本标准规定了出口禽肉中二氯二甲毗pit酚残留量检验的抽样、制样和气相色谱测定方法。本标准适用于出口冻鸡中二氯二甲毗pit酚残留量的检验。 SN/T 0212.3-1993 出口禽肉中二氯二甲呲啶酚残留量检验方法 丙酰化--气相色谱法 SN/T0212.3-1993 标准下载解压密码：www.bzxz.net

中华人民共和国进出口商品检验行业标准SN/T 0212.3—93
出口禽肉中二氯二甲吡啶酚
残留量检验方法
丙酰化一气相色谱法
Method for determiration of clopido!residues in poullry neat for exportPropionylation-gas chronatography1993:06-04发布
1993-0801实施
中华人民共和国国家进出日商品检验局：．发布中华人民共和国进出口商品拾验行业标准出口禽肉中兰氯兰甲吡啶酚
残留量检验方法
丙酰化气相色谱法
Methud for deturminnliun uf opidelresidues in pouttry meator expor]Propionyletlon-gns chromatography主题内容与适用范匹
SN/T 0212.3-93
本标难规定了出口离肉中二氧二甲吡啶盼就留日检验的抛样、制样科气相色谐避定方益，本标造质二出鸡中二氛二甲吡魔酚残图量的检验。2抽样和制样
2. 1检验批
以不超过2500什商品为-检验批。同一拉验批的商品应具有相间特征，如包装、标记、产地、或格和等级等。2.2抽数量
批盘<件）
26-~100
101-~2:0
251--500
501~-1 000
2.3抽样法
最断抽样数（件）
按2.2规定的抽样件数随机抽取源件并启：每件至少取一袋作为原始样品原始样品总品不少于2kg·放入清洁案器内，如封尼，探明标记，及时送交实验室。2.4试样制备
从舞装原始择品中取出部分有代表性择品，将可食部分敬入高癌组织按碎机中摘碎均与，充分混今用四办法频分自不少于1C的试样。装人请活的穿器内，加封后，标明标记。2.5试样保存
·将试样于一18它冷冻保存。
注：在抽样及制样注中，必须范止样品受到污微或发生政雷物量量的变化，3·测定方法
3.1方法标要
中华人民共和国国家进出口商品检验局1993-06-叫批准1993-08-01实施
SN/T 0212.3—93bzxz.net
用甲醇担取内样中二氯二吡啶酚，经化铝柱净化：除去脂肪和色案.以内酸酐反应转化成相应的酯。用内径为D.53切毛细誉生气相色谱法（于俘获检测器》测定，外标法定量。3-2试剂利材料
3.2.1无水硫酸钙：分析纯，轻650℃约烧46。低于平燥器内各用，3.2.2甲醇分析纯，经全玻璃装重幕例，收巢64~55℃馅分。3.2.3瓶化铝：中性层析用，粒度100~200筛日，在800℃灼烧3h，减人子烘器中备用32.4.氧化，中性层析用，校度10g~20端月，在.8000灼烧3h.并在130烘箱中烘烤1h后，放人干燥器中备用，
32.5丙酸配：分折纯、经全玻璃装写度燕馅。3.2.6吡啶，色满纯。
3.2.7·动鸿：Clile545,使用前用甲醇洗萨两次；每次说泡半小时。3.2.B回磷酸销：优吸使，下无水，在配制溶液前，应将货试剂布热流滤中单结函-次。3.2.9四谢酸销溶液：0.1iot/L，取38.0g四硼酸钠（3.2.8)落1000m蒸诺水中，3.2.10蒸恂水，取兹增水100mL，用正凹烷1ml.提取.在应用的色谱策件下，取5pL提取象注入气色谱收内，该正己烷在色举图上应无下被题组分的杂峰，3.2.11正己烷分析纯，蒸简以您67~69亡烯分。取500ml正已烷，通过或充13cm高度中性机化铅（3.2.4)层析.20mm3.2.13二款二中份标准品：纯度多99次，：3.2.14二繁二币此院阶标准轻液（6.1mg/mL）：南解10.0mg二氯二中吡啶必标准品于少最币降中.以甲萨准确定容垒100mL，搭写，作为标產培备奔液。权据需要再配或适用浓的标准工作箱液。3.3收和设备
3.3.1气相色谱仪，配备电于件缺检测器和热式毛维暂性头进样器。3.3.2微注射器：10mL,50.
33.3高建组织圾碎。
3.3.4：康式带药器
3.3.5能转裁发器，
3.3.6恒温水潜蜗、
3.37净化壮：20mm3.4测定步廉，
3.4.1·格取：.
取经级准匀的试样约20多（储确到0.01g）于25DmL具塞锥型瓶中，加入52mL甲醇利g叻滤剂于报菌器.上提取.301mim在学底漏斗内铺F.2g助燃剂+油提取减.用40mL甲醇分?次录维型瓶共将洗换液移人平底满斗，滤液亲量转传到105mL溶量规中，用少盈甲静彩次洗钱滤来统浓收禁于容量瓶中，用中定穿.
3.4.2净化
润多减管准确吸取上述滤孩20imL.移入氧化铝生（3.3.7)中，以2mL/min流速微出.用40m)，甲够洗柱内壁.液及洗液接收于100.mL烧杯中，用，50亡水浴的旗转热发器或在50它水铅史以氮气滋将落剂激于。用2-3mL甲脉落解残液，举定量转入15mL带螺旋盖试管（3-3.8），用氧气流将甲醇涨统至约0.5mL。
iSN/T:0212:3:93
3.4.3酯化
在上述试管中依饮准确加人益Lo.1mbl四酬酸钠骼波*1m己控25腹和56L丙敢酐。加寒，振据1min，在3000r/min下高心5nin，将上层正，己境移人另一干净具试中，经加少量无永蔬贱钠脱水后，供气相色谱分析、3.4.4标准物弱化
取适用浓度的标准工作溶液，用策气将件积涨缩至0.5mL，要3.4.3进行酯化反应，3.4.5测定
3.4.5.1测定色谱条件：
毛细臂免谱生：B10链合相，c.53mm(id)×3Cm熔融石类制柱证：165℃。
选样日温座：250℃
冷到温度250℃
载气.居吹气：款气（299.99%>性流盐3mL/min居以气流整33mL/min。【进样方式，科头进样力式，
3.4.5.2他谱测定：分别准确注人1L经酯化后的样品落液及标准工作减于气柜色谐仪中，按3.4.5.1条件进行色谐分析。购应值片应在仪器检滤的线性范围之内。二氧二甲吡庭两醛的保留时间约为12rrin35空白试跑：愉不称取样品外，按上述测定步骤进行。3.6结果11算和表述
用色谱数据处谨机或按下式计算样品中二氣二甲吡啶酚强留含基：x=hc.P
或中：x
样品中二款二中吡啶爵合贝，mg/kg样减中二氯二甲此噬酸丙醛高.1mmA
力，—标准工作溶液中.熟中吡啶酚丙酯峰高，mm一标准工作潜波巾二套二甲心吨酚浓度，/mL；V—最终样液的体积，
最终样我所代表的样品耳盐R：
注，原自位应从让瓦品来中扣除，.4测定低限、回收率
4.1测定年限
本法测定低限为.srrg/kg
4.2回收率
间收率的实验数期：二象二甲批晚阶酬加添度在005.0.050mg/kg范用内，网收率火74系~1
附加说明；
本标准内中华人民共和国国家连出口商品检验所提出。本标准由华人民共和润大法进出口商品检验局负责起单。3
SN/T D212.3--93
本标难主要起草人高晓敏，许，鹅乃强。考文献
AOAC Juurna? nf Offivil Methud ol Anelysis,Vol 6,2,198,Professional Stamlard of the People's Republle of Chinafor Import and Export Commodity InspectionSN/T0212.3—93
Method for determination of clopidolresidues'in poultry meat for export-Propionylation-gas chromatogrphyScopeand fieldof appllcattoaThis sitandard specifies the method of sampling, eamp.e pre[piraticu unul dutermirutiun by gaschramatpgraphy of clopidol residues in peultry meat fot export.'Taig stundart is aprlieuble to the deecrmir.ation af clapidal residues in broiters fur export.2 Sampiing andsampir prrparation2.1 Inggertion lot
The quentity of sn inspecton lat shauld not be more than 2 5on packageeTl rharirnristits gif the uuitgu withit che aamc inspection lat, sueh as packing ,mark. ozigin.specitication and Rrade, should be the same.. 2.2 Quantiry of sample lakenNunbcr of packages in esch ingpectioni lor Miximum number of packages to be taken1-23
26—10
:101 :250.
251—500
1001-260
2.3 Samplinr procedure
A number of paekegty'syeeified in 2, 2 ere taken at 'random and opened ove by rupa. Frurn euch a:leust one hug shit be'taknn'ni prinury kirnplu, Theitutel.wcight of all primary' eauples ehould tunclers thitu 2 ke, wlich ehall be placed in i clean cauntainer, Rmnteal, islhrlked and 'sene to Eaboratory intinc
2.4,Ireparationof test samplePart of reprcscntative gumple is tekeont fro esoti bag.uf ehe'primary aarople and tlhe edibsle pciliuntof wliua sn houwgerieud hy grinding ii a meat:gaider. The humogenized sample'is thorougbly nixedand,rednced tn'al leaai J aga. by juarteringgThe'tesl saniple is jlared in'clcan coticainer'which issealed and labeled.
2.5Srorege of tes: sample
The test aynzle shiould bc stored at-lgT.Mothoue'fatlinad sanpleeatio,retion take nid mnnt.Appraved by the State Administratiin ofImportand Export CommodltyIaspectiou ofthe Peopie's Hepubllc or Chlan on Jan, 4.1993Impkementea from'Aug. 1, 1993SN/T 0212.3-93
Faciors wrhich mny sinl.t'th.ichungt af Eaidhe contehi.3Method or delerminatiaa
31Priniciple
The clppidol ig extracted from the.meat.tissucs:with methanpl: andrleaned up on an alutnine cal-unn to remove the fat and impuritiea..Clopido, ig esterified with propianic.ashydride..forrning elopidalpragionate which is determined by 0, 53 rim(id) cupillary gas ehromatography with electron capeurcdeterror, using externel stanrierti.3.2-ReagunAtrarariate
3. 2. 1 Anbydrpue eadium suifate :Analytical grade, iguite at 65 tor e h; wnd'stare'in an air-tighiconaine
3.2.2Methanol,Aaalytical grade.fedisrillwith.nll.alsea:apparatuarcollest.the.disilete,of-6465
3. 2. 3 Alumins; Neutral frr chrurrualagriphie. usr, 1n)-20t resh+ heuted at 30'C fut 3 h, store ica lesiccator.
3.2.4 Alunina:Neutral for chromatographic use,100..200 meh,ignite at R00.for,3h:theiheat at130c forih in an:ren.Store.inadesiccatotri.2 5.Prepionie anbydridet.Analytical grade, redistill:soith all alsgs.appararus,3.2.6Pyridine: Chiromatographic griue.3. 2.7Pilur id, Celile 545, waeh winl, methauol 1wiue by raakinugrioipethanal, Euy go. chirg.heloueuSt
3.2. B Dizadiu: tetraborate: GR grade: anhydrcus. Recrystallize thiealt from hot solution beforeuse lor preparing the soluriori.3. 2. 9 Ehgodium tetreharete solurion, 0. 1 mol/L. Diasolve 38. 0 gidigodiam'tetraborazc(3. 2. 8inI UiQ rl. of redistilled watrr.3. 2. 10 Dietilled waler : Exthaer 10 nl. distilled water with 10 mL.hexane: Adjust the Rar chro-matograph under the specified operating conditions and iniect 5 μL ofithe extract: Na interfering peaksshall appear cn the chromarogram3.2.11r-nHcxapca.ngiytical grade,redistill aad collcetthedistillateof 6769.Pasg:50mL f:-hexenc:through.the,column:200 nimX20.mn(id)Jwhich.is.pucked witlr13.xm.of.aluminu:(&-2:4):lowrte ca2,al./nin
3.2.2Acetanc: Anslyisal grade3.2.13Clopidol standatd:Furity-99%.3.2.14iClopidol atandad.aolutionfo.1mg/mL).Disaolve110.omgfrthe-stendard.elopidol:incaJEml..of methanol ': and idilute co. mark with: methaaol.in;s i( k. ypliniel.r ir. Flask,! mix.thorjugily ; i.lhe, stilard,slusk olutiw, frurn whiel-slambard working'knlutiosin of suitaile:cgumirrgitrian re pre:Parad acconlnk tn ile teguiremeitt.3.3Apparatus and equipment
3. 3. 1 Gas chromatograph cquipped with the electron't'apture derecto: landrheaied-type oh-tolurm:capiliary.jnjecior
3-3.?Miero ayiinzeu aL, 5o wL.3. 3. 3 High aperd blencer.
3.3.4 Shaher..
3.3.5Roiary evaporator.
SN/T 0212.393
3.3.6Caostan: ternperaturewatar-bath,3.3.7Aluininncoluma (foreleaaup).200meX20rm(id)gasseulumn,pn:keaC.5cmabanrlericotton (cxtr2cted with aortone-hnkine<2+3>.fi>r 3 h) at thr: hat1aof the column and fill in 16 g alu-mine (3. 2. 3) hy knockiag ightly.Rinse the column with 40 mL methanol before use.3.3.8Screw-cap tubex,15mL(130 mmX13mm),with plastic $crew cap andteflon lined3. 3.9Centrifuger Speed rata 3 ooo t/min.3.319 Nitogen,Purityg9.%
3.4Prucerluru
3.4.1Extractian
Weigh ca 2J gfacturate to 0, O1 g) of the mixd sempte int 250 mL conical flash witli s1our, eulal50 ml rnethano and 3 g filter and, cxtrect for 0 rrin n a xhaker, Filler the extiat:1 with auctinrthrDugh, Buchaer Jillt vunleining a hed or 8 p filter aid, Wash the flaek writh 3 portione (totalling 4)nt,) of methanal and itaarfer eacl porcion of methznol into the Buchner filter for weshing the cake onthe Buchaer and also the filter. Transfer guratitatively Ene combined filtrete inco s loo ml volumetriclask. Wesh the surtion flask geveral tines with fnw mT.af maihuanol mnd rullecl 1he washings ir: therme vulursetriclask,Dilute fi markwith methanol.3.4.2 Ciean up.
P'ipet accutately 20 roL of the ebave fitrate intu -he alumine calumn(3. s. 7) andl ie jiauss tiruughthe colurur. into a 1uo mL beker wil a rale: al 2 J./inin, Wash il teilumel will 40 rnt. of mellintnlFnd caurnlinxt ihe washsintg in the tame benker. Evapnrate Lo crynese in a waler bith at 5ot yritl: Io-tary evagorator or under a'skream of tuitrogen. Dissolve the reridue with 2 3 ml of methanol endtransferquaneitatively inio thc 15 nL gcrew-cap tube(3.3.8)+conrenunder a stream,uf.nizogen.
3.4.3Fatesificatin
arc.the mrthaaol to cu 0. 5 mlAccurztely add 4 ml pf 0. 1 mol/L disodeum tetrabprate solution , 1 ml of hexane, 25 μL olpyridine and tinglly 5o' propionie abedride iata the above tubes.Seal tightly.Shake the tubesfor I min end etiteifingalina' g ouu x/nir for s min. Trunsfer the hexine layer intt unothur lube withsluppur; afher dehyration by ca o. 5 g 3. 4. 4. Esterification of.the 5tandardAecurately ripat siaindard working golution of guitable eanecrtrarisn to a tube with acrew cap:concentrte tu O. 5 ml, inder a ximim of nitrugem. Thi jirucirntl with mwlerfication a, in 3. 4.3.3. 4. 5Tererminatio
3. 4. 5.1 Gc operating sunditions.B.: (apillanr rolurnr, Re 10 croaslinked phase, 3c ra X 0. 53 mm(id), fuged silica(Shimadzu Co.Jezan or SE'Ca Auntrlis) or eguilent.:h
Golurtn tempcrature: 165't.
Injecticn pon. temgeratuce: 25o'g.Dntectar tempeuwte.255
Cerricr gar una make-in gaa; Nitrugeu, jurityy, eXflow aru.3'tnL/min,flow Iate ulInakeupgBr3smL/min.
Inm:lian model: On-oolumu larm.3.4.5.2 GC determinat:on.
SN/T 0212. 3 93
: Inject accurataly l μl of the eaterified staadard working solution (3.4.4) and sanple golutisn(3, 4. 3) separatcly into gax shvThe opcrution of the llank test is the stnu uy thet dcscribed in the method of determingion. butwith pmiasina pl samplr :recitinn.3.6 Calulation ard expression cf resuleThe caleulstion af tesulr is carry out by GC date processor or according to the fol.wing equatian,x
X-Conteat of clupirinl in tesr saml, ig/kgiA-Peak beigh: nf clopidal propinnate in aamplr alutinn, mrrfi,-- i'eak teigh: of clopidol pzupiorate in standard working eolution, mrn,Concentration of clopidot in standard working solctian μF/aiL,V:Finalvolumn of test solctian,mm—Corresponding imnass of thc samgle in the final tese solution, g..Note; The blaok velue ahould be subtraered frem the zbove reult of caicalarion.4 Lirmit of determinatlon and rceurery4.1Limit of determir.ation
'T'hie limit of determinaton is 0. CC5 mg/kg-4.2 Reeuvery
Acconding tn the experirental di, witen he fersifying ouer!rktinni u 'ujida: in ir: thr zangiof.c050.050 g/kg:thereroveryis%11s%.Additional explanatfong:
This standard was, propoacd by.the Stete Adminintration of Import and Ezport Coinmodi-y In-sgcetinn of thu People's Rrplilir or Chinat.This stanliird wai tlri:fted by the Tianjin Inport and Expart Comuadicy lunuetiwn Buruv of thePeop.e's Repubilie: nE China.I'rincipal drafters; Gao Xiaomin. Xu Hong, Mu Naiciang.Keference
AOAC.Jourunl uf Off'cul Me-hods f Amallysi, Vol. h,2.1984Notr. This Fingligh'weraion, + -nanaleriosi Erom rhr. thinesr, tnxe, jk rrle'y fni gaidsne.
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