snt 0213.5-2002 出口蜂蜜中氟胺氰菊酯残留量检验方法 液相色谱法 35页

SNT0213.5-2002出口蜂蜜中氟胺氰菊酯残留量检验方法液相色谱法SN中华人民共和国出入境检验检疫行业标准SN/T02<13.5--2002出口蜂蜜中氟肢氨菊醋残留量检验方法液相色谱法2002-03-15发布Determinationoffluvalinateresiduesinhoneyforexport一Liquidchromatographicmethod2002-09-01实施中华人民共和国发布国家质量监督检验检查豆总局 SN/T02<13.5-2002前言本标准是按照GB/T1.1-1993(标准化工作导则第1单元:标准的起草与表述规则第1部分:标准编写的基本规定》及SN/T0001-1995《出口商品中农药、兽药残留量及生物毒素检验方法标准编写的基本规定》的要求进行编写的。其中测定方法是参考国内外有关文献，经研究、改进和验证后制定的。本标准同时制定了抽样和制样方法。测定低限是根据国际上对蜂蜜中氟胺氰菊醋残留量的最高限量和测定方法的灵敏度而制定的。本标准附录A为提示的附录。本标准由中华人民共和国国家认证认可监督管理委员会提出并归口。本标准由中华人民共和国湖北出人境检验检疫局和湖南出人境检验检疫局共同起草。本标准主要起草人:曾静、戴华、林雁飞、胡小钟、倪澜荪、余建新、吴涛。本标准系首次发布的检验检疫行业标准。??.bzfxw4>>?SN/T02<13.5一2002 前会口本标准是按照GB/T1.1-1993<<标准化工作导则第1单元s标准的起草与表述规则第1部分z标准编写的基本规定》及SN/T0001-1995<<出口商品中农药、兽药残留量及生物毒素检验方法标准编写的基本规定》的要求进行编写的。其中测定方法是参考国内外有关文献，经研究、改进和验证后制定的.本标准同时制定了抽样和制样方法。测定低限是根据国际上对蜂蜜中氟胶氟菊醋残留量的最高限量和测定方法的灵敏度而制定的。本标准附录A为提示的附录。本标准由中华人民共和国国家认证认可监督管理委员会提出并归口。本标准由中华人民共和国湖北出人境检验检疫局和湖南出人境检验检疫局共同起草。本标准主要起草人:曾静、戴华、林雁飞、胡小钟、倪澜蒜、余建新、吴涛。本标准系首次发布的检验检疫行业标准。中华人民共和国出入境检验检疫行业标准出口蜂蜜中氟殷氧菊醋残留量 检验方法液相色谱法SN!T02<13.5一20021范围Oeterminationoff1uvalinateresiduesinhoneyforexportLiquidchromatographicmethod本标准规定了出口蜂蜜中氟胶氟菊黯残留量检验的抽样、制样和液相色谱测定方法.本标准适用于出口蜂蜜中氟胶氯菊黯残留量的检验.2抽样和制样2.1检验批以不超过]000件(或25t)为一检验批。同一检验批的商品应具有相同的特征，如包装、标记、产地、规格和等级等.2.2抽样数量批量，件最低抽样数.件]-]0 11-505]-]00101-50050]以上2.3抽样工具10每增加100.增取5每增加100.增取22.3.1取样管:不锈钢管，长约115cm.内径约2.5cmo2.3.21昆样器z搪瓷桶(或杯)。2.3.3样品瓶，500mL具塞广口玻璃瓶。2.4抽样方法按2.2规定的抽样件数随机抽取，逐件开启.将玻璃管缓缓从开口处放入直至桶底，吸取样品.如遇蜂蜜结晶时，用不锈钢管缓缓插入，直至桶底，抽取样品.每件抽取样品不少于100g作为原始样品.将所取样品i顷人混样器内.ì昆和均匀，分出约1kg.装人清洁干燥的样品瓶内，加封后，标明标记，及时送交实验室. 如属瓶装蜂蜜，按应开件数.从每件中随机取一瓶，标明标记，及时送交实验室.2.5试样制备将取回样品充分搅匀，均分成两份，装入试样瓶中作为试样。密封，标明标记。如取回样品中有结晶析出.则将样品瓶加盖后，置于不超过40C的水浴中温热。待结晶全部融化后，启盖，充分搅匀，均分成两份，密封，并标明标记。中华人民共和国国家质量监督检验检疲总局纫02-03哼15批准2002-09咱们实施SN/'e02<13.5-2002如属瓶装蜂蜜，将取回的全部蜂蜜，倒在一起，充分揽匀，分取出约Ikg代表性样品。再将1kg代表性样品经搅匀后，均分成两份，装人试样瓶中作为试样。密封，标明标记。2.6试样保存将试样于室温下保存。 注:在抽样和制样的操作过程中，必须防止样品受到污染或发生残留物含量的变化测定方法3.1方法提要试样碱化后用正己烷一丙酮混合溶液提取，提取液经燕干后用乙睛和正己烷进行液液分配净化，使被测物进人乙睛层。乙睛提取液再经蒸干，用乙睛定量溶解残渣，溶液供液相色谱测定，外标法定量。3.2试剂和材料除另有规定外，试剂均为分析纯，水为蒸馏水。3.2.1乙月青:液相色谱纯.3.2.2氢氧化钠溶液:0.5g儿水溶液。3.2.3乙酸溶液:体积分数0.2%水溶液。3.2.4正己烷:用乙睛饱和。3.2.5乙睛:用正己烷饱和。3.2.6丙酮重蒸馏。3.2.7正己烷:重蒸馏.3.2.8氟胺氛菊醋标准品:纯度)97%,3.2.9氟胺氛菊酷标准溶液:准确称取适量的氟胺氰菊醋标准品，用乙睛配成浓度为1mg/mL的标准储备液，根据需要再用乙睛稀释储备液，配成适当浓度的标准工作液.3.3仪器和设备 3.3.1高效液相色谱仪:配有紫外检测器。3.3.2旋转蒸发器。3.3.3旋涡混匀器。3.3.4离心机:2000r/min,3.3.5离心管:100mL，具塞。3.3.6浓缩瓶:100mL>50mL.3.4测定步骤3.4.1提取称取试样约25g(精确至。.01g)于100mL离心管中.加15mL氢氧化钠溶液((3-2-2)，在旋涡混匀器上混匀1min，使试样溶解。加人20mL正己烷和10MI丙酮，在旋涡混匀器上提取3min，于2000r/min离心3min，将正己烷层转移到100ml浓缩瓶中。于残液中再加人20mL正己烷和10mL丙酮，重复上述操作两次，合并正己烷层于同一浓缩瓶中，于40C旋转蒸发至近干。3.4.2净化用10mL正己烷饱和的乙睛溶解残渣，转人另一100mL离心管中。加入乙腊饱和的正己烷10ml.在旋涡混匀器上混匀2min，于2000r/min离心5min后，将上层正己烷相弃去。于残液中再加人乙睛饱和的正己烷10mL,重复上述操作两次.将乙睛相转人50mL浓缩瓶中。乙睛相于40'C旋转蒸 发至近干，残渣定量加人2.00mL乙睛溶解，过0.45Wm微孔滤膜，滤液供液相色谱测定。3.4.3测定3.4-3.1液相色谱条件a)色谱柱:C18柱，250mmX4.6mm(内径)，粒径5pm，或相当者;??.bzfxw>?SN/T02<13.5-2002如属瓶装络蜜，将取囚的全部蜂蜜.倒在一起，充分搅匀，分取出约1kg代表性样品.再将1kg代表性样品经搅匀后，均分成两份，装人试样瓶中作为试样.密封，标明标记.2.6试样保存将试样于室温下保存.注:在抽样租和j样的操作过程中，必须防止样品受到窍柬或发生残留物吉量的变化.3测定方法3.1方法提要试样碱化后用正己烧-丙团混合溶液提取，提取液经蒸干后用乙睛和正己统进行液液分配净化，便 被测物进入乙脯层。乙脯提取液再经蒸干，用乙腊定量溶解残渣，溶液供液相色谱测定.外标法定量。3.2试剂和材料除另有规定外，试剂均为分析纯，水为蒸馆水.3.2.1乙精液相色谱纯.3.2.2氢氧化纳溶液，0.5g/L水溶液。3.2.3乙酸溶液z体积分数0.2%水溶液。3.2.4正己烧=用乙脯饱和。3.2.5乙脯用正己烧饱和.3.2.6丙圈:重蒸馆.3.2.7正己烧g重蒸馆.3.2.8氟胶氯菊醋标准品g纯度二三97%。3.2.9氟胶氟菊酶标准溶液z准确称取适量的氟胶氯菊醋标准品，用乙腊配成浓度为1mg/mL的标准储备液，根据需要再用乙脯稀释储备液，配成适当浓度的标准工作液.3.3仪器和设备3.3.1高效液相色谱仪z配有紫外检测器a3.3.2旋转蒸发器。3.3.3旋涡混匀器。3.3.4离心机，2000r/mino3.3.5离心管，100mL.具塞。3.3.6浓缩瓶，100mL.50mLo3.4测定步骤3.4.1提取 称取试样约25g(精确至0.01g)于100mL离心管中，加15mL氢氧化纳溶液(3.2.幻，在旋涡混匀器上混匀1min，使试样溶解.加入20mL正己烧和10时，丙阁，在旋涡混匀器上提取3min~于2000r/min离心3min，将正己烧层转移到100mL浓缩瓶中.于残液中再加入20mL正己烧和10mL丙固.重复上述操作两次，合并正己烧层于同一浓缩瓶中，于40C旋转蒸发至近干。3.4.2净化用10mL正己烧饱和的乙腊溶解残渣，转入另一100mL离心管中。加入乙腐饱和的正己炕10mL.在旋涡混匀器上混匀2min，于2000r/min离心5min后，将上层正己烧相弃去。于残液中再加入乙腊饱和的正己烧10mL.重复上述操作两次.将乙脯扭转入50mL浓缩瓶中。乙脯相于40C旋转蒸发至近干，残渣定量加入2.00mL乙腊溶解.过0.45μm微孔滤膜，泼、液供液相色谱测定。3.4.3测定3.4.3.1液相色谱条件a)色谱柱，C18柱.250mmX4.6mm(内径).粒径5μm.或相当者; SN/T02<13.5-2002b)流动相g乙脯-0.2%乙酸水溶液(80+20),c)流速.0.5mL/min,d)桂温z室温ge)检测波长.257nm,D:ì.挂样量.20严L。3.4.3.2色谱测定根据样液中被测氟胶氯菊醋含量情况，选定峰高相近的标准工作溶液.标准工作溶液和样液中氟胶氯菊醋响应傻均应在仪器检测线性范围内。对标准工作溶液和样液等体狈参插进样测定.在上述色谱条件下，氟胶氯菊醋保留时间约为26mm，标准品色谱图见附录A(提示的附录)中图Al.3.4.4空白试验除不加试样外，均按上述测定步骤进行。3.4.5结果计算和表述用色谱数据处理机或按式(1)计算试样中氟胶氯菊醋残留含量:X=h?<cXV=----h,Xm 式中.X试样中氟胶氟菊醋残留含量.mg/kg;h一一样液中氟胶氯菊醋的峰高，mm;h，一-标准工作溶液中氟胶氯菊酷的峰高，mm;c-一标准工作溶液中氟胶氯菊酷的浓度，问/mL;V一一样液最终定容体积.mL，阳最终样液所代表的试祥量.g。注2计算结果需扣除空白值。4童自定低限、回收率4.1测定低限本方法的测定低限为0.01mg/kg.4.2回收率蜂蜜中氟胶氧菊酶的添加浓度及其回收率的实验数据z在0.01mg/kg时，回收率为87.0%，在Q.05mg/kg时，回收率为90.0%;在Q.10mg/kg时，回收率为90.5%...(1) SN/T02<13.5-2002附录A(提示的附录)标准品色谱图10.0020.月旧3006图A1氟胺氛菊醋标准品的液相色谱图??.bzfxw>?SN/T02<13.5-2002附录A(提示的附录)标准晶色谱图5僵幢匾斟回帽RHHHHHHH;mm-mN20.0030.00 图Al氟胶氟菊醋标准品的液相色谱图SN/T02<13.5-2002ForewordThisstandardwasdraftedinaccordancewiththerequirementsofGB/T1.1-1993;Directivesfortheworkofstandardization-Unit1:Draftingandpresentationofstandards-Part1:Generalrulesfordraftingstandards;andSN/T0001-1995;Generalrulesfordraftingthestandardmethodsforthedeterminationofpesticide.veterinarydrugresiduesandbiotoxinsincommoditiesforexport;.Themethodfordeterrr、inationofthisstandardwasdraftedbyreferringtorelevantdomesticandforeignliteraturesthroughresearch,modificationandverification.Inaddition,methodsofsamplingandsamplepreparationarealsospecifiedinthisstandard.Thelimitofdeterminationinthisstandardisdefinedonthebasisofthecurrentinternationalmaxi-mumlimitforfluvalinateresiduesinhoneyandthesensitivityof themethod.AnnexAofthisstandardisaninformativeannex.ThisstandardwasproposedbyandisunderthechargeoftheCertificationandAccreditationad-ministrationofthePeople'sRepublicofChina.ThisstandardwasdraftedbyHubeiEntry-ExitInspectionandOuarantineBureauandHunanEntry-ExitInspectionandOuarantineBureauofthePeople'sRepublicofChina.ThemaindraftersofthisstandardareZengJing.DaiHua,LinYanf酬，HuXiaozhong,NiLansun,YuJianxinandWuTao.Thisstandardisaprofessionalstandardpromulgatedforthefirsttime.ProfessionalStandardofthePeople'sRepublicofChinaforEntry-ExitInspectionandQuarantineDeterminationoffluvalinateresiduesSN/T02<13.5-2002 inhoneyforexport一Liquidchromatographicmethod1ScopeThisstandardspecifiesthemethodsofsampling,samplepreparationanddeterminationoffluvali-nateresiduesinhoneyforexportbyliquidchromatography(I-C).Thisstandardisapplicabletothedeterminationoffluvalinateresiduesinhoneyforexport.2Samplingandsamplepreparation2.1InspectionlotEachinspectionlotshouldnotexceed1000packages(or25t).Thecharacteristicsofthecargowithinthesameinspectionlot,suchaspacking,mark,origin,speci-fication,gradeetc.,shouldbethesame.2.2Quantityofsampletaken Numberofpackagesinaninspectionlot1-1011-5051-100101-5005411一1000Minimumnumberofpackagestobetaken15105morepackagesforeveryincrementof100packages2morepackagesforeveryincrementof100packages2.3Samplingtools 2.3.1Samplingtube:Stainlesssteeltube,length:ca115cm,internaldiameter:ca2.5cm.ApprovedbyGeneralAdministrationofQualitySupervision,InspectionandQuarantineofthePeopleRepublicofChinaon2002-03-15Implementedfrom2002-09-01??.bzfxw>?ProfessionalStandardofthePeople'sRepublicofChinaforEntry-ExitInspectionandQuarantineDeterminationoffluvalinateresiduesinhoneyforexp。此-…-Liquidchromatographicmethod1ScopeSN/T02<13.5-2002Thisstandardspecifiesthemethodsofsampling,samplepreparation anddeterminationoffluvali-nateresiduesinhoneyforexpo同byliquidchromatography(LC)Thisstandardisapplicabletothedeterminationoffluvalinateresiduesinhoneyforexport.2Samplingandsamplepreparation2.1InspectionlotEachinspectionlotshouldnotexceed1000packages(or25t).Thecharacteristicsofthecargowithinthesameinspection1侃，suchaspacking,mark,origin,speci-fication,gradeetc.,shouldbethesame.2.2OuantityofsampletakenNumberofpackagesinMinimumnumberofaninspectionlotpackagestobetaken1-1011-50551-10010 101-5005morepackagesforeveryincrementof100packages501-10002morepackagesforeveryincrementof100packages2.3Samplingtools2.3.1Samplingtube:Stainlesssteeltube,length:ca115cm,internaldiameter:ca2.5cm.ApprovedbyGeneralAdministrationofOualitySupervision,lnspectionandOuarantineofthePeople'sRepublicofChinaon2∞2-03-15Implementedfrom2∞ιω-01SN/T02<13.5-20022.3.2Mixingvessel:Enameldrum(orcup).2.3.3Samplebottle:500mL.wide-mouthedglassbottle.withgroundstopper. 2.4SamplingprocedureDrawanumberofsamplepackagesspecifiedin2.2atrandomandopenthepackagesonebyone.Takethesamplefromthepackagebyinsertingslowlythesamplingtubetothebottom.lfthehoneyiscrystallized.penetratethestainlesssteeltubetothebottomofthecontainer.Thesampletakenfromeachpackageshouldnotbelessthan1009asaprimarysample.Pourthedrawnsam-plesintothemixingvessel.andmixthoroughly.Drawca1kgofthemixedsampleandplaceinacleandrysamplebott怡.seallabel.andsendtothelaboratoryintime.Ifthehoneywaspackedinbottlesinsidethepackage.drawonebottlefromeachofthepackagesopened.Labelandsendtothelaboratoryintime.2.5PreparationoftestsampleMixallthesamplestakenbackthoroughly.anddivideintotwoequalportions.Eachportionisplacedinasamplebottleasthetestsample.whichissealedand labeled.Ifthesampletakenbackbecomescrystallized.meltitbywarminginwater-bathbelow40;Cwiththesamplebottlecoveredtightly.Whenthesamplehascompletelymelted.removethecoverandmixthoroughly.Divideintotwoequalp。同ions.eachportionisplacedinasamplebottleasthetestsample.sealedandla-beled.Forbottle-packedhoney.pourallthehoneytakenbackintoavesselandmixthoroughly.Drawca1kgoftherepresentativesample.mixwellanddivideintotwoequalportions.Eachportionisplacedinasamplebottleasthetestsample.sealedandlabeled.2.6StorageoftestsampleThetestsamplesshouldbestoredatroomtemperature.Note:Inthecourseofsamplingandsamplepreparation.precautionsmustbetakentoavoidcontaminationoranyfactorswhichmaycausethechangeofresiduecontent3Methodofdetermination 3.1PrincipleAfteralkalified.thefluvalinateresiduesinthetestsampleareextractedwithn-hexane-acetone.Af-terevaporated.theextractiscleanedupbyliquid-liquidpartitioningwithacetonitrileandn-hexanetocausetheanalytetoenterintoacetonitrilelayer.Theacetonitrileextractisevaporatedandtheresidueisleachedwithacetonitrile.ThesolutionisusedforLCdetermination.Externalstandardmethodisusedforquantitativemeasuren、ent_3.2ReagentsandmaterialsUnlessotherwisespecified.allreagentsusedshouldbeanalyticallypure.;Water;isdistilledwa-ter.SN/T02<13.5-20023.2.1Acetonitrile:HPLCgrade.3.2.2Sodiumhydroxidesolution:0.5g/Laqueoussolution. 3.2.3Aceticacidsolution:0.2%(V/V)aqueoussolution.3.2.4n-hexane:Saturatedwithacetonitrile.3.2.5Acetonitrile:Saturatedwithn-hexane.3.2.6Acetone:Redistilled.3.2.7n-hexane:Redistilled.3.2.8Fluvalinatestandard:Purity,97%.3.2.9Fluvalinatestandardsolution:AccuratelyWeighanadequateamountoffluval:nateStan-dardanddissolveinacetonitriletoprepareasolutionof1mg/mLinconcentrationasthestandardstocksolution.Accordingtotherequirement,prepareastandardworkingsolutionofappropriateconcentrationbydilutingthestocksolutionwithacetonitrile.3.3Apparatusandequipment3.3.1Highperformanceliquidchromatograph:EquippedwithUVdetector. 3.3.2Rotaryevaporator.3.3.3Vortexmixer.3.3.4Centrifuge:2000r/min.3.3.5Centrifugetube:100mL,withstopper.3.3.6Concentrator门00mL,50mL.3.4Procedure3.4.1ExtractionWeightca25gofthetestsample(accurateto0.01g)intoa100mLcentrifugetube,add15mLsodiumhydroxidesolution(3.2.2),mixintenselyinavortexmixerfor1min.Add20mLn-hex-oneand10mLacetone,mixagainfor3minforextraction,thencentrifugefor3minat2000r/min.Transferthen-hexanelayertoa100mLconcentrator.Totheremaininglayer,add20mLn-hexaneand10mLacetoneagain,repeattheaboveprocesstwice.Combinethen-hexaneextracts tothesameconcentrator.Rotary-evaporatejusttodrynessatabathtemperatureat40'C.3.4.2CleanupDissolvetheresiduewith10mLacetonitrile(saturatedwithn-hexane),transferthesolutioninto.??.bzfxw>?SN/T02<13.5-20023.2.1Acetonitrile:HPLCgrade.3.2.2Sodiumhydroxidesolution:0.5g/Laqueoussolution.3.2.3Aceticacidsolution:0.2%(V/V)aqueoussolut??on.3.2.4n-hexane:Saturatedwithacetonitrile.3.2.5Acetonitrile:Saturatedwithn-hexane3.2.6Acetone:Redistilled.3.2.7n-hexane:Redistilled. 3.2.8Fluvalinatestandard:Purity;;.97%.3.2.9Fluvalinatestandardsolution:AccuratelyWe??ghanadequateamountoffluval;natestan-dardanddissolveinacetonitriletoprepareasolutionof1mg/mLinconcentrationasthestandardstocksolution.Accordingtotherequirement,prepareastandardworkingsolutionofappropriateconcentrat??onbydilutingthestocksolutionwithacetonitrile.3.3Apparatusandequipment3.3.1Highperformanceliquidchromatograph:Equippedw??thUVdetector.3.3.2Rotaryevaporator.3.3.3Vortexmixer.3.3.4Centrifuge:2000r/min.3.3.5Centrifugetube:100mL,withstopper3.3.6Concentrator:100mL,50mL 3.4Procedure3.4.1ExtractionWeightca259ofthetestsample(accurateto0.01g)intoa100mLcentrifuge!ube,add15mLsodiumhydroxidesolution(3.2.2),mixintenselyinavortexmixerfor1min.Add20mLn-hex-aneand10mLacetone,mixagainfor3minforextraction,thencentrifugefor3m??nat2000rlm??n.Transferthen-hexanelayertoa100mLconcentrator.Totheremaininglayer,add20mLn-hexaneand10mLacetoneagain,repeattheaboveprocesstwice.Combinethen-hexaneextractstothesameconcentrator.Rotary-evaporatejusttodrynessatabathtemperatureat4O;C3.4.2CleanupDissolvetheresiduewith10mLacetonitrile(saturatedwithn-hexane),transferthesolutioninto8 SN/T02<13.5-2002100mLcentrifugetube.Add10mLn-hexane(saturatedwithacetonitrile)totheacetonitrilelayer.mixintenselyinavortexmixerfor2min,thencentri1uge10r5minat2000r/min.deletethen-hexanelayer.Totheremaininglayer.add10mLn-hexane(saturatedwithacetonitrile)again.re-peattheaboveprocesstwice.Transfertheacetonitrilelayerintoa50mLconcentratorandrotary-e-vaporatejusttodrynessatabathtemperatureat4O'C.Addexactly2.00mL01acetonitriletodis-solvetheresidue.而Iteritthrougha0.45μmmicro-holemembranefilter.ThefiltratedsolutionisreadyforHPLCdetermination3.4.3Determination3.4.3.1HPLCoperatingcondítiona)LCcolumn:C18,250mmx4.6mm(id).pa同íclesíze5μm.orequivalent:b)Mobilephase:acetor甘trile0.2%aceticacidaqueoussolution(80+20):c)Flowrate:0.5mUmin:d)Columntemperature:roomtemperature:e)Detectionwavelength:257nm: f)Injectionvolume:20μL.3.4.3.2抖PLCdeterminationAccordingtotheapproximateconcentrationoffluvalinateinthesamplesolution,selectthestan-dardworkingsolutionwithsimilarpeakheighttothatofthesamplesolution.Theresponsesofflu-valinateinthestandardworkingsolutionandsamplesolutionshouldbewithinthelinearrangeoftheinstrumentaldetection.Thestandardworkingsolutionshouldberandomlyinjectedin-be的veentheinjectionsofthesamplesolutionofequalvolume.Undertheaboveoperatingcondition.there-tentiontimeoffluvalinateisabout26min.Forchromatogramofthestandard,seefig.A1inannexA.3.4.4BlanktestTheoperationoftheblanktestísthesameasthatdescribedinthemethodofdetermination,butwithomissionofsampleaddition.3.4.5Calculationandexpressionoftheresult CalculatethecontentoffluvalinateresiduesinthetestsamplebyLCdataprocessororaccordingtotheformula(1):，卢EV---me---ma7nEn-=X)1(....whereX-theresiduecontentoffluvalinateinthetestsample,mg/kg;h一thepeakheightoffluvalinateinthesamplesolution,mm:hs-thepeakheightoffluvalinateinthestandardworkingsolution,mm:c-theconcentrationoffluvalinateinthestandardworkingsolution，μg/mL:V-thefinalvolumeofthesamplesolution,mL:m-thecorrespondingmassofthetestsampleinthefinalsamplesolution.g. SN/T02<13.5-20024Limitofdeterminationandrecovery4.1LimitofdeterminationThelimitofdeterminationofthismethodis0.010mg/kg.4.2RecoveryAccordingtotheexperimentaldate,thefortifyingconcentrationoffluvalinateinhoneyanditscor-respondingrecoveriesare:0.01mg/kg,therecovery87.0%;0.05mg/kg,therecovery90.0%;0.10mg/kg,therecovery90.5%.10??.bzfxw>?SN/T02<13.5-20024Limitofdeterminationandrecovery4.1Limitofdetermination Thelimitofdeterminationofthismethodis0.010mg/kg.4.2RecoveryAccordingtotheexperimentaldate,thefortifyingconcentrationoffluvalinateinhoneyanditscor-respondingrecoveriesare:11)0.01mgl闸，ther田overy87.0%;0.05mgl阔，therecovery90.0%;0.10mgl闸，therecovery90.5%.SN/T02<13.5-2∞2AnnexA(informativ8)Chromatogramofthestandard@Ma 何回m-6、，SEt--anHHH的阴阳的;20.00r----r-寸30∞monFig.A1Liquidchromatogramoffluvalinatestandard