【商检行业标准(SN)】 出口禽肉中乙氧喹残留量检验方法荧光光度法

中华人民共和国进出口商品检验行业标准SN0282—93
出口禽肉中乙氧喹残留量检验方法荧光光度法
Method forthedctermination of ethoxyguinresidues in poultry meat for export-Photofluornmetric method
1993-12-28发布
1994-05-01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检验行业标准出口离肉中乙氧喹残留量检验方法荧光光度法
Method fot 1he determination of ethoryguinresidues inpoultrymeatfor exporlPhotofluoromelric method
+主题内容与适用范围
SN0282-93
标准视定了出口舍因中乙唑朗量检验的推样.制挡和荧光光度别定法，太标准适压一出口鸡肉中乙急喷残曾见的检验。2抽烊和制样
2.1检验北
以人超过 2 5CC件为一检验批
同一按验批的商品座具右相同的特往：如包装，标记、产地，规格和等级等。2.2拍样数量
批，件
3i--1GC
101--25c
251~·500
5a1-1occ
1 031--2 oc
2.3抽样方法
最低拍样效，件
接2.2规走的拥样件数随机由取，炼件开底。每件率步取5C0多或一稳作原始样品，原始样品息盈得少于2。加封后标味标记，及时送实验齐.2.4 试择制条
将所收原始样品增分出」k，取可食部介，经组识摘译巩报降，均公放份.装入消协穿器内，作为试样，密些，并标明标记
2.5试祥候车
将达样于一18%以下冷冻保存，
注，在油择和部排的择作过型中，为新止择品受再污巢成置牛残臣物含量物变化。3定方法
3. 1方法提要
以异辛烷提取试趋中乙氧噻，将有机相与硫慢-疏酸钠溶液一起掀搭。曦提取液经加赋波谢节PHI中华人民共和国国豪进出口商品检验同1993·12-28批准1994-05-01实施
SN 0282—93
后.再用异辛烷提取，异辛完提取液供荧光光度法测定。3.2试润利材料
3.2.1环辛境：分折纯。
3.2-2磁酸;分析纯，
3.2.3南酸许离;0. 15.mol/L,将 S. 4 mL疏加到500 mL相水中,稀样到 1 000 mL.3.2-4酰酸钠;分析纯。
3.2.5施酸-硫酸钢熔液，将20k硫酸钠溶汀10)mL疏酸落液中：3.2.6驾化钠：分护纯。
3.2.7氧化钙落液6mol/，将240g氢氧化钠解1C00mL蒸水中。3.2.3元水硫载钠分折纯.650亡灼烧4h，冷知后储于干燥器巾。3.2-9无水碳醛钠：分折纯。
3.2.101.氧本标准品，气93.8%或其他比知纯度的标准品）。3.2.11乙氯唑标准落液：准确称取适的乙氧噻标随显，月异辛烷配成浓虚为1CC/mL的标催储备溶薇，根据需要再配成含乙甄肇11g/mL的标准工作溶液。3-3仅群利设备
3.3.1爱分片光度汁.配有10mm石英比色显：3-3.2组织势降机。
3.3.3分绒斗：2Gml
3.3.4带等器。
3-3.5维彩瓶，兵离口室，150ml3.3.6容盐瓶：10(mL
3.3.7全鼓瑞系就蒸增装胃
3.4测定步张
3-4.1提取
移取试祥约5精确到0.1)于研钵中，加入1无水硫酸纳利无水碳致钠。均匀，在干燃器中放1h，将十炼过的馄合物放入1501.证形瓶中，加人1(10mL异亲烧，最落30mi滤入2 mL分液潮牛中，
3.4.2净化
将辛境提取液每欲划入ml.碰酸-硫酸韵缩液轻摄，推提1min，共进行两次，合并酸提取波护加人10mL主北钠溶液（6mol/L），用2×50mL异率烷提取碳生降液。合共异卒炭提取滤并用元冰益酸钢下源15mr；倾析消范并用异辛烷稀释至100m，供荧光定。3.4.3测定
3.4.3.1荧光杀件
微发液图：365m
b.乐返长.410nm
3.4.3.2标准曲线的翁制
在1个50mL的容基所出.分别加入0..1.n，1.5和2.GmI标准工作溶液(10R/mL),用异率效筛释定容。窃液需当大配创，以费光延度与对应的乙氧睡举度（邱/mL给制标准曲费。3.4.3.3荧光分光测定
测定样波中乙策噬的英光强度，样波中乙求唑含量应在仪器检的线让范围内。止标堆曲线查得样微中乙的依度（/mE.)
3.4.4空户试验
除不加试样外，按上述测定步骤进行。3.5结果计算和表述
下式计算试样中乙氧唾残留含最：SN 0282—93
式中·x-
一试详中乙氧唯残留量，mg/kg1乙氧唾的浓度，/m
V样能品降定容体民，l
报—称取内试控量8。
注：计算流遇需抑除空白位，
4测定低限、回收率
4.1测定低限wwW.bzxz.Net
空方的定限为o.1g/kg。
险收率的实验效据：乙氧添如浓度在.1~.0mg/kg范围内，回收率为73.9%~9，1%，附加说明：
本标准出中华人民头和辆国家进出口商品检验后提出，车标准由中华人民未和国达江进自口商品检验尺负贵起草。本准土要起草人郑自强、唐红苏、徐充。恭文，
Official Methods of Analysis of the Association of Officie! Aaalytizal Chemises,sn edit:cn.968.48.1990
Professional Standard of the People'g Repuhlic of Chinafor Import and Export Commodity laspectiorMethod for the determiuation of ethoxyguinresidues in poultry meat for export-Photofluorometric method
7 Scope and field of applicationSV 02B2—93
This staadard szecifies chne methads of sanuplirk,samp.e preparatinn ant: dalermiwninn lyphotofluoromeury of ethoxyyuia ridaex in pou.tryalea:fo:export.This standurd is muril:cable to cac determniaation uf cthoxyquin residscs ia chicken meat for ex.Fnrl.
2Sanspling and sample mreparntion2. 11:u-pri:1ian lul
The quantity of =n inspecon Jat shou.d not be more than 2 joo pazkeges.Tha characteristics af the cargo uithia the same ingpection lot,such s packing,tnark.origin.s[ueification and grade,should be cac satec.2. 2 Qua:1il.y nf srmple takenNuuler uf prrkagus in
each inspection lot
1—25
151—250
251—500
$51-100C
131250
2.3Semelmg pri:pilr
Minilti number of
packakes to be 1aken
sen at rzndom and apeneti ore by one.The quarlilyA number of pckages specified in 2. 2 are ta'stakrn as the pzimary gample From eaek package should be et lcaat 5oo grarns or uur bag- The totalw+igh! ul :-ll ari-.ary si.inples shuuldi iut bu less thar 2 kgwhi:l, xhall be ealed,laleled and scat tJaooratory ir. time.
2.4Preraraton of lestsaple
Apprnrecl by the Stale Admialstretion orImpnrtand Rxpart Commodity lespectinn afthe People's Rrpubllc of China on Dec. 28.1993Lmplemented from May.1.1994
SN 0282...93
Th, rcnhineel prirrury uanpl, is realuced to I kg rthe edille portions are blended ,aad then diviwedinto twp equal portione. Eech portion is placed in a clean container as the test sample, which is thenaealed and iabeled.
2-5 Srorage of teat gample
The tes:sanupies shuutd lur stured below-ls'CVote, In the course ef xarypling and sample preparafzetors whiph my chur the chunge cf reidue conten.3Method of determinatfon
3.1 Prple
Th ethoxyquin is extracted from the rest sampe with ispoerene,and the organic phase is ghakerith sulfuric acid-audium sulfate salution. Tac pH of the rxtract is adjxsted with elkali and the solu.twtt is [sexirarll wil isuoxl:-. The ixoti:l.ine exleaal is used Ear phninunrore1.ric de1erminaian.3.2 Reakents and materia's
3.2.1 lsooctare.Analytical grace.3-2.2 Sulfurie acid,Aralv-cal grade3.2. 3 Sulfrrin: auid xriluia. d. 15 rmm:l/T.. A:ld 8. 4 mE. f N.alfurit: acinl ln 50o rml. e[ il.slilleil w.nr.and dilute to 300 mL with disti.led water,3.2.4 Sodiurn sullate:Analytical grade.3- 2- 5 Sulfuric arid sodum su.futr solution: Dissuivr 21; g uf slium su.faute in 1 o mL of snlfuriarid aohins.
3.2.6Sod.un lydroxide:Analyical grade3. 2.7 Sodium hydroxide soletion,6 mo!/L. Disaolve 24c ol sodiurn hydroxide in 1 QcC mL of ci.eilled watar.
3.2- 8Ar:hyleuaus suxliunn snllale: Analytical gtarle. Ignile al 6soC far 4h amd storr in a ilesitattir.3.2.9Arhydroja sodiuni carbonzte:Anelytical grade3.2.10Ethoxyguin standard.Purity 93.Bh(or arandard ol otner krown purity).3. 2. 11 Ethoxyquin atande:d aolution,Acruruzuly wcigh En adequate Bmuunt uf ethoxyguir. ssendertl,dissolve in isuutanr aril prepare Esalutinn oj l00 g/mf. as lhe kianiare sicuk solulinn, Acxarding tn the requirement.prepare a ata:dard working solution cortaining ethoxyguin pl Ic ug/mL3.3Appararus and equipaent
3-3. 1Syirul.uoropaotomcter,Eqappce rith 10 mtl quartz crll..3-3.2 Hende:-
3.3.3 Separarozy fannel.25o rt..3.3.4Shaker.
3.3. 5 Coaical flusk:lst mL,with ground scopper 3- 3. 6Vuluanel.:ie: Flask :190 m..3. 3. 7All-glas distilling system.3.4Frocedurc
3.4.1Extraction
Weigh ca 5 g (accuryle tu d. I g) of che teat semple in a mortar and add 1s g of arhyerous sodiumxulfate and 2 g of anhydrcus sadiur carhanate,grinu unil uniforn and place in desiccatpr for 1 h,SN 0282—93
Slake the dried mixture for 30 min in a 150 mL conical flask with 100 mL of isooctane.Filter into 250 ml. geparatary funnel.
3.4.2Clramp
Gently ahake the isooctane extract for Irain twiar,each tine with 50 mL of gu:furic acid-godiumsulfate solution, Combine the acid extracry and add 1G ml of sodium sydroxidec solution ( mol/L).Eatraet tae alkalinc solution with twu suxessive o nL porlioun or ixaorleirr. Comhine the isnoctanecxtracts and dry for 15 min wi:hs anhydraua odium eulfate adecant and diluce ta 1o0 mL with iscactanefor determioation.
3.4.3[ete:mination
3. 4. 3.1Paoto[luurunietric: aperalirg condilinna.Fxeiatinn wavelength:3i5 nrnb.Emission waveleagth:4=o am.3. 4.3.2 Preparaign af standerd curveAcd 0. 5,-. 0,1. 5 and 2. 5 mnL ul slamlarrd warking arlulinm (l. C pg/mt.) tn four 50 mt. vaiumetric Elasks and dilute co volurun with isooctene. Prepare freshly for daily use, Construet the atandardcurve by plotting the fiuorescence intenaiey against ethoxyguin concentratior(pg'mL).3.4. 3.3Phstafluosamecrie determinationMerisiirr ili- lurescenre iniensicy aE the sample solution. The reecings shoulc be in the linealange of the instramental detection. Obtain the concentratioa of erhoxyguin (pg/ml.) in the samplesolatior. from the siandayd curve.3. 4. 4Blans test
The operatiain af the blauk test is the same 2s that described in the method of determination,bulwrithout sddition of sample.3.5Caleulation and expreasion of regulcThe calculatiun uf ethoxyguiu rexidlue in ile Iret sample is carriec out accordinr to the fallowinsmuation:
X—thecontcntcfechoxyquirrim ihe leni sample,my/kg—thecuncert:rariponaf ethnxyquin in thoample solutior pg/mL;tithe Final valume of eample solution.ml:m the mass of the test sample.g-Noue: The blauk vaug Ehould ba zubrseted from the abore resul: o: eplculstinn.4Limlt or deterninatlon and recovery4.7 Limit of determinarioa
T'ae limit of determination of thia mcthod is U. I rng/kk4.2Recpvery
SN0282—93
Arcurding lo the esperiruental date, when ihe fortifying uoneenlrieliou af -thuxyuie: is in iherange af 5,10,0.80 mg/kgithe recovery is 73. 9% -.94.1%.Addillonal espanations:
This standard was progosed by the State Adrninistration pf Import and Export Cominedicy Inpeclinn nf tle Penple'e Repuhlie of China.The star.dard was drafted by the Zhejiaag Import aud Export Commodity Inspection Bureau of thePeople's Rep.iblic of China.Principel drelfters;Zheng Ziqiang,Taug Hongfang,Xu Liang.Reteree:
Official Methods of Analysis of the Associstion of Official Aualytical Chemists.isth edirioa:968.48.1390
Nore: This Englieh version, = tranelaticin frora the Cininese text ,is solely lor gu.daae-
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