【商检行业标准(SN)】 出口肉及肉制品中己烯雌酚残留量检验方法分光光度法

中华人民共和国进出口商品检验行业标准SN 0210—93
出口肉及肉制品中
己烯雕酚残留量检验方法
分光光度法
Method for determination of diethylstilbestrolresidues in meat and meat products for exportSpectrophotomeiric method
1993-06-04发布
1993-08-0.1 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检验行业标准出口肉及肉制品中
己烯雕酚残留臣检验方法
分光光度法
Mrthod Fur determinuntion of diethylslilesirulresidues in meal ant meul prudiarts for espurtSpertrnphnlametric methad
1主题内容与适用范围
SN 0210-93
本标难越适了出了内及内制造中已端两践自品检验的拍样，制详和分光北度制定方法，本标准适月于出流、牛免，鸡及出爱肉、试菜猪肉和威二缅头中己烯辅酚残留些的捡丝。2抽样和制样
2.1晚验范
以不超过250件为-检整征,同一检验批扩南品应只有相间特正.刘包装、标记产坛，死括和等级，
2.2拥单数录
批（洋）
26~·1Co
231~50
501--10bzxz.net
:001--250
2.3推联方法
按2.2划规定的轴样件数随机担聚，逐件计局最低拍片数(件）
内及内制品（能头隐外每件至少联一我为始详品谅始样品总效大·放人所诺等器内。订封后，标标记，及时选实验室。件中无小包蒙或有小塑装每装重过2剂门润（酒灭片击包件中，每件产收不让十10c多，海今后肾小冶容脂内，作为据合原性群，混在原始范或年不于2kg：加均后，标明标记，及时送交实验室。链头每件随凯或--链
所拍取的择品加过后，标明示记，及时必安验整，2.4试常备
陶及内割品（旅头除外），从所取全部推品中吹出有代表性样品约1出1.充分施率.运分，均分中华人共和国国家进出商品检验厨993-06-04批准1993-09-C1实施
SN 0210-93
两份·分别装人洁宰奔器内，密封并标明标记，做头：将所坂全部样品开罐所.充分境碎，混取出约100，均分成两学，分引装人洁净穿器内，衡封井标晓标记。
2.5试样保疗
将试以下一18冷冻存。
往：在地样和刮样的操市过理中，必新防上降易楚到导染或效些能胃动含质的变化。3测定方法
3.1有法提要
月正烷别盒每化消穿依次提皮试样中的二烯催输.取分含已烯性配的差化钜穿滤，用牌退至火，鲜水系一定怀积，比没满液在紫外灯下与照，使雅耐转变为醒式的化合物至波长418m期尝吸收值，由际准的线改得其吉。3.2法剂相村料
3. 2.1 正己境：盐断纯。
3.2.磷单外板纯
3. 2. 3两线游限11—1
3.2.4氢氧化销浮液.8mi/，求出口和15mT0.8mnl/1.笔化创落戏所需磷酸落微的落升数，以酚为指示剂至粉色例消类。
3.2.52分纯
3.2.5元水磁酸纳：分析纯.530℃灼烧41.于密问容器内，3.2.7已将证酸标准品：纯度99%，3.2.日元新盼标推港备溶脱：称已增标准品25.0加范制花生油率50.00号每活克中含
3-3仪器和设备
3. 3. 1 紫外灯: 5 W,
3.3.2分光光度计：A有10mm或40m比色池英），3.3.3识热机1.
33.4追形瓶：259mL其磨IT圳案：3. 3. 5分液确4;25 r:1. .
3.3.空址瓶：2ml.,0mL，
3.3.试，23m，磨和
3.4步媒
3.4.1标难电就的偿制
准称取三命需准烤备返10.5g含己烤维价59此2元0ml整闪中用50mL正己烧定受转移车分液漏手中。用氢氧化销游商23,2010根取三次，合并氢氧北落液，收效氧1的班液C.3:1.0,2.5,5.0.7.5和10.0m<分别含己妈雄5.5,1.心,5.0,7.5和10.C分别至一划m1.试管中，用置或化销补足至1m1.按3.2.4策单光求出的笔升数入磷配溶液，加之醇m最用水稀至2FmL。上述率液并今烯障断分别步0.02,0,1,C,10,0.20,0,33和0.北，分别取适量上述穿放肾一比色地，搭3.4.2条预先选好的幅阻条作，立紫外灯下据照，在被长m处测定真吸光变，以术报盟的落滤为参比波，拨吸光对浓度签制抗产曲线。3.4.2强3牛的远挡（件意保限，如直接接魅紫外光载）格最证当半的签询际商线的客液，1/入比色性中，乘息放性在新紫外灯约7SN C210-93
处，契照10min，在控长418nm处到忘共吸光，以未描源穿为参比胶然每积照上--2i求复测定其受光底。记录达到最大吸光度的辆照时间，重复以上试验，效收变比色池证紫外灯的距离，与至拉到最台适的条件，得出艳定的非可以其实的效大哦光度的为3.09），记猫时间距离，以与降验接此条件并行，
法，带度对妞照时间长妞存一定影的空的商括照，起，3.4.3测定
款取试作5-再确到0.1）于:5m.烧杯~52无水范醛纳.充分混.定量转维形瓶中，划入烷100mL强剂微据2mim.静，收清极60m扫当于1-12g故推置分滚递斗中2室氧化钠咨被，2mi，静罩外层必要时可改热），取1ml氧化销（相当下3-~9减样,试肾接3.2.4杀半先凹的适升数入磷酸溶微中：再加乙惊2.L.最后用永确择至25m，2下按非由我绘制3.1.1承十\取适其上还液肾丁比包池，”，进行紫外器后测定文来.
3.5空白法验
用15mT.0.8mnl/.氧氧化钠辑液代替样品育液，3.4.3系泌定出聚进行。3.6结果的计其部表述
控下式计算样品己烯硅酚含性，己靠酸tmg/kg）-m
我中：心：接测行的设光度从标市期上查得每者几落微中有的己烯啡两量·xm—每率升性液含有的试样量，
件：计算站乐需怪李片值拍净
如性品中产在太盘温格油指6计享个下己提取能球只之内。4方法的测定低限，回收率
4.1谢完低限
本方法测是低限为.05m/
4.2收率
支率的实验数期：需摊价添活度在5.05~1.20m/kk范用内，同收卓为83.9%~90.5%。附加说明：
牛标由中华人民光和国国家造山山成靠检整司供工，本标准山中华人民式和国心率违出口店5验高象责司中，本标在七要起幸人孙兆芬，宋愈点张源祥、民。主要考文献：
1. ao:t: Offieial Methocs u: Ana'ys.g s9.c18--39.521,14th hditio.lss h.3.Fa-Animal Drug Aralitical M m ai,Fe I I--s.1935-3
Professional Standard of the People's Repuhlic of Chinafur lmport and Expert Comnmodity inspectiotVethod for determination of diethvlstilestrolresidues in meat and meat products for exporlSpectrophoiometric method
1Seupe nit ftell af applicationSN0219-93
This ls:t rinrri njifie+ th: rrrilinc. of sanepliek-ganiplz prep-ia-on and dere:miration by 5pec.Inplrunmar.:y of diethylstilsestrctiDEs) residues in meat and meat Frocucis for expori.This standzrd is apaicahle to the deterrninarign ef DES res:duey ir. frozen park,beef,rubbit aad-heThu uuarlily gf an irn.weliun list slasjd not hn nce than 2 500 Fackapes.T:na ehatacta istics cf :hne cargn wittin tae sane inapection lot,such as packing,markrorigin,grade ar.o syecifizationshoule: be the aame.2.7 Quanri-y : samjile aken
Nutnber of paakages
ir rech iaspretian lu:
101—25
351—0
5011399
1591-3$cc
2.3Sunpliag arocedute
Minimun aum'ser uf
Erekagea a bu 1akra
A nusrber of pazkegcs szecifizd in 2. 2 : t tukrir a: siml: al apned ana. hy nne.Mea: unl ry- junailuintnxp rmfrl fosilr.),From eara.at leas: one bag shal be taken as a priYary samn.c.The tstal weizht of all the pnmaiy sarupiea ahanld ao: be len thar 2ky,which ztal bepla:l in a clean romeine:.scaled-.abelcd nsd sent te the sahoraluy in ti-rr.f. cas -he Erezxc. neal jis ar! nt tontuinril in kmall buge insiln er.l jiar'sg'.ur f thutu areFrn.l! ihigs inside ilr pa:kege bul rhe ccrtent af the bag *xceecs 2 kgicut ouat = part froru the neat incr-h prcsugr cl uot less thun 100 g with a sharp kntferdis:nfeeted wirh elesbol). Mix the Fa:ta of thea.t t: s he mixeil ariaary semgle,waiclt shull nst he iey4 than 2 kg- Ptare in F e.eay contuinetescal.abo il serr to the tubu-ary n limr.Approved hy the State Adninisiratinn nfImpurt aad Espa't Commodity Inspection othe Peopte'g Republic or China oa Jun.4.1993Implemealed from Aug. .1993
SN 0210-93
Canneil faads.Take l can from each peckagu at rurudurt. Tlie sanupes 1akea should be labeled sndsen: to labaratory in time.
2.4 P:eparacion uf sarugl
Muet aril mest products(except cenned meat),dt representutive sartipl- af about I C0o g is takenfru ihe combined primary eamples, blended, mixed wrill and ilien divided inco two equul postions.Each pertion is piazed in clcan cuntninrr,whicin is then sealed and labe.ed.Car.ned meh:,Tuke the rni1 frnr all the apend canx sampled,blend,nuix well ened redur: tis I nng,then dividy inin: Iw erjusl portions. Each Ecrtion ig placec in clean contaianr,whinh ia iher: sealecaml Islelec.
2.5 Sturag The test snuplei Ninculrl be srored at --1gC.Nate: Jnhh ansea ampling end aampleprrgiarutCavto:s wh.sh may esuhe the changr nf rosiditr elin'ernt.3 Meihod of determlnatfon
utubibetaken
3.1 Principle
DEs in the sample is exirar -t: wih n-hexane ard sodium hydroxide soluuon s'scessively. A pir1.on cf che extract 1r lnin.ng TDFs.is tasen and adjusted with phosphorir urid to aH ca 8. Art. aleahalaruu H,O r, n defiaite volu.c. The elean solurioa is irrediarec. witt. Lrv lighe,under such coaditicn theIDFs is changed intu quinoid compound,and the r.buurlsnit aif the 5olutian is uoasared at +'B nrn. TheDES zon'ter,r in caleu'ared from thu sriulinl rurve.3.2Reagees and nmtrrial:
3.2.1 -He..me.A.R..
3.2.2 Phospaoric acid:A. K. -3. 2. 3 Phoxpharic acid selatwt; 1+43.2.4 Sodium tydruxid: x:ilni.rn:0. R mol/LDulwrmine the roililiters of phosahoric acid soiutiaaC:+ l)rsyuireil fisr unulraliaia 1i mL ot0. R mol/L NatH solution usiag pbenolphchalein as inlinalsr junl Ln the disappearence of pirk color.3.2.5Aleoho..A.R.
3. 2. 6 Aavydrius sod:iti slphate : A. R.. Igrite for 4 h at 6C C .store is s well cigntl imlziaer.3. 2-7TES standard:Purity9.
3. 2. 8 DES nrandard groak sslutior:A:ct:rarely wrigt: 25. ing ut DE5 slarul.ril.l :eiired gcanut cil to oual welaht of 5G, O0 gTG. 5 PR LEST- OL.).
3.3Appuratug anc eqaipmeat
3- 3.1 I lan2:15 w
3.3.2Spwtrophoromtrur,Wiyl0mnor 40)msabsouptioacelistqrartz).3. 3. 3Blesdr.
3. 3. 4 Elmeyer flaxk:2=c ms. with ylasa arsFFer3.3.5Separacory fannsl.2Ec mL.3.3. 6Vulenerie fiass;23 ml,.50 mt..3.3.7T'ekr tubes:2o TriL wit's gias5 stopper and graduated.3.4Frocuci:r:
3.4.1PreEBration of gtandard rurveSx 0210-93
Arsurintely weigh 100. 0 mg f DES wluncard iock sulution(rontaining 53 μg cf DES):nto 2 50l.beaker.then guanti-atively trans[er t a ezar.anry funnn'with br) n:L of n.hexenc.E'xtrazc earee1.mex wth NaCH ao.urion(2c,20,10 mL),combine thc extract Na)TI sclutinn.T'ruaniler thr aauve s0-irtiau 5.5.1.c.2.5,5.0and10.0 ml.(cortain:ng 0.5,l.0.5.0.7.5aad :5.0 μR of DF5 yespectivey)ir t i xtries of 25 rnL tust tubes+add NaOH soiucicn uF ta the volune of 15 mL. Add Fl,PO, ealution,the amoun: of which in determinad ts in 3.2. 4,to nevtralizu -he solution. Add 2. 5 ml. ct a,cosol.fi-nal.y add H,O up to 25mL.
Fhe ccncerirationx of the abovs zalution are 0.02,0.C4.D.10.0.20.t..30 ar:rl C.41 ug DES/mLre'sjertivaly. Tranafer the ubove solutiong into an abserprian cell suc seszively acccrding co the irraidistinn candirior. of a. 4.2.pare i:ndar Liy liyht.uutl rensurc the absorbance at 418 rn &gainst the u-nirradiated solutioa as a refcrence solution.arid: prepare thr xlanriarri curve by plorting abaorbance vsconccn.rgnon.
3. 4.2 Irudiatiun orditions sclecting(Caurion,Proreat eyen from direct LV ight).T'raasfer the PF.s Ni utivn tn, O+ reg/zLinre B 1C mm abaorpelon celi,aed place it vertizally ca7 ct un:le: a 15 wasts UV lamp. Izradiate for 1G mir.an:l nitahurr tle ahyorturee at 4is nr. sagairstthr anirradiared DEs so.utior aa a refarenice. Repeat absorbance msasurement afre: rt, _-3 min irra-il itinsre.nlil lie mr x valv uf nhsurbance obtaired.record the time af irradiazion.Repeat chc abeve measurement ,change Ilue linianrr lretwien Uv lamp end cel,uuti a stasie andrepeatable coud:tions are found cut,the max abeorbance shnuld! be t:s n.o9.Nul-: Tine uf :rridlinrun anntsme: c:F Lrrilclint::>n.
3.4.3 Jetermination
rarure,the higher the so.s ta.peature,thr tholter theWeigh 5—15 of samplctaccurae to 0. 1 g>in A 100 mL beakeriudd 2C --50 g of ar.hyi.rnus s:diam xulg:ny r ian:l rrix tlraaghly.T-anefer tte mixture ttauiraively intn a 25int ml, Erieuruyrr flask wit stopper,add ic3 l oln-kexane.shke vigcrously for 2 min.and set aside uuti a ciear anluliun in pkivirud, Trunsfer 8o ultucarivalent -o 4—12 5eroplelof thig clear roletion irto a soperatary tantei.add 20 ml.nJ NaOH s:il.Tlon,sin.k vigarmsiy fer 2 min.and st escie fcr =eperatng Proseed =s in a. 4. a.using 1fi ml, of t. 8 ail/l. Nut >H xil.s. inslhis.3 : n.irmile so.uclcn.3.S Ca.culslion aad expression ot resultThir runicnt of DES is ca.culated by the formala.JDFSt.g/kg) = w;im
mi,nh+ ef Fst+r milililr iaf finul ien, ilalionttouul ro, the standa:d susve aceording co absorbancereading.μ!! — civrrexpondiag mase of samp.e in each milliliter o: the final teri woiuli:ml g.Ntte L:The Llinh va.ue. sneoni:t e xuharnetrd frnm the niv.ve rsi:lr l caletlatisr.SN0210-93
Nase E,[e a iarge of Eat existx in samp.e,the vntume sf Eat mun: be calculated ir, valume cf n-exarr extrast.ALimet ar determinution and receveryd.1 Liit of dere:minarion
The Jimir uf ectermiratiou of this mathad is C.os mg/kg4.2Re:uvery
According to the experirnental data,when the concentration of DE5 is in the range cl 3, 35-1. 23mg/kg,therecoveryiaB3.9%—sc.0yAdditdoaal explanations,
-his s-eiulard wax arivpus-l ly th- Starr Aslrininlration af Trmgaprt and Expvel Conrulily Tapectiku of thPenple's Repuh.ic af China.This standard was drafied by the Tiaajin Import and Expert Commodity Snspectioa Burcau oi th:Peaple'g Rezsblic oi Chine.
Tsis starular! way rainly ilrafhet ay Snn Zh:ofen.Sung Finfr-ig-Zhng Zher xiang-Yi. Rnrin.Reference:
1.AOAC-Dff.c.al Merhods cf Analgais 39.c18—39.021._4-n Editian,19342.FDA Arimol Drug Aaalytical Maauai,Feed I-&.iuxs.Norsi'his F.nglsh verxionia tranxlaripn fror. the Chinese text,is sc.ely fot giid nc.
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