行业制造-标准-出口粮谷及油籽中快杀稗残留量检验方法

中华人民共和国出入境检验检疫行业 标准 excel标准偏差excel标准偏差函数exl标准差函数国标检验抽样标准表免费下载红头文件格式标准下载 sN/T1017.5-2002出口粮谷及油籽中快杀稗残留量检验 方法 快递客服问题件处理详细方法山木方法pdf计算方法pdf华与华方法下载八字理论方法下载 Methodforthedeterminationofquincloracresiduesincerealsandoilseedsforexport2002一01一16发布2002一06一01实施中华人民共和国国家质量监督检验检疫总局发布SN/T1017.5-2002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 关于同志近三年现实表现材料材料类招标技术评分表图表与交易pdf视力表打印pdf用图表说话 pdf 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 对教师党员的评价套管和固井爆破片与爆破装置仓库管理基本要求三甲医院都需要复审吗 进行编写的。其中测定方法是参考国内外有关文献，经研究、改进和验证后而制定的。同时制定了抽样和制样方法。测定低限是根据国际上对粮谷及油籽中快杀稗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。本标准由国家认证认可监督管理委员会提出并归口。本标准起草单位:中华人民共和国吉林出人境检验检疫局。本标准主要起草人:李庆才、荣会、郑希铭、洪权春、曲中文。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粮谷及油籽中快杀稗残留量检验方法sN/T1017.5-2002Methodforthedeterminationofquincloracresiduesincerealsandoilseedsforexport范围本标准规定了出口粮谷及油籽中快杀稗残留量检验的抽样、制样和气相色谱测定方法。本标准适用于出口糙米、大豆、玉米、小麦中快杀稗残留量的检验。抽样和制样2.1检验批以不超过200t为一检验批。200t袋装玉米或大豆约2200袋;袋装糙米或小麦约4000袋。玉米或大豆有时为散装品。同一检验批的商品应具有相同特征，如包装、标记、产地、规格和等级等。2.2抽样数量2.2.1袋装货品按式(1)计算抽样袋数:a=丫了，·······················⋯⋯(1)式中:N—全批袋数;a—抽样袋数。注:“值取整数小数部分向前进位为整数。2.2.2散积货品(玉米或大豆)货堆高度不超过2m。按货堆面积划区设点。以50m，为一个取样区，每区设中心及四角(距边线1m处)5个点。每增加一个取样区，增设3个点。23抽样工具2.3.1金属单管取样器全长55cm(包括手柄)，直径1.5cm--2.0cm，沟槽长度应超过袋对角线长度的一半。2.3.2金属双套管取样器:全长分1m,2m(均包括手柄)两种。内、外管同部位分段开几个槽口，每个槽口长15cm--20cm，口宽2.0cm-2.5cm。内管的内径为2.5cm-3.0cm;取样器的探头长约7cm2-3-3取样铲或取样勺。2.3.4分样板。2.3.5盛样器:筒或袋，可密封2-3.6分样布或适用铺垫物。2.4抽样方法2.4.1袋装抽样中华人民共和国国家质里监督检验检疫总局2002-01一16批准2002-06-01实施2SN/T1017.5-20022.4.1.1倒包抽样从堆垛的各部位随机抽取2.2.1规定的应抽样袋数的1o%(每批一般不少于3袋).将袋口缝线全部拆开，平置于分样布或其他洁净的铺垫物上，双手紧握袋底两角，提起约成45。倾角，倒拖约1m，使袋内货物全部倒出。查看袋内和袋间品质是否均匀。确认情况正常后，用取样铲随机在各部位抽取样品，并立即将样品倒入盛样器内。毒袋抽取样品的数量应基本一致。2.4.1.2袋内抽样按2.2.1规定的应抽样袋数(扣除倒包抽样袋数)，在堆垛四周的上、中、下各层以曲线形走向随机抽取。然后按糙米、小麦、玉米、大豆，用下述方法进行取样:对糙米、小麦，用金属单管取样器(2.3.1)槽口朝下，从每袋一角依斜对角方向插人袋内，然后将管槽旋转朝上，抽出取样器，立即将样品倒人盛样器内。对玉米、大豆，用1m长的金属双套管取样器(2.3.2)，关闭槽n，从每袋一角依斜对角方向插人袋内，然后旋转内管以开启槽口，待样品流满内管后，再旋转内管以关闭槽口。抽出取样器，立即将样品倒人盛样器内口每袋抽取样品的数量应与2.4.1.1基本一致。每批所抽取的样品总量应不少于4kg.2.4-2散积抽样按2.2.2规定的取样点，逐点抽取样品。将取样器(2.3.2)槽口关闭，以倾斜45‘角度插人货堆至相应深度，旋转取样器内管以开启槽口，待样品流满内管后，再旋转内管以关闭槽口抽出取样器，立即将样品倒人盛样器内，从各点所抽取样品的数量应基本保持一致。每批所抽取的样品总量应不少于4kg。2.4.3大样缩分袋装样品合并从倒包和袋内抽样所取全部样品，倒于分样布上，用分样板按四分法缩分样品至不少于2kg，倒人盛样器内，加封后标明标记，并及时送交实验室。散积样品:将抽取的全部样品，倒于分样板上。以下按上述袋装样品方法进行。2.5试样制备2.5.1制样工具2.5.1.1磨碎机。2.5门2筛子:2。目筛。2.5.1.3分样板。2.5.1.4盛样瓶:具塞广口瓶2.5.2制样方法将样品按四分法缩分至500g，用磨碎机全部磨碎并通过20目筛。混匀，均分成两份作为试样，分装人洁净的盛样瓶内，密闭，标明标记。2.6试样保存将试样于一5c以下避光保存。注在抽样及制样的操作过程中，必须防止样品受到污染或发生残留物含量的变化3测定方法11方法提要试样中残留的快杀稗用丙酮提取，提取液经蒸发后用水浸出。然后用二氯甲烷先于碱性溶液、后于酸性溶液进行液一液分配净化。所得二氯甲烷溶液蒸去溶剂，后配成丙酮溶液，用重氮甲烷进行甲酷化。然后溶液经过硅酸镁柱净化，所得洗脱液经蒸干后，残渣用石油醚溶解并定容。溶液供配有电子俘获检测器的气相色谱仪测定，外标法定量。3.2试剂和 材料 关于××同志的政审材料调查表环保先进个人材料国家普通话测试材料农民专业合作社注销四查四问剖析材料 sN/T1017.5-2002除另有规定外，所用试剂均为分析纯，水为蒸馏水。3.2-1丙酮;重蒸馏。3.2.2石油醚:重蒸馏.3.2.3无水硫酸钠:650C灼烧4h,贮于密封容器中备用。3-2,4二氯EP烷:重蒸馏。3.2.5乙醚;重蒸馏。3.2.6N一甲基一N一亚硝基一4一甲苯磺酸胺:分析纯。3.2.7氢氧化钾溶液:10mol/L浓度。3.2.8重氮甲烷:置4mL乙醚和2mL10mol/I氢氧化钾溶液于反应管中.加人Sm工乙醚溶解的2gN一甲基-N一亚硝基一4一甲苯磺酸胺的溶液，平稳吹氮气5min，收集反应管中乙醚溶液。3.2.9硫酸分析纯。用时配成3mol/L浓度。3.2-10氢氧化钠溶液:1mol/L浓度。3.2-11碳酸氢钠分析纯。3.2.12硅酸镁:层析用,100--200目。用前于130C活化4h.冷却后贮于密封容器中备用3.2门3快杀稗标准品:纯度)99%.3.2.14快杀稗标准溶液:准确称取适量的快杀稗标准品，用少量的丙酮溶解，并以石油醚配制成浓度为1.00mg/ml的标准储备液。根据需要再用石油醚稀释成适用浓度的标准工作溶液。3.3仪器和设备3.3,1气相色谱仪:配有电子俘获检测器口13.2振荡器。3.3.3旋转蒸发器。13.4硅酸镁柱:25cmX1.5cm(i.d.)，自下而上依次填装2cm高无水硫酸钠,15g硅酸镁,2cm高无水硫酸钠。使用前用50mL石油醚预淋洗。3.3.5微量注射器:10pLe3.4测定步骤3.4.1提取称取试样20g精确至。.1g)于250mL具塞锥形瓶中，加人100mL丙酮，振荡提取30min。将提取液过滤于250ml一心形瓶中。用50ml丙酮分两次洗涤残渣，洗涤液经过滤后合并于上述心形瓶中于40C水浴中减压蒸至近干，加人lom工，水和5g碳酸氢钠。溶解后，加人约2m工，1mol/l,氢氧化钠溶液，调pH值为9士。.2充分混合后移人分液漏斗中，用20ml_水分二次洗涤，溶液合并于分液漏斗中。于上述分液漏斗中加人100ml，二氯甲烷，振摇5min,静置分层。弃去下层有机相。再用2X50ml-二氯甲烷重复洗涤水相两次。于水相中加人约5ml.3mot/1-硫酸溶液使pH值为2士0.2加人100ml二氯甲烷，振荡提取5min，静置分层。分出下层有机相于锥形瓶中。水相再用2X50ml二氯甲烷重复提取两次，合并有机相。经无水硫酸钠脱水，置于具塞心形瓶中，于40C水浴中旋转浓缩至近于，加人2ml_丙酮以溶解残渣。3.4-2衍生化干上述丙酮溶液中加人5ml,重氮甲烷溶液，密封，置60C水浴中反应10min.蒸除溶剂，用sml.石油醚溶解。3.4.3净化将上述溶液倾人硅酸镁柱(3.3.4)中，用200mL石油醚分数次洗柱，弃去流出液.然后用100ml.丙酮一石油醚(9+1)洗脱，收集洗脱液于心形瓶中，于40C水浴中旋转浓缩至近干。用石油醚溶解并移人容量瓶中定容至5.0ml.供气相色谱测定。SN/T1017.5-20023.4.4标准物衍生化准确移取适当浓度的快杀稗标准工作液于具塞心形瓶中，干40C水浴中旋转浓缩至近干，加人2ml_丙酮以溶解残渣。以下按3.4.2操作。3.4.5测定3}4.5-1色谱条件a)色谱柱:25inX0.53m.(i.d.),膜厚1.0um,BP10石英毛细管柱，或相当者;b)色谱柱温度:240C;C)进样口温度:280C;d)检测器温度:290C;e)载气:氮气，纯度)99.9900,10ml./min;f)尾吹气:氮气，纯度>99.99%,50m工_/min;9)进样量:1PI。3.4.5.2色谱测定根据样液中被测农药含量情况，选定浓度相近的标准工作溶液标准工作溶液和待测样液中甲基化农药的响应值均应在仪器检测的线性范围内。对标准工作溶液与样液等体积参插进样测定。在上述色谱条件下，快杀稗甲酷的保留时间约为3min标准品的气相色谱图见附录A中图A1,3.4.6空白试验除不加试样外均按上述测定步骤进行。I5结果计算和表述用色谱数据处理机或按式(2)计算试样中快杀稗残留含量:·‘·vx=h(2)h,。m式中:x—试样中快杀稗残留含量,mg/kg;h—样液中快杀稗甲酷的色谱峰高,mm;人—标准工作液中决杀稗甲醋的色谱峰高，mm;。一一标准工作液中快杀稗的浓度。ug/mL;v—样液最终定容体积，ml;m最终样液所代表的试样量，9注计算结果需将空白值扣除。4测定低限、回收率4门测定低限本方法的测定低限为。.05mg/kg.4.2回收率4.2.1糙米中快杀稗的添加浓度及其回收率实验数据:在0.05mg/kgB寸，回收率为89.2%;在0.50mg/kg时，回收率为87.90/n;在1.00mg/kg时，回收率为82.90004.2.2玉米中快杀稗的添加浓度及其回收率实验数据:在。.05mg/kg时，回收率为92.7%;在0.50mg/kg时，回收率为91.3%;在1.00mg/kg时，回收率为92.2%04.2-3小麦中快杀稗的添加浓度及其回收率实验数据:SN/T1017.5-2002在。.05mg/kg时，回收率为88.2%;在。.50mg/kg时.回收率为92.70o;在1.00mg/kg时，回收率为88.2%.4.2.4大豆中快杀稗的添加浓度及其回收率实验数据:在。.05mg/kg时，回收率为82.6%;在0.50mg/kg时，回收率为83.10o;在1.00mg/kg时，回收率为80.9000sx/T1017.5-2002附录A(提示的附录)快杀稗甲醋标准品色谱图图A1快杀稗甲醋标准品的气相色谱图SN/T1017.5-2002ForewordThisstandardwasdraftedinaccordancewiththerequirementsofGB/T1.1一1993"Directivesfortheworkofstandardization-Unit1:Draftingandpresentationofstandards-Part1:Generalrulesfordraftingstandards"andSN/T0001-1995"Generalrulesfordraftingthestandardmethodsforthedeterminationofpesticide,veterinarydrugresiduesandbiotoxinsincommoditiesforexport".Themethodofdeterminationofthisstandardwasdraftedbyreferringtorelevantdomesticandforeignliteraturesthroughresearch,modificationandverification.Inaddition,methodsofsamplingandsamplepreparationarealsospecifiedinthisstandard.Thislimitofdeterminationisdefinedinthisstandardonthebasisofthecurrentinternationalmaximumlimitsforquincloracresiduesincerealsandoilseedsandthesensitivityofthemethod.AnnexAofthisstandardisaninformativeannexThisstandardwasproposedbyandisunderthechargeofChinaNationalRegulatoryCommissionforCertificationandAccreditation.ThisstandardwasdraftedbyJilinEntry-ExitInspectionandQuarantineBureauofthePeople'sRepublicofChina.ThemaindraftersofthisstandardareLiQingcai,RongHui,ZhengXiming,HongQuanchunandQuZhongwen.ThisstandardisaprofessionalstandardpromulgatedforthefirsttimeNote:ThisEnglishversion,atranslationfromtheChinesetext,issolelyforguidanceProfessionalStandardofthePeople'sRepublicofChinaforEntry-ExitInspectionandQuarantineSN/T1017.5-2002Methodforthedeterminationofquincloracresiduesincerealsandoilseedsforexport1ScopeThisstandardspecifiesthemethodofsampling,samplepreparationanddeterminationofquinclo-racresiduesbygaschromatographyincerealsandoilseedsforexport.Thisstandardisapplicabletothedeterminationofquincloracresiduescontentinunpolishedrichmaize,soyabeanandwheatforexport2Samplingandsamplepreparation2.1inspectiontotEachinspectionlotshouldnotexceed200tonnesAninspectionlotof200tonnes,forunpolishedrichorwheatinbags,shallbeca4000bags;formaizeorsoyabeaninbags,shallca2200bagsThecargoofmaizeorsoyabeanissometimesinbulk.Thecharacteristicsofthecargowithinthesameinspectionlot,suchaspacking,mark,origin,gradeetc..shouldbethesame.2.2Quantityofsampletaken2.2.1CargoinbagsCalculatethenumberofbagstobetakenbyformula(1)a二、缅(1)whereN-totalnumberofbagsinalot;a-numberofbagstobetaken.Note.Ifvalueaiswithdecimal,roundofthedecimalpart,whichisaddedasunitytotheintegralpartofa2.2.2Cargoinbulk(maizeorsoyabean)Theheightofthecargopileshouldnotexceed2m.SetupareasandspotsforsamplingontheApprovedbyGeneralAdministrationof即alityImplementedfrom2002-0e-c1资upervision,inspectionandQuarantine少__thePeoplesRepublicofChinaon2002-u-,cSN/T1017.5-2002pilesurface.50m'isconsideredasanarea,inwhich5spotsshallbefixed,oneinthecentreandfouratfourcomers(1mfromthemargin)ofthearea.Foranadditionalarea,threemoresamplingspotsshallbefixed.2.3Samplingtools2.3.1Metallicsampler;length(includinghandle):55cm;diameter:1.5cm一2.0cm;groovelength:longerthanhalfthediagonallengthofthebag.2.3.2Metallicdouble-casingsampler;length1m,2m(bothincludinghandle)withsomeslotsondeferentsectionsandrespectivelyatthesameheightsforbothinnerandoutercasings;lengthofslots:15cm一20cm,widthoftheslots:2.0cm一2.5cm;insidediameteroftheinnercasing:2.5cm~3.0cm;theprobelengthofthesampler:ca7cm.2.3.3Samplingshovelorladle.2.3.4Plateforquartering.2.3.5Samplecontainer:Canorbag,whichcanbesealed2.3.6Cloth(orothersuitablematerial)sheet:Forsampledividing(quartering)2.4Samplingprocedure2.4.1Forcargoinbags2.4.1.1SamplingbyemptingoutDraw10percentofthenumberofbagsspecifiedin2.2.1(notlessthan3bags)atanypartofthepileatrandom.Unseamandopenthebag,andlayitonacleanclothsheet(orothercleansheet)，Grasptighttwocornersofthebagbotomandraiseuptoanangleof450,tugbackwardforca1muntilallcontentofthebagisemptiedout.Checkwhetherthequalityofgoodsisuniformwithinandbetweenthebags.Afterconfirmingthegoodsareinnormalcondition,scoopupthesamplefromdiferentpartsoftheout-pouredcontentatrandom,andpromptlyplaceinasamplecontain-er.Thequantityofthesampledrawnfromeachbagshouldbebasicallythesame.2.4.1.2SamplingfrominsidethebagsDrawthesamplesfromthenumberofbagsspecifiedin2.2.1(bydeductingthenumberofbagsdrawnin2.4.1.1).Alongthesinewaveofthepile,drawthesamplesfromthebagsoftheupper,middleandlowerpartsaroundthepileatrandom.Forunpolishedrice,wheat,maizeorsoyabeanproceedasfollows:Forunpolishedriceorwheat,insertthemetallicsampler(2.3.1)，withitsgroovefacingdown-ward,diagonallyintoeachbag,thenturnthesampler1800,drawoutthesamplerandpromptlypourthesampleintoacontainer.Formaizeorsoyabean,insertthemetallicdouble-casingsampler(2.3.2,length1m)(theslotsshouldbeclosedwhiteinsertingin)diagonallyintoeachbag.Turntheinnercasingtoopentheslotssothatthesamplemayfilluptheinnertube.Againturntheinnercasingtoclosetheslots;吃)SN/T1017.5-2002anddrawoutthesampler.Promptlypourthesampleintoasamplecontainer.Theamountofsampledrawnfromeachbagshouldbebasicallythesameasin2.4.1.t.Thetotalweightofthesampleofeachlotshouldbenotlessthan4kg.2.4.2SamplingfromthecargoinbulkInsertthedouble-casingsampler(2.3.2)successivelyintothepileatthespotsspecifiedin2.2.2,toappropriatedepthat450(theslotsshouldbeclosedwhileinsertingin)Jurntheinnercasingtoopentheslotssothatthesamplemayfilluptheinnertube.Againturntheinnercasingtoclosetheslotsanddrawoutthesampler.Promptlypourthesampleintoasamplecontainer.Theamountofsampledrawnfromallthespotsshallbebasicallythesame.Thetotalweightoftherepresentativesampleofeachlotshouldbenotlessthan4kg.2.4.3ReductionofgrosssampleForcargoinbags:Pourallthesamples(fromboth2.4.1.1and2.4.1.2)onacleansheet.Reducetonotlessthan2kgbyquarteringwithaplate.Placeinasamplecontainer,scal,labelandsendtothelaboratoryintimeForcargoinbulk:Pourallthedrawnsampleontoacleansheetandproceedasforcargoinbagsdescribedabove.2.5Preparationoftestsample2.5.1Tools2.5.1.1Grinder.2.5.1.2Sieve:20-meshsieve.2.5.1.3Plateforquartering.2.5.1.4Samplecontainer:Wide-mouthbotle,withgroundstopper.2.5.2ProcedureRuducethesamplebyquarteringtoca500g,gradewithagrinder(2.5.1.1)andletallpassthrougha20-meshsieve.MixthoroughlyanddivideintotwoequalportionsasthetestsamplesPlaceinsamplecontainers,seaiandlabel.2.6StorageoftestsampleThetestsamplesshouldbestoredbelow一50Candkeptawayfromlight.Note:Inthecourseofsamplingandsamplepreparation.precautionmustbetakentoavoidcontaminationoranyfac-torsthatmaycausethechangeofresiduecontent.3MethodofdeterminationllSN/T1017.5-20023.1PrincipleThequincloracresiduesinthetestsampleareextractedwithacetone,theextractisevaporatedandleachedwithwater.Theaqueoussolutionispartitionedwithdichloromethanefirstinalkalineandtheninacidmedium.Thedichloromethaneextractisevaporatedandleachedwithacetone.Thequincloracinacetonesolutionismethylatedwithmethylazideandcleanedupbypassingthroughamagnesiumsilicatecolumn.Theeluateiseva-porateandmadeuptoadefinitevolumewithpetroleumether.Determinationismadebymeansofagaschromatographequippedwithelectroncapturedetector,usingexternalstandardmethod.3.2ReagentsandmaterialsUnlessotherwisespecified,allthereagentsusedshouldbeanalyticallypure,"water"isdistilledwater.3.2.1Acetone:Redistilled3.2.2Petroleumether:Redistilled3.2.3Anhydroussodiumsulfate:Igniteat6500Cfor4handkeepinatightlyclosedcontainer3.2.4Dichloromethane:Redistilled3.2.5Diethylether:Redistilled3.2.6N-methyl-N-nitroso-4-toluenesulfonamide3.2.7Potassiumhydroxidesolution门0mol/L.3.2.8Methylazide:Place4mLofetherand2mLof10mol/Lpotassiumhydroxidesolutionintoareactiontube,add5mLofethersolutionof2gofN一methyl-N-nitroso-4-toluenesulfonamide,andpassnitrogengasslowlyfor5min.Keeptheethersolutioninthereactiontube.3.2.9Sulphuricacidsolution:3mol/L3.2.10Sodiumhydroxidesolution门mol/L3.2.11Sodiumbicarbonate.3.2.12Magnesiumsilicate:Forchromatography.100一200mesh.Beforeuse,heatat1300Cfor4h,andkeepinatightlyclosedcontainer3.2.13Quincloracstandard:Purity,99%3.2.14Quincloracstandardsolution:Accuratelyweighanadequateamountofquincloracstan-dard,dissolveinasmallvolumeofacetone.Dilutewithpetroleumethertoformastandardstocksolutionof1.00mg/mLinconcentration.Thendilutethestandardstocksolutionwithpetroleumethertotherequiredconcentrationasthestandardworkingsolution.SN/下1017.5-20023.3Apparatusandequipment3.3.1Gaschromatograph,equippedwithelectroncapturedetector3.3.2Shaker.3.3.3Rotaryevaporator3.3.4Magnesiumsilicatecolumn:25cmx1.5cm(i.d.),addinsequence2cm(height)ofan-hydroussodiumsulfate,15gofmagnesiumsilicateand2cm(height)ofanhydroussodiumsul-fate.Rinsethecolumnwith50mLofpetroleumetherbeforeuse.3.3.5Micro-syringe:10RL.3.4Procedure3.4.1ExtractionWeighca20g(accurateto0.1g)ofthetestsampleintoa250mLconicalflaskwithstopper.Add100mLofacetoneandextractfor30min.Filtertheextractintoa250mLpear-shapedbotle.Washtheresiduetwicewith50mL(intotal)ofacetone,filterandcombinethewashingsinthesamepearshapedbotle.Evaporatethesolutionunderreducedpressuretoneardryness,add10mLofwaterand5gsodiumbicarbonate,solution,thenadjustwithabout2mLof1mol/Lsodiumhy-droxidesolution,thepH=9=0.2.Mixandtransfertoaseparator,washingthepear-shapedbotlewith20mLofwaterandcollectingthewashingsinthesameseparator.Add100mLofdichloromethaneintotheaboveseparator,shakefor5minandsetasideforsepa-rating.Discardthelowerorganiclayer.Washtheaqueouslayerwith2x50MLofdichloromethane.Totheaqueouslayeracidifywithsulphuricacidsolutionca5mL(3mot/L)topH二2s0.2,add100mLdichloromethaneandextractfor5min.Drainthelowerphasetoaconicalflask,andtheaqueousphaseisextractedsuccessivelywithtwo50mLportionsofdichloromethane.Combinetheorganicphaseinthesameconicalflask.Dehydratewithanhydroussodiumsulfate,transferthedichloromethaneextractintoapear-shapedbotle,androtary-evapo-ratetoneardrynesswithabathtemperaturebelow40'C.Dissolvetheresiduewith2mLoface-tone.3.4.2DerivatizationTotheabovesolutionadd5mLmethylazidesolution(3.2.9).stopperandkeepitinwaterbothat600C10min.Evaporateoftheetheranddissolvetheresiduewith5mLofpetroleumether.3.4.3CleanupTransferthesolutionintothemagnesiumsilicatecolumn,washthecolumnwith200mLofpetroleumetheranddiscardtheefluent.Thenelutewith100mLofpetroleumether-acetonesolu-tion(1+9)mixedsolutionandcollecttheeluatesinapear-shapedbottle.Rotary-evaporatetoneardrynessinawater-bathbelow40'C,andthenexactlydilutetheconcentratedsolutionto5.00r.iLwithpetroleumetherforGCdetermination.3.4.4Derivatizationofthestandardl苏SN/T1017.5-2002Accuratelypipetquincloracstandardworkingsolutionofsuitableconcentrationin一toapea卜r-Ssnh8apPedbotle,rotary-evaporatetoneardrynesswithabathtemperaturebelow4landdissolvetheresiduewith2mLofacetone.Thenproceedasinsection3.4.2forderivatization,finallystillmakeupthesolutionto5.0mLwithpetroleumetherforGCdetermination.3.4.5Determination3.4.5.1GCoperatingconditiona)Chromatographiccolumn:25mx0.53mm(i.d.)，1.0pmfilmthickness,BP10,silicacapillarycolumnortheequivalent;b)Columntemperature:240'C;c)Injectiontemperature:280℃;d)Detectortemperature:290℃;e)Carriergas:Nitrogen,purity〕99.99%,10mL/min;f)Make-upgas:Nitrogen,purity,99.99%,50mL/min;g)Injectionvolume:1gL.3.4.5.2GCdeterminationAccordingtotheapproximateconcentrationofpesticideinthesamplesolution,selectthestandardworkingsolutionwithsimilarpeakheighttothatofthesamplesolution.Theresponsesofmethy-latedpesticideinthestandardworkingsolutionandsamplesolutionshouldbewithinthelinearrangeoftheinstrumentaldetection.Thestandardworkingsolutionshouldberandomlyinjectedin-betweentheinjectionsofthesamplesolutionofequalvolume.Undertheabovechromatographiccondition,theretentiontimeofquincloracmethylesterisca3min.Forgaschromatogramofthestandard,seefigureAIinannexA.3.4.6BlanktestTheoperationoftheblanktestisthesameasthatdescribedinthemethodofdetermination,butwith0missionofsampleaddition.3.5CalculationandexpressionoftheresultCalculatethecontentofquincloracresiduesinthetestsamplebyGCdataprocessororaccordingtoformula(2).h-c-V入=~，石一r(2)门，门〕whereX-theresiduecontentofquincloracinthetextsample,mg/kg;h-thepeakheightofquincloracmethylesterinthesamplesolution,mm;h,-thepeakheightofquincloracmethylesterinthestandardworkingsolution,mm;c-theconcentrationofquincloracinthestandardworkingsolution,frg/mL;V-thefinalvolumeofthesamplesolution,mL;m-thecorrespondingmassofthetestsampleinthefinalsamplesolution,g.Note:Theblankvalueshouldbesubtractedfromtheaboveresultofcalculation14SN/T1017.5-20024Limitofdeterminationandrecovery4.1LimitofdeterminationThelimitofdeterminationofthismethodis0.05mg/kg.4.2Recovery4.2.1RecoveryofquincloracinunpolishedriceAccordingtotheexperimentaldata,thefortifyingconcentrationofquincloracanditscorrespond-ingrecoveriesare:0.05mg/kg,therecovery89.2%;0.50mg/kg,therecovery87.9%;1.00mg/kg,therecovery82.9%.4.2.2RecoveryofquincloracinmaizeAccordingtotheexperimentaldata,thefortifyingconcentrationofquincloracanditscorrespond-mgrecoveriesare:0.05mg/kg,therecovery92.7%;0.50mg/kg,therecovery91.3%;1.00mg/kg,therecovery92.2.4.2.3RecoveryofquincloracinwheatAccordingtotheexperimentaldata,thefortifyingconcentrationofquincloracanditscorrespondingrecoveriesare:0.05mg/kg,therecovery88.2;0.50mg/kg,therecovery92.7%;1.00mg/kg,therecovery88.2%.4.2.4RecoveryofquincloracinsoyabeanAccordingtotheexperimentaldata,thefortifyingconcentrationofquincloracanditscorrespond-ingrecoveriesare:0.05mg/kg,therecovery82.6%;0.50mg/kg,therecovery83.1%;1.00mg/kg,therecovery80.9.1几SN/T1017.5-2002AnnexA(informative)GaschromatogramofquincloracmethylesterstandardFig.AlGaschromatogramofquincloracmethylesterstandard1日