0272—0109—04基于HPLC—MS／MS的黃瓜、番茄和土壤中噻唑磷殘留的檢測段婷婷卜，陳湘燕，張盈，魏進(jìn)，伍貴方。(1貴州省植物保護(hù)研究所，貴州貴陽55006；2．黔南州農(nóng)業(yè)委員會，貴州都勻558000)[摘要]為建立黃瓜、番茄和土壤中噻唑磷的殘留量檢測方法，對分散固相萃取一超高效液相色譜一串聯(lián)質(zhì)譜法(HPLC-MS／MS)測定噻唑磷的殘留量務(wù)件進(jìn)行了研究。結(jié)果表明：以乙腈為提取劑，N一丙基乙二胺(PSA)和
2、石墨化碳黑(GCB)為凈化劑，超高效液相色譜分離，電噴霧電離、正離子掃描，三重四級桿串聯(lián)質(zhì)譜儀多反應(yīng)監(jiān)測掃描方式進(jìn)行檢測，以碎片離子對m／z284．3／228進(jìn)行定性分析、m／z284．3／104進(jìn)行基質(zhì)匹配標(biāo)準(zhǔn)品的外標(biāo)法定量，在噻唑磷添加水平為0．002～2mg／kg時，噻唑磷在黃瓜、番茄和土壤的平均回收率為86．0～10l_9％，相對標(biāo)準(zhǔn)偏差(RSD)為1．7～9．4，噻唑磷的檢出限(LOD)為0．042～0．049t*g／kg，定量限(L0Q)為0．141～0．164t~g／kg。結(jié)論：HPLC-MS／MS檢測方法簡便、快速、準(zhǔn)確，可用于黃瓜、番茄和土壤中噻
3、唑磷的農(nóng)藥殘留檢測。[關(guān)鍵詞]噻唑磷；農(nóng)藥殘留；超高效液相色譜一串聯(lián)質(zhì)譜法；黃瓜；番茄；土壤[中圖分類號]$481．8[文獻(xiàn)標(biāo)識碼]ADeterminationofFosthiazateResiduesinCucumber，TomatoandSoilUsingUPLC-MS／MSDUANTingting，CHENXiangyan，ZHANGYing，WEIJin，WUGuifang。(1．GuizhouInstituteofPlantProtection，Guiyang，Guizhou55006；2．GuizhouQiannanAgriculturalCommit
4、tee，Duyun，Guizhou558000，China)Abstract：Inordertobuildarapidandsensitiveanalyticalmethodfordeterminationoffosthiazateresiduesincucumber。tomatoandsoiI．thedeterminationconditionsoffosthiazateresiduesbythemethodofUPLC—MS／MSwerestudied．Results：thesampleswereextractedbyacetonitrileandthenpu
5、rifiedbyprimarysecondaryamine(PSA)andgraphitizedcarbon(GCB)．Themassspectrometerwasoperatedwithelectrosprayinthepositiveionmode(ESI+)．Thefosthiazatewasquantifiedbyexternalstandardmethodandmatchedstandardsolutionusedtocompensateformatrixeffect．Thequalitativeresultswereobtainedonretentio
6、ntime，theprecursorionandtwodaughterions，andthequalitationresultswereontheintensionofthecharacteristicm／z284．3／228ionandm／z284．3／104ion．Averagerecoveriesoffosthiazateincucumber，tomatoandsoilatfourlevels(0．002mg／kg，0．02mg／kg，0．2mg／kgand2mg／kg)rangedfrom86．0tolO1．9A0withrelativestandardd
7、eviationsfrom1．7％to9．4％(n一5)．Limitsofdetectionsoffosthiazateincucumber，tomatoandsoilwere0．042～0．049ug／kg。whilelimitsofquantificationswere0．141t0．164t,g／kg，respectively．Themethodissimple，rapidandaccurate，anditcanmeettherequirementsofthedomesticandinternationallegislation．Themethodadapt
8、stoco
