SNT 2451-2010動物源性食品中呋喃苯烯酸鈉殘留量檢測方法液相色譜-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)SN/T2451—2010動物源性食品中呋喃苯烯酸鈉殘留量檢測方法液相色譜-質(zhì)譜/質(zhì)譜法2010-01-10發(fā)布2010-07-16實施I1SN/T2451—2010動物源性食品中呋喃苯烯酸鈉殘留量檢測方法液相色譜-質(zhì)譜/質(zhì)譜法2規(guī)范性引用文件GB/T6682分析實驗室用水規(guī)格和試驗方法(GB/T6682—2008,ISO3696:1987,MOD)5.5呋喃苯烯酸鈉標(biāo)準(zhǔn)品(Ci?HgNNaO?):CAS登錄號為54992-23-3;純度大于等于99.0%,購自Wakepurechemicalindustries5.70.1%甲酸溶液：取1.0mL甲酸用水定容至1000mL。5.8溶解液：0.1%甲酸溶液十乙腈(4+1,體積比)。25.10標(biāo)準(zhǔn)儲備溶液：1.0mg/mL,取25mg標(biāo)準(zhǔn)品用少量甲醇溶解并定容至25mL,-18℃避光現(xiàn)用。下同7.1.1。向溶解液中加入3mL乙腈飽和正己烷(5分),稍加振搖后靜置分層后，取下層溶液于9500r/min離心5min,供液相色譜-質(zhì)譜/質(zhì)譜檢測。表1梯度洗脫程序時間/min流動相比例A%B%3SN/T2451—2010表1(續(xù))時間/min流動相比例A%B%7.3.2質(zhì)譜條件d)其他條件參見附錄A。8.1標(biāo)準(zhǔn)曲線的繪制用空白基質(zhì)溶液將呋喃苯烯酸鈉標(biāo)準(zhǔn)中間工作溶液(5.11)逐級稀釋得到2ng/mL、5ng/mL、酸鈉。相對離子豐度/%>10～20允許的最大偏差/%±士304 本方法在5.0pg/kg、10.0pg/kg、20pg/kg添加水平的回收率及精密度參見附錄C中表C.1.5質(zhì)譜/質(zhì)譜測定參考條件1)表A.1呋喃苯烯酸鈉質(zhì)譜/質(zhì)譜多反應(yīng)監(jiān)測條件化合物母離子子離子破裂電壓/V碰撞電壓/V駐留時間/s呋喃苯烯酸鈉258.3214.0?5a離子用于定量。67(資料性附錄)LC-MS/MS法添加回收率及精密度表C.1LC-MS/MS法添加回收率及精密度樣品名稱添加濃度/(μg/kg)回收率/%相對標(biāo)準(zhǔn)偏差/%豬肉579.6～90.04.381.9～87.083.5～87.5豬肝582.4～87.081.9～86.878.0~93.0豬腎585.0～99.281.2～90.24.482.5～90.0鰻魚580.0～86.281.5≈86.3雞蛋576.886.482.0～84.2牛奶577.~86.45～86.58ficationandAccreditation.ThisstandardwasdraftedbyJiaRepublicofChina.ThismaindraftersofthisstandardareZhanChunrui,WenZhihai,GuoPing,LiHaiyan,ZhouPingyong,GuiJiaxiang.9Thisstandardisapplicabletothedeterminationofsodiumnifurstyrenateresiduesinliver,kidneypork,eel,eggandmilk.Thefollowingnormativedocumentscontainprovisionswhich,throughreferenceinthistext,consti-tuteprovisionsofthisprofessionalstandard.Fordatedreferences,subsequentamendmentsto,orre-visionsof,anyofthesepublicationsdonotapply.However,partiefessionalstandardareencouragedtoinvestigatethepossibilityofapplyingthemostrofthenormativedocumentsindicatedbelow.Forundatedreferencetivedocumentreferredtoapplies.GB/T6682Waterforanalyticallaboratoryuse—Specificationandtestmethods(GB/T6682—2008,IS03696:1987,MOD)3Samplepreparationandsto3.1Topork,liverandkidneysamples,about500greprestionofthetestsampleisputintoacleancontainer,thensealandlabelit.Thesamplesarestoredbe-low-18℃.Pleasecoo3.2Toeggs,pealofftheskin,mixthroughlyandthendivideintotwoequalportions.Eachportion-18℃.Pleasecoolatroomt3.3Tomilk,stirmixthroughlyandthendivideintotwoequalportions.EachportionofthetestPleasecoolatroomtemperaturewhenuse.Thesodiumnifurstyrenateresiduesinthetestsamplesareextractedwithacetonitrile,thenpurifedbyliquid-liquidpartitionwithsaturatedhexaneinacetonitrile,afterconcentratedanddiluted.Thefi-method.Unlessotherwisespecified,allregents.are.analyticallypure,“water?isdeionizedwater.5.1Methanol:LCgrade.5.2Acetonitrile:LCgrade.5.3Formicacid:LCgrade.5.4n-hexane:LCgrade.5.5Sodiumnifurstyrenatestandard(CgHaNNaO?):CAS54992-23-3,purity≥99.0%.Buyingfrom5.6Anhydroussodiumsulfate:Igniteat656Cfor.2h,andkeepinasolvetovolumewithacetonitrile.5.8Combinationsolution:0.1%Formicacidinwater+acetonitrile=4+1(V/V).oughly,drawabovehexane.5.10Standardstocksolution:1.0mg/mL,Accuratelyweigh25mginto25mLvolumetricflack,dis-solvetovolumewithmethanol,andmixtohomogeneity.Thesolutioncanbestoredatthetempera-5.11Standardworkingsolution:10.0μg/mL,Accuratelyweigh(5.10)into10mLvolumetric,di-lutewithmethanoljustbeforeuse.6.4Centrifuger:4000r/min.9500r/min.6.5Colorimetrictube:50mL.6.7Nitrogenblowingdevice7.1.1Pork,liver,kidney,egg,eelWeigh5g(accurateto0.01g)ofthetestsampleintoa50/mLcentrifugetube,add25mLofaceto.nitrileandmixfor30s,thencentrifugefof5minat4000f/min.Theuppers50mLcolorimetrictube,repedttheaboveprocedureohce,combinedtheextractionsolution,dilutedevicewithabathtemperaturebelow.40C.DissolvWeigh5g(accurateto0.01g)ofthetestsampleintoa50mLcentrifugetube,andabout5ganhydroussodiumsulfate,mixfully.Theotherstepwassimilarto7.1.1.cardhexaneaftercentrifugefor5minat9500r/min,forLC-MS/Ma)Chromatographiccolumn:PhenomenexLunaCia,150mm×2.1mm(i.d.),3pm,orequivalent;e)Injectorvolume:20μL.Time/minRationofthemobileA/%B/%b)Scanmode:Negitive;c)Monitoringmodel:Multiplereactionmonitoring(MRM)d)TheotherconditionWeigh5g(accurateto0.01g)8LC-MS/MSdeterminationDilutestepwisethestandardworkingsolution(5.11)tomatrixstandardsolutionswithconcentra-tionsof2、5、10、20and50ng/mLbyblankmatrixsolution.AccordingtotheLC-MS/MSconditiona-bovementioned,determinatedthematrixstandardsolutionsfromlowtohigh.Drawthestandardcurve,abscissapresentstheconcentrationofmatrixstandardsolutionsandordinatepresentsre-figureB.1.taintimeofsodiumnifurstyrenateis8.3min.Underthesamedeterminationcondition,theratioofthechromatographicretentiontimeoftheanalystsshallcorrespondtothatofthecalibrationsolutionatatoleranceof±2.5%.Therelativeintensitiesofthedetectedionsofeachanalysts,shallcom-poundtothoseofthecalibrationstandardatcomparableconcentrations,withinthetolerancesshownintable2,thenthecorrespondingforrelativeionintensitieswhileconfirmation.Relativeintensity/%>20～50>10～20Permittedtolerances/%Accordingtotheapproximateworkingoperatingcondition,theresponseofsodiumnifurstyrenatethesampleshouldbedilutedwiththeblankmatrixsolutiontosuitableconcentratin.Calculatethecontentoffollowedformul