【商检行业标准(SN)】 出口禽肉中二氯二甲吡啶酚残留量检验方法液相色谱法

中华人民共和国进出口商品检验行业标准SN/T 0212. 1- 93
出口禽肉中二氯二甲吡啶酚
残留量检验方法
液相色谱法
Method for delernination of clopidolresidues in poutry meat for export-Liquid chromatograpby
1993-06-04发布
中华人民共和国国家进出口商品检验局1993-08-01施
中华人民井和国进出口商品检验行业标准出口离肉中二舞二甲吡
酚残留量检验方法
液相色谱法
Method for determination nf elopidolresidues I ppullrymrat for rxport-Llquid chromatoraphy
主题内容与适用范围
SN/T 0212.1-93
本标准规定了出口离肉中二筑二口咔啶弱规留检验的抽样，制栏知液相曾谱到定力法。本标准适用于出冻妈中_就二H酚戏留量的检验2把样和制祥
2、1检验批
以不超过200件商品为一检验批。同一检验指的商品应具有相间贷行如；包装.标记，产地.裁销和等级等。2.2抽牛数盘
批（件）
101--250
251~-500
5:1-1000
1 001-~2 500
2.3排方法
最低抽样数（件）
按2.2规定的推撑件数，随机扣取，避件开启，每件至少取一转作为原始样品，总量不少2<，敢入消洁容战内，加过后·标明就记，及时送女室。2.4试样别径
从每整原始栏品市欣自部分有代类举样品，格可食整分效入高速渠织据机中换碎均订：充分据用四分法编分出不心于500点，装入清沿的容带内，加封片，标明标记，2.5试格保存
将试择=-18C险陈保存
：正油详及数岸过程中，必或助出择幕割得望成发牛强留物含量的变化，3测定方法
3.1方法提要
中华人民共和国国家进出口商品检验同1993-6-叫批准1993-08.01实施
SN/T Q212.1-.-93
用乙时提取试样中二就二甲吡定断，经减化铝性，阴离子交换柱净化，用带素外检测器的液相也诺这测定二熟二甲吡呢酚残胃量，外标法定垫，3.2试刻和样料
除特别说明外、积有试剂均为分析纯，本达重势摘水3.2.1乙瞻,紫外光谱纯。
甲醇：紫外光港纯。
3.2.3乙酸钠水铬袋：100g/L，
2酸中醇穿液0.25%（V/V）
乙酸带幕溶波：U.（V)。
3.2.6饱和硝配循滤。
无水瓶酸的：650C灼资4h.忙1渐封瓶宁，3.2.73
氧化铅：压析用，中性，70~230日，3.2.33
3.2.9開离子交换树脂：mwex1-X8，1m~2c0日氧离子型，钱雨前接下列片法转换战之酸岁：临1CcRDwex1-X8快脂授入10%乙度钠水做中，不时觉，设施2h后，成人布比满斗，用GtmL10%心钠火游液淋洗至权存根整能高手（用鸡和硝酸银丙酬落液检验，呈微混油）再用水减洗无高于再依次用200m下列溶波淋洗：甲，11.25%乙酸甲萨轮波（3.2.5)日醇，拼后，！试剂，加用酸设备用。
3. 2. 10二表二甲吡啶酚标准密癌3.2.10.1标准贮备减，称取上0.0m一禁二甲北吃（含量.%），甲酵熔期并定舒至1叫1.即为10产g/mI.二效甲吡喷酚际准烂备液。3.2.10.2标常工作溶浓；根据需要出标谨贮备依用甲萨竭级蒂释虎适当淡的标准工作穿，3.3仪器和设务
3.3.1高效液抵色谱仗并配有下列袋置：。紫外检型器
b.色谱数据处现机惑记录仪
3.32组织糖碎机。
3.3.3快递混划器或灯浆机，下载标准就来标准下载网
3.3.4安动能微带化群战处理仪或其他相当的仅器，3.3.5氧化铝房析折柱30cm×1.Bcm(id），下填戒确棉寒，杜内装约三分之一中，绕说加入155可化品：吊心口让第预洗挂字，
3.3.6朗离子树脂交换柱17cm×1cm(id)，下填璃确塞，加人乙酸根型Doex树股浮(3.2.3.使沉降后商约2~-3血，用甲醇洗之使用前.再依次用20mL0.5%7.酸平酵溶波3.2.51.和20 mL 甲养法途
3.3. 7离心机:4 r /min
3.3.微基可谢移满餐：10--2002℃--1000L：3.3.9 离心 mL.
3.3.10微日送样券，20
3. 3. 11 高遵离机,:14 C00 1/mm3. 4谢定步爆
3.4.1提取及化
你取约5带至0.01）试样和5无水酸纳于50mL离心管中.加入25ml.之晴.于买述混器或约浆机上匀案2inin，在离心机上以3000r/min高心2min，将上清液瓶人下接阴离子交换生的其比铝坐中便提取装通过两个净化住净化，再用20m工乙提取满潜一达，离心后同学将士：消液诚入2
SN/T 0212.1-93
氧化铝性杜净化.待提取液全部过柱后，用21m工币萨淋洗辆个柱手，室此，弃去全部淋洗液，取下戴化铅柱.将25ml.离心昏宽下用离了变换性下+用20mL0.5%乙酸甲醇裕控（3.2.5）洗脱二氛二甲呢哦阶，于多功能微鼠化片品必理仅上.60C蔗干，以0.50mL甲醇落辨鸡查。经高理高心(14CC0r/min>3质，供液色诺测定
3. 4.2测是
3.4.2.1刚定色谱条件
：色谱挂：十八烧钟育用定相(O()负谱栏，13rem.25tm.X4.6mcil)
流动排：Z晴-水（20+80），近津为1mL/min：h.
检递被客：240m：
d，色谱片混43c
进样盘120rL，
3. 4. 2. 2危诺测定
根据波中二点二年吡啶的含量情识.选定高指选药标准工作资液标准工作溶液和样滤中二款二甲吡纷响应值出应在仪器检测线性范固内，对标准工作落液和烊液等体积容辅进测定，在上造色活条什下，二氮二月吡赋酸保解时问约为与m，3.4.3、空自试验
除不创试举外，按上到定步骤进行。3.4.4结其的计第和表运
用急潜致据处理扩，或接下式计第二熟二甲吡啶的双留盘：X
中：x
样忌中二载.二中比院醉含量，mg/kg样波中二款二甲限高，m
、——标准工作搭减中二氧二甲吡啶酚高，m一标准工作中二舞二甲批啶感法度，g/m!！——试样
悼液量将积mL
注：计结果和除空兰位，
2方法的测定低限和回收率
2.1副定恢限
.本行法的测定低限为9.01mg/kg：..2回收券
同收案实股数据：氟单唯陡爵浓度在0.010~0.1cGmg/kg范树内回以事为81.1%--,G。
附加说明：
SND212.1—93
本标崔由中华人民共和回国象进出口商品检验局提出。本标雅由中华人民共和国湖南、案皇岛进出口商检骏局负贵起克，本标准主要起草人表智崩，恋厕劳，彭三和、曹意忠、藏华范春林、我洪秀。主要要考文献，
Cerutte A. Mtetliu. Hiruyuki Nukaxawa. and Figu Takabatakr .F. Assut- Off. Arl. Chul. 5:(2),2241584).
Professional Standard of the People's Republic of ChingforImportandExport CommodityInspectioMethodfordetermination of clopidolresidues in paultry meat for export-Liquid chromatography
1Senpe and field of applicationSN/T 0212.1 93
Tlis slanda:d wpecifien the methods Df sapliagi zampje preparation ard cetermirarion by liqud-lirsratagtaphy(LC) of clupidel reriduen in pou.try meat for expart.This ztandard is applscable ro the determiaatiot: uf clupirird rrsirlur in, hrsilars chicken ruzal forexort.
2Sampling and sunplepreparaliom2.1[nspeetion lur
Tii ejuir.tily of an inspection lot shauld nat be more than 2 Soo Eackages.The characteristics oi the cargo w:thir the game ingpces.on lot, auris as parking, tlark, urigin,gradeane speeification,shouldbethe sai.2.2 Quyatity of samnl- ukr
Numher nf packages in each inspeckion lot Minimum number ol packagea to be Laken125
26—100
101—2:50
25！-.500
5ci—10u
2- 3S.irr:pliag procedure
A r.umber of packagea apeeified :n Z.2 are token ut tr.nulwm and ouunel one by onc.Fron caich aoieast One bag saall be taken as w prineuzy Rutreple. The talai weight af ali primaly ampls shuull no?I.ss thila 2 kgs which alill he placed in e clean container. sealed, labeled and sent to iaborarory i.timt-
2.4 Freparatigu ot test sempleParr of represcntetive gampl is laken ram each bag of the primary Eample end the edibie Fartianr.f wti:ci i, homrigenized by grinding in a meal grinder. The hornogenized sample is thoroughly mixedar.d recuced to at lenst soo g by quartering. The trst sample is placed in e clcan containcr erhich igNeuled are Inblec.
2.5Storeg of sarplu
Tihe trsl xaimples ghnuld he stored ar-JR C.Appruved by the State Adainisrratlon otAmportandExpartCumamudityIasprclionofthc Peuple's Republe or Chlva on Jun.4.1993Inplemented fran Auy.1,1993
SN/T 0212.1.-93
Nnte : In the Liurne of 5aripling and sample prepzrationfactury which may cause the change of -exidrecentenr
3 Method of determiuatinn
3.1 Principte
utia:tmuat betekenTtopvoid rnrtarr.ine.tinncr anyThe ckuidul rsudures are exrracted frcm the samgle with acetonirrileand the extract is elcased cpCn Hn ilunsina cnlcran aad sn anion exehatige coluran. Clopidal g determined by liyuitl -htainiutngray:with Uv detecior, and quartified by externa staunrd ueibil.3. 2Keagents and maturals
Ualess uthrrwise specified all thc reagenis should be of an:lyticsl grade, \warer' ghal. be twic :distillerl.
3.2.1 Acetonitrile,UV apectra pure.3.2.2Methanot,'V apeatra purr3.2.3Sodium aretnte nrlisnlo>g/L.3.2,4Atic acid-nethar.ol slutioa:o,25%i(1/V)3.2.5Aeticacid-methanolsoluriaa:o.toicV/1)3.2,6Silve:aicraresEturaredsulurnn inncelimn3.2.7Anhydruun lintt n.lfate,Ignite ar trio C Ear 4 hrand xeep in a tighuly clased container afreolirg.
3.2.8Alumina;For ctromalography, nsutral, 70—230 mesh.3.2. 9 Anicn excharge resin,Egwex 1 X8,loum200 mesl, rhlnride form, Caaer: anicn exchirktrto acetare form by the folluwik prnrdure:Snas loo g Towex 1-Xa in sodium acetate uiu'o.(3.2.2) for 2 s wil 3.2.10 clopidol standurd solerion3. 2. 10. 1 Standard acock yoletian,Veigh 10, 1) ug uf rlupilol xlandard(purity99, ow), diskole innethano. ar.e preparc selutiet ul li jμg/ml. i lhe siandard stock solution.3. 2. 10. 2 Standurl wirkiug raiti:ion: Aceording to the reyuirement, prepare a scandard working a?lliun af apprapriate concer.trz.tivtiwith standard stock solutiun3.3Apparaas ar.c egaiprment
3. 3. 1 Liguid chromategtaph cquirprit wi-h :a.Lydtcetur;
b.Rerder ar -hrnmatgraphie data processor.3.3.2 Tissue rinder.
3.3. 3Vortex mxer or blencer.3. 3.4Multifuaction semple treimpat uni: for microclemical.method,ar equivalent,3.3.5Alunine culumn;Place Rnail cotcon piug at thebottom of 300 mmX15mm(id)colunua indfill buut I/3 full with methanol, lowly pour in 15 g of alumina nnd riase the colaun with 2:n ril. ofmzhanol.
SNT 0212,1—93
3.3.6Aaian exhangeculumn,Placesmallcurlon pinkattl-hettnmof17cmmX1cmm(id)olumnznd fail abaur 1/3 full witk rvethenul. Pour &ullinjen: Dowex resin suspersion(3, 2. 9) into the colunn1a give bed height of abul 2 3 cut ufinr retinig - Rinsc the column with 20 mL af o. e aceric acid-mkthanclls. 2. 5) end 21) nil, ef muthenol hefare ast.3. 3.7Cenrifuge: 4 oc r/mn.
3.3.8Mierv adjusiable nlume pipeztes;tc—200 μL.2001050 pL.3.3. 9 Centrifuge rale: jo ul..3.3. 10 Mict xyringt: 2C nl..S.3. 71H.gh spil tent:ituge:14 ccu r/min.3.4Prlure
3. 4.1 Fxiraciian and clean ugWeigh ca g(arcurate to , ot g) of theiest samgle and s R of anhyriruus soelum sulfate into acrntriluge rube, add 2s mL cl acetonitrile aad hlend with blerder fnr 2 rmit, rntrifuge at 00) 1/uin, Place the anion exchange column under alumine cotu'ng, Pour rhe surerna.anc exiracts into thealunisa co'umr. and let pass through cnc ulumina colemn and the anion exchangecolumn.Once againexlract the residues wth 20 ml. of acitanitrile+ euntrifugr anrl pass the supernatant 1htough taioroluzaas. Wash bo:h eclumas with 23 rT, al ieeilanol after ail extracts have passed tat culun1os.Jiscard al. the washaing salytiun. Remove aluminn colunn, place 50 mL centr.fuge tube utider suiwn txcaange column: nad alute tlopidol wi:h 2c inl. nf o. 5X zcetin acid-methaoll3. 2. 5). Evapornte theeluale lo dryness or. muiriluctign sainple treatnent unit for microrheraical method nt BoC. Digsulvethe residus in 0. 55 mL af meth:inol., The snl:stinn ia centritugalisrd lo: 3 mia ar 14 Owo r/min artl thex.aperhsrart in uged fnr I.C rlrterminatint.3.4.2Denrmnal
3. 2. 2. 1. I.C ojieratis:g condnionu.toluunanscolunn10μm25emx4.6mm(id)The rubie phase: acetanitrile-water(20 +8o+flow rate: 1 rnl.fniub,
Detautiou weveleagth:27c nml:e.
dColunr temper21uz2;40C:
.The volume od sample injected20 μl3. 4. 2.21.C ieterminalion
nrrationofelopicol inthesarplesilatinn,selecttheztandardau:ording iriihe apuroximate concenwirkin solutinn oritl: sirmilar pcak heighr ro that pf sarspl, sulotiun. The jesponses of clopidol in thesiar.dard so.ucior and gample suluticn ahuu'd be n th lineir Tung of the instrtroental deteetioa. Fhstardarc workiag koluticn shoald b= :ngeted is betwea utininurally with the semple sotuttaun of r-qu.l volumc. Lader the ahova chronargraplir 4tttition,the retention time oi clopidol is ze 5 mt3.4.3Blr.nk rest
The u[pcretisn af tlhe blsnk rest is :he sur ht that described in the merhod of derernination, lmwrt:om:ssion otsampln additipn.3.4.4 Caleulatiun aunt: erpressiun uf regultrhe cale-latiun uf renult is carriet nus hy'chminarographic data proeesaor or securding tu the Falwig lornale:
SN/T 0212. 1—93
Clapidol conteat af aample,mg/kg+ Prak height af clopilet iut the Kamiple Nalutioll, rm;Peak height of clopidol in the standard working solution, mm:Concentration of clopidol in the standard workink solutian- μg/ml.:m-Mans of test sample,gt
V - Final vulurne uf test solutwn, mL.Note, The bank value sho-ald be wubtraeted froru the above rexult n calculaticrt.4Limit or determiautinn und rccavery4.1 Lin.it of determinztien
The Jimit of determaination is o.ol mg/kg4.2Reruvrry
Accordiag io the experineatal data, whe: the conrearalinn f rlupih! is, in ihe rang f . jio.230mg/kg.thetueoveryis64.1/--106.%.Aditional cxpluations
Tiin sti rulurrd was prupused by the Stute Administration of Impor: and Expore Comraadity In-spec:ion cf the People's Republic nf China.This atancard was drafred by the Hunan, Qinhuangdao Lmpart aad Export Commodity luspeci..r.Bureau uf the Pcuple'g Republir of Chira.This shamiaril was rtwinly dzaliwl by Yuun Zhineng+Pang Guofung+ Peng Sanhe,Ca YenzhongDai Hua, Fan Chualin. Ne llongyong.Keference.
Carullu A. M-cms. Hiroyuki Nekazawa, end Eigo Takabetake,.. Assoc. Off. Anal. Chen. .s?(2).224(1584)
Me:Le: This Frglish vers'nn, n trnnsl:rinn frnm the C.hir.eas text, is aolcly fo g widenceB
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