【商检行业标准(SN)】 出口肉及肉制品中滴残留量检验方法

中华人民共和国进出口商品检验行业标准SN 0195-93
出口肉及肉制品中2.4-滴
残留量检验方法
Method for deternnination of 2,4-D residuesin mcat and meat products for export1993-06-04发布
1993-08-01实施
中华人民共和国国家进出口商品检验局发布中华人民共和国进出口商品验行业标准出口肉及肉制品中24-滴残留检验方法Method frr delermiaiton cdf 2.4-n regidpesla meut and taeat praducig for expnrt1主题内容与适用范围
SN 0195-93
本标难规定了出口肉及肉制品中2.4-滴留量检验的挞样制样和气相色潜测定方法，本标准适用于白口冻分削内、清燕猪肉睡头和感牛肉中2.4-滴残曲逊药检验，2抽样和制样
2.1检恰批
以不趋过2件为--验批。
司~-检验批的商品起县有相同的特征，如包装，标买、产地、规格和级等，2.2抽样数基
批量(件)
26+-100
101-25
531--1 000
1001~2 500
2.3排排方运
最少油样数（件）
按2.2规定的拍样件数随机拍疫，逐件升房。内及内制品（递义除外）从每件中敢一装作为原始样品，其总量不少于2kg放人清洁溶器内，加势后，标明标记，及对送交实验室。刻每件出无小包装惑有小包装但每重好超过2者，别可用降利刀（用特灭菌过）在抽出的包件中，每件制收不少十1006，提合后些于诺洁容器内，作为混原始样，混合原始样的单服不少一2kg，划封后，标明标记，及时送实务究.罐头：每件随机取一。
所推取的举品应标明标记及时送交实验室，2.4或样甸各
肉肉制品（端头险外从所收全部详品中段出有代性举品的1000充分搅碎，涯勾，均分感两份，分装入洁净容器内，密封：作为试样，标明标记。睡头：将所取全部祥品开播后，充分搅席，混匀，取出约1000，装入洁净容器内，密对，作为试推，标明标记。
2.5试祥保存
中华人民共和国国家进出口商品检验高1993-06-04批准1993-08.01实
将试样于一1$心冷冻保存。
SN 0195-93
转：在抽样制样的操作正轻中，必或防止样品学到污象或发生残留物含量内变化，3测定方法
3.1方共提要
醛唑案性下，以三熟中姚要取组织中残留的2.4·滴及其钠益，并转移室减液中，用有机溶剂洗瓷后再将其酸化：2，1滴再三氧甲烷旋取。蒸除溶剂将其甲酯化.用气相色谱仪电子径求检测器检测，列标洁定择，
3. 2试齐和均料
3.2.1三熟中烷：分析统.单举增，3.2.2乙醇，分纯，更蒸馅
3.2.3F.己碗分折纯.虱蒸馈，
3.2.4元求硅分护纯·重蒸饱，
3.2.5硫醒-水(119):以就级纯张统酸配制，每500ml.荷牌-水(1-19)用50ml.二氧平烷拍摄两次后.
3.2.E氢化销落液（T.）优级纯氢率化钠配制，年59）ml.氢氧化钟溶液（30多/.)用25mL三采中统扯提病改后各用。
3.2.7点化纳：优级违.每250效化钠日100mL止己烷超声退拍据再次，拆干，650T灼烧4h，汇于其室杭中。
3.2.8地合就化钠溶微：激优级减额化钠配制。每2%0ml1.他合款化纳溶液用251nT.三氯甲烷抽提两饮后果。
3.2.9元水宽弟：分研统，每1C0%无水纳用20m1.T二流声波抽提两次后，担干，一630么约络于车器压
3-2.1G晚崴范溶液40 g/L:移取水硫龄13. 2,914g溶于1CL:L蒸储水中，每10 raL.溶液用aml正己烧抽是两次后备用.
3-2.17一化期-乙避试券[470品/L：分纯、北京化丁，3.2.12甲资化游液，将三冠化册-乙酰试剂和甲降于一15℃下预冷，将50m冷三然化研-乙醛试剂和12)r冷币群泄和，案0~.4心下缺存备电。3.2.132.4-满称准品纯质5%。
3.2.142.1-滴标准溶液：准确球取2.1-循标准距以无水乙醛(3.2.4)配制或液度为0.1Ⅱg/mL示净贮务溶液。再九术乙健稀择成造用装度的标准工作溶液，3.3位器礼总备
汽相色详收配寄电平准按按通器33.2组识将呼挑、
3. 3-3束氏振病%。
3.3.4机;250 mL
3-3-5封试15ml，离旋孟（附西乙烯内村密对坚）。3.36祖益水溶箱。
，全效期势以经声被洗，用脏以少正烷林洗，3.4定
3.4.1提收及净化
你战穿滤对的试样药29树确到0.1g于500mL具室锥形做，15l.2版，5L硫限不二+9）！多氧化钠和100L三氮境。加需，握落提取30min。道过快速继纸让涉，滤液收您于0
SN 019593
25)m1.分液满斗中，用约$0ml.三策甲烯分三火洗嵌证形瓶及缺满.合并洗浓于分液滑斗中.于上逆分减满中2mL氢氧化钩（30g/）和50mL蒸确水再加人10L饱利氧北钠游做比时水相II应>12，列补加适域氧氧化钢溶波（3-6）。对于极易乳化的拌品可再补划约3款化的1.报梯据取±min。静罕分层，奔去三氧甲烷层。以25nL三氯甲烷洗涤水层二改产去三氯半统层。再以2mL乙髓洗漆永层，峰臣分层·将下层水柜轻移至丹一250m.分液需斗中，旁去乙醛层，于上述水祖中，人25ml疏膜-水(1+9)逆行酸化+捞勾水相pIE应2.否则应适匠补加死酸-(1+)).整后分别用50mL25mlL.2号mL二氧中烷据取水柜，将三氯中烷探取液收兼-\25℃ml，心形中.16cC水浴中通以需气施格三靠甲烷挥至约3~-5m，以数案升三氣甲境将其定量转移至密封试使（3.3.5>再以氢气统将三氯甲院完全挥院，
3.42牛醋
于上适册纤试管中，加1aL中断化液（3.2.12)将螺旋益带划，充外报动混与，十70C水游非化1 h,放冷至促,以约 10 mL 统酸钠溶波(3. 2. 10)将甲酯症转格至 25 mL具密试管中,分别以 4 rL 正已烷提取两改，用滴管将正己层转移至另一25ml.具墨试管中.以2m1.硫载的链液能绿正已境尽二改用滴管吸除水层，以容母频定容至1CmL，吸取上让正统落滤3--5mL.下:其寒试你，那药1R无水疏酸缺、报搭悦水，其气相危诺分护。3.4.32.4-滴酯标准上作穿液的制务准确吸收适用该废的2,1满标准溶液1mL于片想疏相盗的试普(3.3.5)向。以忽气流将路齐挥除，按34.2操作进行甲罪比后供气相色诺办析。3.4-4测定
3.4.4.1色谱条件
包谱柱：皱璃去，2m×2m(il）.筑元物为2.5%(m/m)0V-17-3.3%（m/m>QF1涂于C:P(8~190R
色诺住道意：220℃：
满撑口温座，280心
器度：280！
e.我气：宽气.质>9.99%，ml./min3.2,4.2色潜避定：分别准确些联上述液(3.4.2)或标旁L作溶液(3.4.3)1 -~2μL(等收连)注入一色书交，实际更洲的标准上作流液及待测样波中，，4-滴甲造的向应尚产担手均序卡检测器的线为。
企.上述签件下2.4-清甲醋保需时间约为2mim.3.4.5空户试验
除不加祥品外，按上述作同录件和步照逆行。3.5结果计算和衰述
同产溃据理扩或搭一烈公式章：h-s.v
式：x—试样中2.4.编含量，mg/kgl——样被下 2,4 滴甲酯的率高,mm;h，样让溶较中r2-满甲的择尚，rt.;一起料工件流液户9.滴派度145mE：V—样定容区识，inl.
精命重。
生，计算约更商扣除空白值，
4方法的测定低限、回收率
4.1德定频限
本方法测定低限为0.2mg/kg。
4.2巨收率
SN0195-93
回收率的实验数据;2,4-滤依度在1.02~-h.20m1g/kg范固.回收率为个0兴~97%。附加说明：
本标推自卡华人民共和国国家过出口商品检验同理出。本标准由中华人民共和国天冲选出口商品检验局负贵起点，本标准土要起草人稳乃强，林安循,王虹，主要考文献：
FDA-Pertieide Ana'ylizal Manual, Vol. [.201-11-15,198s.Prufesslonal Standard of thc Fcople's Republic of Chinafor Import and Export Commodlty InspectionSN 0195-93
Meihod for determination of 2,4-D residuesin meat and meat products for expori1Scppeandfleldofappilcatlon
This standrd specities the method ol sampiing,sample areparaticn and determinarion by gaschrcm2.tography of 2.4-1) residues in meat snd mcat produetg for cxporr.This srandard is appliuable: tu thr del rrniuticn nf 2,e-T residus :n iraaen cs:ls of neal,cannedsteemerl purk al ror:led tef inr export.2Suiapling anal sainple preparation2.1Inspection lor
Thr rjunntily al an iaspectinn lot shauld not be more than 2 5oo yackages.The characteristics uf the zargo wihin the ama inapeetian lot, gueh es packing mark arig-n,apecificaron and grade,should be the seme.Quantity uf sanple ti ker
Numher af packages :n
each iaspecticn lot
26—1
n1—25m
255—500
501-1035
1 cul—2 5un
2-3Sampling procedure
Minimum nur.ber of packages
to be taken
A rembe: af packageg speedied in 2. 2 are taken at taudon ard opencd cre by uuu.Meet und meut μrocucts (exeegt zanted fouug),Frur ruel..a lunt uru. leg alall le ,kra a i. priniary Niurmple. Tine ioial wright of al he priua:y hacuples el.culd nal bhe leae thar. ? kg.which shall beplaced in B clean container.sealed,labeled and scnt to the laboratory ir. time.la care the frozer meat-pieces are nat canrzined in mall bags ngide eacs pacaagcer if thes aregraeil begs insitr. th pickig. bu: the euueint ul :he luig rkepwln g kg-tal iue gpriri frsin ite a.eai inar:' prkage n: nn: less thas 100 with a starp knife (disir.fected with alenhal s, Mix -be parts of themeat as the rixed prinary sample.which shall not be luss tha 2 kg. Sealed.lzbeled and zent te iheIiboretory in tirie.
hppravet by the State Administration afImportand Export Comtkdity Inspuctina ofTheFeopie's Republic or China on Jun.4.1993Implemented from Aug.1.1993
SN0195-93
Canurd fuels;Cne ean shall be tuken t Iandon frurr ceeh gackag.Sumples taken &hauld be Jabeled and sent to Laboratory in tinre.2.4 Fregaration c tesl sampleMear and meat products (cxept anned foods),The ccmbined primery sample is reduset ta I oocg which is bleuded μmixed und! eivitird insu twu equrl [urtiuns rcach portion :9 plared in elerr veaselag m test Ngurnp'e, whiel, i, thru nealeel nnl lahnpleil.Carned fcods:Open all the cans sample,blend,mix and reduce ta 1 ca g,whic:s is tliviale:l inl:!two egual pcrrian3,each 2ortion is pleced ia a clean veasel as a test *ample.which is then scaled aad la-belec.
2.5 Storage nf sarople
The test samp.e should be tered it .-1a'c.Nnvei Is thr rciren nf snmphng nad snrmple prepetmrenn,jrcaitica muist be tnkrn to aued contoination or enyEnetnrs wherh m.ay enisr ti. chnr.g. of re.si:lisr anntant.3Methnd af determiaatinn
3.1Prinriple
The chlarophelnexy acid (2, 1-Dh residues and it: Na a.ce ere xtrazled frrt.t ili lissut wih rhli-rofortt unde: atscified cordito,tliea transferted ir.to a.kaline solution. The zlkalirc salution is washedlw:th orgeniz solverta aad acidifice,2.t D are thacn recxtrsetrd with calosaform and neth.ylarec alte-Ihr :-llooinra. has aeen avaposaled. Naieireinricr. in malr lry (c wi i r:rs-lran uajitt.tt detcter rudquantified by Jsing the external stancard.3.2Reageat3 and mareria.s
3. 2-1 Chloroform rAnelyicel g:ade redisrilled3. 2-2Ethewl :Aalyticel grale ,rrdistilleu.3. 2. 3n-Hexanx:Ant.ytisal grada,redistilled.3.2.4 Echy. ether-aahydrous.Aralyzieal grade.redistilled.3- 2. 5 Sullurc acid-water (1-t 3),Preare the so.uor. with GR grade sulft:ri: acid, Each 500 l, ofsulfuriu acii water (+s is extraesec. with 5u nL uf ehluruforn iyrice.3, 2. 6 Sadimt t.ylinxiln rlalinn (3o n/l.), PreFare the anlutic: with GR gaaln af suriurt hydrcx-ide.Each fo0 ml, of sodium hydroxide salution is extraccd with 25 mL of chlsrefarm twicr.3- 2.7 Sodium :h:oride:Gk grale,wask 260 g af socium rklaride w:th 150 ml, of a-hexane twice byulir, susie lurcr. Evawrur tu exal thec solert aad igrite at 5i C: Eur 4 tstore ir a sto2pered glassjar.
3- 2.8 Saturated sorcium ehlrrile solutin:s:Prepar+ with GR grade sndicm chalniln. E: rh 25r' L uEsaturated sodiurn :h.oride solution is extracted with 25 ml ot cllcroforz. twicc.3. 2. g Anhydrous sodit:m sullare,Araly-.cal grace,waah lo0 6 of anhydro.is sodiuun sulfate wicl 20nL :f n Jkxan: =wice by ultresonis eleurer, Evusorut: iu xp,l th suivrne,igaite at 6oc C for - h,and s.orz ir ar-tipl riaiaer.3. 2. CSudiut. suliate sslation <.10 g/L>, Weigt: 4 g of ushydrous odiam ssliste an. ilisanli in _:n)ml. waler. Euc: so ml of this solulio: is exirucred with 1c mi.cl n-hexat.e twicc.3.2.11Borun rriflzoride-ccher zeagenr (17ug/L):Aaalytical grsde.3.2. 12Mthy.alia suluticr.; Prs twul l:jrir :ri'ucrir:r-r:lr Tuageat and mzchanol st15 tadd at ml. of cole hornn nir.uar.ce-e:har reayet't intn 123 mt. cf enli nma:na\us url mix thusaghly.stopper.s1ore st 04'C..
3.2.132.4-D standard,Purity985.SN0195-93
3.2.142,-D standard soluon,Prepare 0.1 mg/ml, standard atock go.ution winh erbyl μther,lhedilute to suitallr tuauertraian with eihyl elir at staad.rd workeiug sulutict.3.3Aapararus and euuipment
3.3-1Gas chromatcgraph equipped with electron apture detector.3. 3. 2Blender.
3.3.3 Shaker.
3. 3. 4 Hearl xhupe flesk.250 m..3 3. 5Tet tube:15 ml..teilon-liaed screw tap3. 3.6Thermostaric waler ba:h.Nare: all Ive eg-ikswa-rs sveull L. wasiled by ul.raruaut cleauet,rinse the Elaseware: wit, lirtie u-liexye tetirtLse
3.4Frucedure
3.4.1Exuractan and clear. upWeiga 2l g(ucuurit4 la n. I gJof ifsl Nirmpl- in u Sc inl. eurien, flink with wtupparull I5 ilnf elhanl,5 rI, nt suifmric acic-warert1 +g),lo g af sadium chorice and 1ou mL af chloroform. Stop-per tightly+shake tu: 3 tnin. Tben tilier the ex:ract througa rapit lilter Psper into a 25i ml eparato-ry funnei.riosc tne conirel ilaak Bud filtcr cake with 5o mL ui chloroforu. Tranafer al. wrashiags intothr: se[?rlury [urtul. Add 2= nii, of sediu-n h:yrltuxicle solticm (30 g/E) anrd S(l rnL cl ilislillrr: water.Arll lo -ail, tacurall scdium clilaride talurion (pH nf rhe agenus phase shnul: be -1=,nthe:wise,additignsi gediut hydrxide so.ution is tleeded. Additioral 3 g cf sodium ckloride should be adtled tothe eaaily emulgifiad sample, ,shake for 2 min. Let sten2 to seperete,diszare the ch.oroisrrr. eyesWash thc agueuus yhrse witl 25 mL portiors of chlorofort vice,diseir:d the chlorofortr lawer. Andler: wanh the aujlleius ahase wich 25 mt, of etier,disrard tke ethrt I:yer, Tht i:luve muein plasi: inacidified with 25 ml of sulfuric acid-water (1+9) ard mix thrroughly (plI af the aquecu5 phaaexhoull te -2iethetwise.addixonal aulfur:e acid-ware: .l 1 9>is nsesled). Then extract thie agusuusphase suscessivcly wi-h $C,25 Bad 25 mL chlorufor, Collee: the extreet of ehlorpfsrm into 259 ml.heart stepe flaek, Evapurate llir. ehlkrifnrm 1n cn 3-s ir:l. in : water buth at 5ot uinr titrugenflaw. Tlet. 1ransfe: 1l..nitatively tr the tusc (3. 3. 5) with a Jew ni. nf ehhrrr.f:rm. F.xp-l te.e ell.ir:Earrs completely inda:ui-agen ow.3.4.2 Mernylaticr
Acd 1 mt. methylarion solution 3. 2, 12>intu the yhjvu -sbe aad esl tightly,roix rborough.y,plare -he -ahe in weter b:lli fu- _ h al ?n C. Cnnl tr room thr perater.,transer the njeihylajid solu-linu wili ra :) ml. n: xedi.m aulal anlutio: to a 25 .L tube witis 5tnppei. F x1riel wi:h .-hekanftvie at.l d ml., Trasfer rhe n-hexane bayer to atother 25 nl. ube. Extract -ae a-hexanc layer -ithuch 2 l of xadiur. sulfate ssiu: r: twige and digea:d -h= aguztus layer. lile:ie thae hekae leyer to lomL in e vo.utrtric flask. P per 3-5 mL hxuau luyer in t a ll: mL lubi, witt. sto2ut.nce. ra : g cfahydrrt.s antinr st:ligi+,mis wuil. The toluti is re.dy Enr xas -lrnatigri.ghic lhe:eue'in. inn.3. 4. 3 Freparition of me-alylated 2,3-D standarc working solntionAccurately pipelie I ml of 2,d-D giandarl so.utior: of agirable corcentrstion tu tt:be with screwcap (3.3.5),removetha galvent under n:troger.flew.proceec as 3ecio:1 3.1.2.3.4.4LxetermiEtinn
3. 4. 4. 1 GC opwriling cunulitior.SN 0195-93
R. CplumnR.a55.2 mX 2 mm6id).packed with 2. 5%(m/m) (OV-17 +3. 556(m/m>QF-1 onChramo6orb HP (8100 mesh);
b.Coiumn temperartre:22c'CbZxz.net
Injcetion port temprralure:28c'C:Det-tor ieuperasyre:2ga +
Ni1roren:puri-y99. ss%, 50 ml./min.3.4.4.2GC doterminaticn
Inject &ccuretely squal amount (i—2 μL>of the Toachylated srandard workiag solutian (geeion3. 4. 3) anc samil- solatiun (srr:irn 3, 4. 2) intu gas chruma:rgraph ruseelively. The Tespnnsrx of th2.4-D murilyl in tine stanl:ntd warking salutinn aad Rample snlutinn should be siail.r and must hewich.n the Jinezr range al the detector.The Ietention rime of 2.4- methy. is ca 2 nin uader the above conlirions.3.4.5Hlank ces:
The uperaiioa oi blank test is thu sume as bovu,but with omwsiun uf samale addition.3.5Cateuliatinn ard ekpressicn of reaulsCalculale the content of 2,d-D by GC data praccseor cr accarding to the follcwing farmul: :x
X—the residue canteat of 2,-D in test saruple.mg/kgih-peak heighe of 2.4-[? methyl in saanple galarion,ur;h.-perk height pi 2.d-D methyl in staudard soleuon.mm.t5coucentralion o: 2.4-1) in stancand so:utior.ng/rl:Vthe final valure of -he ampla solution,ml.tm-massuftestsample.g.
Netef The blzoke va'uo xna'! bn +tbaxseted fra. the abore resuie a calsulitipn.4 Limlt or determization and recovery4.1 Limit of determinaon
The lait of dererrninat:or. of this metaod :s . o2 mg/kg4.2Reresry
Ar:urdeing lu the exptrirarmlal rate,whira. sne irmrrm.-alinu l 2,4-D is in the renge uf 0. 02-0. 20 rak kg.e ret:nvery is 703%—379%.Additional raplanatians:
Tli stariaril way proruanrd by :ne Staln Aslninintratinn af Impurl arii Exurt Ccttrodity In-spection nf the Pecpla's Republic af Cin.na.Thi starcard was dralted Ly Tianjan lzport anl Exeert Cammedity Inspectio Burcau cf thePeaple's Repusie af Chiaa.
his srandard was mainly drafred by Mu Natqiang ,L.n Anging,wan HoagRetereacet
SN 0195-93
FDA-PestieideArnlycieal Munual,Vol,I,201-ll-6,i98sNctr, This Eaglist -eryion ra Tarslsuian from tive Chinese textkis golely Eor guidance.
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。