【商检行业标准(SN)】 出口肉中甲砜霉素残留量检验方法

中华人民共和国进出口商品检验行业标准SN 0199—93
出口肉中甲砜霉素残留量检验方法Method for determination of thiamphenicolresiducs in mcat for export
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实施
中华人民共和国进出口商品检验行业标准出口肉中甲矾需素残留量检验方法Methed tor delernination of Iblamphezlenlresidues In meat or export
1主超内客与适用范雨
SN0159
本标难规定了出[内中甲鼠每素残留量检整的抽样、制科和气相色谱澳定方法，本标准适用于品口鸡窝中单风等承残留版检验2抽样和制样
2.1检验批
以不超过25商品为检验批
一性胆批内商激应民有同一特征，如包表.标记，产选、规路，等级等、2.2抛样拉量
检验批中的件致
26-100
101~253
21-~500
501~-1 090
1 l~2500
2.3抽样方法
单低编样件数
度2、？规定的拍样件数酬机抽取减件升片。再作至少取一包，去挡科薄膜，以每包抽感肉举不少平50·总述不少下2·敏入清洁客器内·如封后标明标记，及时送空实整卒。2.4样显的划条
将所取原始样品错分出】kg，最可食部乎，象组划书降折势率，均分成份，装人治净容器以，密时,作均试，并标明标记、
2.5试单本
将试准F一13以下降陈保存。
注，在当兰和间样函势指过程中必统防止禁员量别得染或发生我所物盘的变化。3测定方法
3. 7 方法提要
将鸡肉伴用丙源提取，加入無化钠溶液，用乙酸乙增缇取，蒸除乙酸乙霜片，加入乙等及已烧，板中华人民共和国国家进出口商品检检居7993·06-04批准1993-08-01实施
SV0199-93
御鸟与，分敢乙牌层，真空除去乙髓后，用乙酸乙酯、乙酸醉、吡进行乙酰化，用战腔柱净化后用配有火陷光度检测端的气柑色谱收测定，外标法定量，3.2试剂和料
3.2.！两存折笑，单热恼。
3.22正二烷：分折地，重蒸瘤
3.2-3乙酸乙酯：分析纯，或满
3.2.4乙崩：分折纯，重蕊瘤。
3-2.5甲酵：版光谱纯，
3.2.6三第甲境：分新纯，重蒸衡，3.2.7乙酸酐：忧绒纯。
3.2.3吡啶，很毁纯，
3.2.3化销优级纯。
3.2.13无水统酸钩分析纯.于65℃灼烧4为.冷后忙于带闭睿器中，32.11求群素标催站，纯度学落。3.2.2甲两再求标准格满，精确称取中码等素标难品10.0mg于内制，定容至50mL.取此减5m1内离插稀至50L，为标准工作裕减。此液1mL含甲码来20叫3.3设器和设备
33：离心:53L
3.3.2高速均质器，
3.3.3旋传燕发器
3.3.4离含机，下载标准就来标准下载网
3.3.5烂您柱，将片色诺用硅腔（100--200月）36用三氧单惊装入10mm×3cDmm载离语析中，上面落人无水硫酸钠1多一
3.3.5气村色整仪：配FPD检测器5型滤光片(329而）34别定长票
3-4.1提取
微改试样20g（精确到0.2@）50ml.商心答户，加入30mL内调，均资1min后，以3000~35C0：/min离心三mir，将上得滤倒入另一个50mL高心曾中，残留物中加入20mL内配，同样均质离心片令片上范凌，留物中可如人10m丙酮，同样沟离心后，合并上清液，3.4.2净快
将密心誉内的两提致微理离心5min.将上清变移人分疫通斗加入3%化钠1，混每，再人50m.乙酸乙酯派播混，萨笠分层后将Z酸之酷层转称到50%0mz烧瓶中，水晨资液再用10m，0！乙酸乙酯搭上逆步骤率取两次，命井乙酸乙脂荤取减，用能转蒸发器蒸除其中的咨剂砭留均用5mL.3L及2mL乙肺分次洗入分液满牛.加入正已烷3CmL，报摇，静宜，办层层去正已烧·用施转热发器换干/断层
在留物出致乙能0.5m2.乙酸0.6ml及2滴，满勺后置30ml，在反度波中加人水5m-，滤勺，月：二条甲境提取3次，每次地5mL，收三领甲烷提承液，用水统录兰次，每次用5:L水·弃去水熙与，在三氮中烷中加入无水硫酸钠5g癌句，静留后将溶波注入建胶柱。用三率甲境33al.洗到下的配酸钠，将院液比入硅腔性，弃去琳洗减。用单蕾-三款甲烷2十3>30mL洗脱，收集资脱准，用能转发究蒸发至T.以两朗0.5mL溶解残留物.快气相色谐到定。3.4.4测定
3.4.4.1色清杀件
SN0199—93
色游:玻性+1m×3mm（内径）填充物为2%(m/m)0V-17除于Chrom090rbWHP3C~>
色谱性温度，280℃，
进样甘温度：300℃;
整测器温度，300T：
氧气：纯3.99%.60mT.imin
氢气：75mL/m
空气，100ml/mim
3.4.4.2色递制烂
根据样液中甲限荐来含量惯况，选定畅高祖近的标工作溶液，标避工作溶斌和排滤出甲取荐率响应值均应在仪器检烫线性范用内。标准工作溶商和样液等体部多摘进样两定，在述色诸策行下甲基事保留时间约为 4.5 mim
3.4.5空白试验
除不加试详外，按上述测突步聚进行。3.4.6结果计算和表述
用色谱数据处理机或按下列公式计算，X
式中，X—试栏中中取群素留，mg/kg！样波中兽药的样商，m
,——标准工作掩狱中善药的峰商，mnh-c-
准工作落较中兽药的港度，u/ml.称取药试样量，；
地液最终奔体积，ml..
出：计再结果需李白位
4方法的测定低观、回收率
4.1到定低限，0.5mg/kg，
4.2国收率
同女率的实验效据：甲限察素依成在.1~1.0/kg范围，回收率为80%~99光。附加说明：
本标推山中张人民共和国国家进品商品签验月提白标准由中华人民共和国河北、河卤、化京进出口商品按验高负贵起卓。态标准主要起草人王风池、段文中、括雾州，胡文炬。主要参专文献：
原生省坐者下生高别内卫牛调编架，商水产食品中の离谢物质检查法25.学下下二一几p202--2u6。
Professional Standard of thePeople's Republic of Chinafar lmport and Export Commodity InspectianSN 0199-53
Method for dettrminalion of thianphenicolresidues in meat for expart
1Scopeand Fieid of applicationThis brandard specifien the rnethods of samping.eample preparation arr deterrminaticn hy gaschromstegraphy2Sampliag and snplr prepasation2. 1Imse-in b:
The juantiry af an inspectiou lot shosld uot ba more taan 1 50ui packtges.'Fhe characteristice ul the nrgo within an nspecio lar,guch as packirgrmers,origir.,krede andsgeeficatinnshorld br the samc.2.2Quanily uf xgaple
Number of packagcs ir.
l, ingpHidins kil
24—100
101-250
251—500
501-1000
- 01 —2 500
2.3Samling Frocedure
M:nimun nurr.ber of
arkayes to le raken
Tin muiker uf ln:hagun wugifil in 2.2nrr tnk+n al riandre and unpacked one by oac.At leas:ana ba shoyld be taken froro caxin Fackare and no: .css than o g sheufd be :aken froar. each bas asthe 2riz.ary ganple. Ihe tolal weighe cf a.l primrry namples shoull nu; h. lesa ilisn 3 kg.which ghellEe piaced in elea curtuiners ,sealer.,iarlet rel xent tu labraratery in time.2. 4 Frj.irliun f (est N:npleTiae cambined primary sample is redurerl to I kg,:he edible yortion is blerced.and then divseedinto Lwo equal portiona, Each porcion is placed ir a clcur. cousininey as teet fatiple,wnicb in xealed undlsbeled.
Appruved by the Stale Adminlstrallon nt[mport aud Export Camnmodity Iuspeetion nfTht People'a Repuhlic nf China on Jun, 4.1993[niplemtnted From Aug- 1.19932. 5 Slkrigs uf xumple
SN0199-93
The test samples should be stored undet.-18 ..Nute; Tn ihe cacrse of se:upliog uud amle prepearation prceautiou muet be rakell to avoid ro7tetnination oT r.yJe!urs weicl: ruay cal
3 Method of dezerminallan
3.1 Panciple
he sbauut of Esidue sop'ep.
The samale g extracted with ecctone ther add sudium chlotid: sel.:ion.the saiu:inn is artirior:rilwit: th.yl aketiele, Fvaporlr. 1he ethyl a.etate lo dryness, add scerotitrie and n-hexaie to thcrexiduee. Sh:ke,let the layers beperate,evaFarate the abetonitrile layer to dryuees and acetylated withethyl acearc,acetie RahydHed aad pyridine.'T hen purify with gilice gel column and μnalyzed by Gwith lamc phctomctric detertor.using exteraal stundu-d methuel.3. 2 Rengents i? maieriel.
3.2.1 Acetore:A. R. rediztilled.3.2-2 -Hexane:A.R.-red:stilled.3.2-3Eayl aectate.A.R.rrediati.led3. 2.4Arrlunitrilr:A. R. trelistiller.3.2-5 Methaaoi.UV grade.
3.2.6Chiorosorm.A.R..zedisled.3- 2-7 Areti yrhytlr:te G.R..3. 2, 8Pyricline,G. R..
3. 2, 9 Sadium ealoride G. R.3. 2. 10 Sodium salfetc (anhydroua),A. R. ,ignite at 50 Y fot 4 h. aud sccp ir. a tightly closed cun-reinar afirr couing.
3.2.11Srandad ttiampheniol,Purity:9963. 2. 12 Tliamplenicol sranderd soluon: Accurarely weigh 10. 0 of standsrd thiomphenico_ inrc EElaak. Drssulve in Eceturr. Quanritalively transfrr the xlautuon To So ml. volunel:ic Elask anl make uptu rmgrk with aeenre.
Transla: 5 L c the above sol:tion into 5o ml.voumetric flaak ane make p to snark with acetone as the srandard working solutiu.The concentralion us whinh is o μg/eL.3. 3/Appzratuy ad wuipraen
3 3-1 Crrtrifugal tuhe.53 ml..3. 3.213omagnizor.
3.3.3Rolary evzporhtot.
3. 3.4 Cenr-ifuger.
3. 3. 5 Silitu gel tis.uz.n:A suspersion ul 3 g of silica gel (for chromatography use 100 -2cc ruesh) inCT[Cl. is pou: inzo a clhrotnatograpkic calumn Csoo mm X1c m. (id>),cn the top of the silica Rel ispisrknd wi-h a of enhydruus sodium gulfate.3.3.fChromatagragh,Equppedwith flamephotomctrie detertor und sulfer filter(3z9 na.).3. Pracederc
3.4.1ExrEctiun
Weigh ca zo g of the test sample (accurate to , l g>into a centriuga. rpbe,homogenize for l minwith 3 ml of acetone.Cenrrifuge for 5 min at 3 0003 500 r/min.Trunsfer the supermaant intu an-5
SN199-93
other cenirilug-l luba. Horngenize aad entrifuge the reyidues for 2 tipea more zith 20 ml anc 1o m.uf scetoa.t fs abre.Combine the superrtilaris.3.4.2Clea up
Cenririfuze agai lhe scetoile exiractinn for 5 min. Lecunt the gupernatancs iata scperacing funnel,add 150 .L of 5/ sodium chlnride galutina,hixtl thcronghly. Ald 5u mL ethyl acetate,ahakevigarousely and let layers seperate,traneler the ethyl acetate layer imtt a Snn riL Elar-k. Reptat twicethe albove-mentiohed operatian with 1oc mL and fo mI. of ethyl aceliale and ciormlie ihr rlhyl uuctatein the flask. E'aporare the galution to dryness in a rotary evaperator, Transfer the renidue inin a seperatary funncl with quccegajve 5 ml,.3 ml and 2 mL of acetonitrile. Add 30 mL of n-hexane. Shak: immllet layers sepcrete ,diszard cha hexane layer, Evaporate to expel acetonitril.3.4.3Acry.ation
Add C. 5 mL of ethyl acetate.0. & mL pf acetic enhydride and 2 drogs of yridine ro the regidues.Mixed tharoagbly une s:andy for sc min. Add in 5 ml af water to the reaction.mixed thoroughly.Extract th: sulutiuz with three 5 mL porcions af chlozotorm. Collect the chloroforn extract and waskwitl llrer 5 mt. pi:tiorw cl wa:tr. Dissard the aqucous leycr ,add 5 g sogium suliateshake vigprousely. Traresfer the mltion ig the siliee gel column. Wass the remained gadiur saliate uzith 30 mL ofchlcroforu. Transfer thr weshsing is thr ailici gu:l sulunnn, Diseerd the weshirg. Elurc with EC ml ofmethanol-chloroform(2+R).Collect the eluaces,evapkirata lia tlryns in a rotary cvapuratur.Dhssoivccae Iesidut with , 5 ml, of zcetane. The solurinn i% uxwd fnr rbruratograjbie descirinaripr.3.4.4Detetmination
3. 4. 4. 1 GC operatir. conditianCalumn :Giass, 1 m×3 mr(ed),packed witE: 2%(n/m>Oy-11 >r: Chrumesurl W HP(83-100拍eh）.
Calumn erm7eralur+1280 C.
lajcaripn porttemperature:3o0.Dctcctarremperaturc.sooC
.Nitragun.Puricy.!.6omL/min.f.Hytrugua:7s ml/mir..
g.Air.cnnL/nn.
3.4, 4.2GC deternirt:tior
Acneding tn thur: approxiaute coacrutrition of thiamphea:coi in the sample soletian,select theSLeadard working arluti wirh, vimiiar [unk height to that oi samp'e solurior. The rcsponacs of thiamphenico in the atandiurd olutitu arul atuple,sulution zhould be in the incar renkc ol lw inatrurnen.tal decection, The stand:ud wrrking suiulisr: shuuld be i-sieucud in-betwrutt prensiona.ly with the aample solutions ot egual volume. Under the above chrunutgriphi, cuudilinn,ile rn.eition liuc of thtamhphenicol is about -, 5 min.3.4.5Blank test
The operition af the blank teet is the same as Lhil deacrikal ir: ihe netlnd cd idterminintiun,butwith omission of sarnpleaddition.3.4.6Calcuiation and expressian af testleThe caltulation af rest:lt is carried out by GC data p:acessar or axcording to the following [arinula
SN E199-93
X-Reside canteat of thiaraphenical+mg/kgf—Peak heightoi thiamphenicot in the sample Bolution+mmh.-Peah height af thiamphenirul in the standard working solution,mmi-Concentrarion nf thiamphenicol in the gtandard workiag solutioa-Fg/mLmMasty af Lant sansple g
V.--Final volume of test zample solution,mL.Nate.: The hlank va'ue shatl be subtreelec irim Line abive Tesu't.4Limit of determlnation and recarery4.1Tlin imit of derejminacion is G.5mg/kg.4.2Recovery
According to thc cxpcrimcntal caea+when the coacentratian of thiamphanico! s in the ange of0. 11.0 mg/kg itf.n rreuvery is 80%—99%.Aalditinnjlexptanatfons
This standard was proposed by the Srate Administratiau of lmpoct and Export Crmmodity Ir.apectiot nf the People'g Republic of China,This stendard wes refted by the Febei,Henan and Beijing fmport and Export Commedily lnapecTion Bureau Reference:
厚生省生活卫生品乳肉卫生保继巢，畜水产食品中の残留物质查法3.25，子了二二一P202—206
Motu: Tlia E:glish vereion a ira:wlaticn frunt tie Ctunese te. lis aolely ur uidaue.
小提示：此标准内容仅展示完整标准里的部分截取内容，若需要完整标准请到上方自行免费下载完整标准文档。