SN-T 0527-2012出口糧谷中甲硫威(滅蟲威)及代謝物殘留量的檢測方法 液相色譜-質(zhì)譜質(zhì)譜法

中華人民共和國出入境檢驗檢疫行業(yè)標(biāo)準(zhǔn)代替SN0527—1996量的檢測方法液相色譜-質(zhì)譜/質(zhì)譜法Determinationofmethiocarbanditsmetaboliteresiduesincerealsforexport—2012-05-07發(fā)布2012-11-16實(shí)施I1出口糧谷中甲硫威(滅蟲威)及代謝物殘留量的檢測方法液相色譜-質(zhì)譜/質(zhì)譜法1范圍3方法提要4.720mmol/L甲酸銨水溶液(含0.1%甲酸):準(zhǔn)確稱取1.2612g甲酸銨，加入1mL甲酸，用水溶26試樣的制備與保存稱取均質(zhì)樣品1g(精確至0.01g),置于25mL聚丙烯離心管中，加入10mL乙腈，渦旋混合2min。超聲振蕩20min,在3000r/min下離心5min,取出上清液于另一50mL聚丙烯離心管中。殘7.2凈化3時間/min流速/20mmol/L甲酸銨水溶液(含0.1%甲酸)/%乙腈/%00.4030.4050.4050.40相對離子豐度/%允許的最大偏差/%士25士30 (1)4SN/T0527—20129測定低限和回收率9.1測定低限本方法的測定低限：甲硫威19.0pg/kg,甲硫威亞砜10.0pg/kg,甲硫威砜10.0pg/kg。5LC-MS/MS參考質(zhì)譜條件”psi);psi);電離模式化合物名稱參考保留時間/min監(jiān)測離子m/z去簇電壓/V碰撞電壓/V采集時間/ESI+甲硫威亞砜242.1>185.1*8甲硫威砜258.1>122.1*258.1>107.0甲硫威226.1169.1*4·為定量離子。6(資料性附錄)b)7化合物名稱甲硫威砜甲硫威添加水平/回收率范圍/%回收率范圍/%添加水平/回收率范圍/%大米玉米大麥小麥糙米8ThestandardisdraftedaccordingtoGB/T1.1—2009principle.ThestandardisreplaceofSN0527—1996Methodforthedeterminationofmethiocarbresiduesincerealsforexport.sulfoneandmethiocarb-sulfoxideinrice,corn,broiwnrice,barleyandwheatIforexport一Thetestsampleisextractedwithacetoni—ThecleanupprocessureisimprovedThisstandardwasdraftedbytheShanghalEntry.ExitInspection/andQuarantineBureauofthePeople'sRepublicofChina,ShanghaiInstituteofqualityInspectionandTechnicalResearch.ThemaindraftersoftThestandardreplacesthestandardpreviousversionspublishedas;—SN0527—1996.9Thisstandardspecifiesthemethodoftestingmethiocarbandmetabolism(methiocarb-sulfoneandmethiocarb-sulfoxide)residueincerealsforexportbyLC-MS/MSmethod.Thisstandardisapplicabletothedeterminationofresiduecontentofmethiocarbandmethiocarbsulfoneandmethiocarb-sulfoxideinrice,corn,brownrice,barleyandwheatIforexportThefollowingdocumentsisnecessaryforthisstandard.Fordatedfeferences,onlydatededitionsshallapplytothisstandard.Foruhdatedreferences,thelatesteditionofthenormativedocumentreferredtoapplies.Allthereagentsusedshouldbeanalyticallypureunlessotherwisespecified.“Water”isdoubledistilledwater.4.2Methanol:HPLCgrade.4.3Formicacid:HPLCgrade.SN/T0527—20124.4Ammoniumformate.4.5Anhydrousmagnesiumsulfate.4.6Acetonitrile:water(1+1,V/V):50mLacetonitrilea4.720mmol/Lammoniumformate(contain0.1%formicacid):Weighammoniumacetate1.2612g,add1mLformicacid.Dissolvewithwateranddiluteto1000mL.sulfoxide(CASNo.:2179-25-1):Purity≥98%.4.12Standardworkingsolution:dilutethestandardmediumstocksolutionwithblanksampleextractstotherequiredconcentrationtomakethestandardworkingsolution.4.13Blanksampleextracts:Weighofthetestsample,for7.1and7.2procedure5.1Liquidchromatography-mass/massspectrometry,equippedwithelectrosprayionsourceandtriquadruplemassspectrometer.5.2Electronicbalance:Accurateto0.01g,0.001g5.6Centrifugetube:25mLElectronicbalanc.5.8Waterbathcontainer.Takeapproximately1kgofrepresentativesample.Smashthoroughlybyacrusher.MixthoroughlyPutincleancontainers.SealandlabelthemThetestsamplesshallbestoredatroomtemperature.Whilesamplingandpreparingsample,pleaseavoidcontaminationoranyfactorsthatmaychangeresiduecontent.Weigh1g(accurateto0.01g)ofthetestsampleintoa25mLcentrifugetube.Add10mLacetonitrile.Homogenizefor2min.Ultrsonicextractfor20minandcentrifugefor5minat3000r/min.Taketheuplayerofacetonitriletoanothertube,theresiduewasreextractedwith10mLacetonitrile.Combinealltheextractsinto50mLconcentratebottle.Add0.5ganhydrousmagnesiumsulfateand0.5ggraphitepowder.Vortexmixfor2minandcentrifugefor5minat3000r/min.Transfertheuplayerinto100mLconcentratebottle,Evaporatetheextracttodrynessunder40℃.Add1mLsampledilutesolutiontoredissolvetheextracts.Vortexmixfor2min.Filterthesolutionwith0.22μmmembraneThesolutionisreadyforLC-MS/MSdetermination.LCoperatingconditionsareasfollows:a)LCcolumn:Ccolumn,50mm×2.0mm(i.d.),3.0μm(orotherequivalentones)SN/T0527—201220mMammoniumformate(contain0.1%formic%%055MS/MSoperatingconditionsareasfollows:a)Scanningmodel:positiveion(ESI);b)Monitoringmodel:multiplerfactionmonitding(MRM);LC-MS/MSDeterminationUndertheLC-MS/MSoperatingconditions,thestandardworkingsolutionandsamplesolutionisinjected.Iftheretentiontimesofsamplechromatogrampecksareconsistentwiththatofstandardsolution,calibrationcurvemethodisusedforquantitativemeasurement.Therelativeintensitiesoconcentrationofstandardsolutionshouldbesamewiththoseofsamplesolution.Thepermittedtoleranceslistedintable2,thenthecorrespondinganalytemustbepresentinsamplepermittedtolerances/%士25LC-MS/MSDeterminationAccordingtotheapproximateconcentrationofanalyteinsamplesolution,selectthestandardworkingsolutionwithsimilarresponsestothatofsamplesolution.Theresponsesofanalyteinthestandardworkingsolutionandthesamplesolutionshouldbewithinthelinearrangeoftheinstrumentdetection.Reconstituted(MRM)chromatogramofstandardworkingsolutionislistedinFigureB.1.CalculatethecontentofmethiocarbresidueinthetestsamplebyLC-MS/MSdataprocessororaccordingtothefollowedformulawhere:X,-theresiduecontentofmethiocarbanditsmetabolisminthetestsample,mg/kg;A,—thepeakareaofmethiocarbanditsmetabolisminthesamplesolution;c,—thetotalconcentrationofmethiocarbanditsmetabolisminthestandardworkingsolution,Lg/mL;V-thefinalvolumeofthesamplesolution,mL;A-thetotalpeakareaofmethiocarbanditsmetabolismTinthestandardworkingsolution;m—thecorrespo