MS的黄瓜、番茄和土壤中噻唑磷残留的检测.pdf

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1、贵州农业科学2014，42(4)：1O9～112GuizhouAgriculturalSciences[文章编号]1001—3601(2014)04—0272—0109—04基于HPLC—MS／MS的黄瓜、番茄和土壤中噻唑磷残留的检测段婷婷卜，陈湘燕，张盈，魏进，伍贵方。(1贵州省植物保护研究所，贵州贵阳55006；2．黔南州农业委员会，贵州都匀558000)[摘要]为建立黄瓜、番茄和土壤中噻唑磷的残留量检测方法，对分散固相萃取一超高效液相色谱一串联质谱法(HPLC-MS／MS)测定噻唑磷的残留量务件进行了研究。结果表明：以乙腈为提取剂，N一丙基乙二胺(PSA)和

2、石墨化碳黑(GCB)为净化剂，超高效液相色谱分离，电喷雾电离、正离子扫描，三重四级杆串联质谱仪多反应监测扫描方式进行检测，以碎片离子对m／z284．3／228进行定性分析、m／z284．3／104进行基质匹配标准品的外标法定量，在噻唑磷添加水平为0．002～2mg／kg时，噻唑磷在黄瓜、番茄和土壤的平均回收率为86．0～10l_9％，相对标准偏差(RSD)为1．7～9．4，噻唑磷的检出限(LOD)为0．042～0．049t*g／kg，定量限(L0Q)为0．141～0．164t~g／kg。结论：HPLC-MS／MS检测方法简便、快速、准确，可用于黄瓜、番茄和土壤中噻

3、唑磷的农药残留检测。[关键词]噻唑磷；农药残留；超高效液相色谱一串联质谱法；黄瓜；番茄；土壤[中图分类号]$481．8[文献标识码]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