【商检行业标准(SN)】 出口饲料中棕曲霉毒素A的检验方法

中华人民共和国进出口商品检验行业标准SN 0347—95
出口饲料中棕曲霉毒素A的检验方法Methud for the delermination of ochraloxin Ain fodders Tar export
1995-05-29发布
1995-11-01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饲料中棕曲毒素A的检验方法Method far the delerminatinn nf ochrainxin Ainfnddernfor expirl
1主题内穿与适用范围
SN(34795
：本标准规定了尚间料中接出市索A检验的旧样，侧种高效依扫色送测定方法。本标准道用于白针豆糊些、三米拍粉，莱打粘粉等切料棕曲裤声素A的检验，2抽样和制样
2-1检翌批
以不超过0一愉整批，
间检验泄的商品产县有明司的特征，加包装、标记、产地、规务、等级等2.7拉持数证
接批总袋数拍方根式（1力抽收。a-
中：N
全批我数：
一-抽栏您数，
计：以些联基数，小教支间的讲品为整题2-3拍祥T具
2.3.1金属单节抽样器：全长15-~75m，摘口长5~5..凹宽1~1.84m.次火录，录大外约2. 5 cra,或其他等数样临
2.3.2收样护铲
2.3.3分样、温机市，分详台外参样板等。2.3.4排1简（袋>：可谢封。
2.4伸样万法
2.4.1袋内协推：效2.2规岸的扭推装数（和除色包他样装数）车境绿四周上、小、下各部位出统形走向，随机拥收等指向下以排袋-自依斜对勿方向指入整内，燃户将打旋转望工，他出订性器，立门入盘样穿器内，包稳项样品教以应述一致，2.4.2判包两样从摊求的各部位随机抽度2.2条规定的抛样件数节10%（不少」3包）.格可线全部近并，平分举个减真地资的铺垫物上，放于紧费底两单提起约5m高到1.5m区企部倒出后，铃在货物内外观，味，有为发障，变质等并查者货内和货间品是否均分，确以行说正带与.用取样争随机存各部微抽取样品，作也收样数量座-收。2.4.3人样维价，单造内和别包所取的样品，」分样市上，渴勺，使册分样板教四分法缩分推站个少F4k，何入盛样容器内，加村行，标明标记并及时送实验室。2.5样谢符
中华人民共和国国家进出口商品检验局1995-05-29批准1395-11-01实施
SN 0347:. 95
将品编分！，全事碎道连2℃日筛，冬，均分成内装人法容器内密封你期标记。2.6比样保存
湖试排于5心下避光保存。
3别定方法
3.1行尝
档品法统山减牵案A经坏取，净化、缩示元以乙髓1.5%乙为流动柜，采月高效相它恶风英光控测器迷行消定，外标法定量，32试剂和划
隐有制定外，试净尚为分析纯水为超等水3.2.1艺清
三然因烷。
3. 2. 3 不细酶[佛程 a0 --GoC)。3.2.4 益酸。
境酸，优级纯，
乙酸。
碳酸须溶微：38/，称碳氢钠溶于200水中。总化锅将液：4g门.称40g化漆I0cmi-水市3. 2. 9
氧化萨-微酸落微：左L就化钾落液（3.2.8)中加4)r:T。浓硫膜。规取齐乙腊-点化短硫酸溶线（3..9)（S6+10)，3.2.10
3.2.11出穿求人标能品：经度的，3.2.72棕典举款A标准片各变：称夜梯时需#式A东雅品（辨至0.0001R配成5~10ml的率载，作为答波，可用装外分光光度法标定浓度（品大收球被长333L分子103，度尔消光乐数为5。
3.2.13禁出变市聚A标准T.炸说：用Z谢将上述购备滴精确帮释成缺终浓度为C.1Jg/raI.的你准1牛液，
迷标避落微图货低于色制：收遇冰菌一1！内保存。3.3收器利设备
3.3.高效液对色谱疫配备炎光洲需利自动进偿设备：3.3.2格碎显。
3. 3. 3报减器。
3.3.4选报发露，
3.3.5格剂过滤器.游适用有机总膜。3. 3. 5
次唑滤顺C.45m，
3.3.了全服高系统食然留装置
3.3.3微诺款器;.[...JG..
3.4则准好
3.4.1提取
取3.拍确笔试提于25案维张瓶中1提吸剂3.2.湿润瓶案，益紧，要商m房，以地递定源纸过滤，1ml.奔重，用提取剂洗成源数改，您能股终定容全100mL：收定客片书滤股5c，ml.于分度漏牛内用行油酰萃圾两次（次用量2)ml.）等大泪旅医，在-求层加20m.水，月三氢中统三求取邮索时见依次为25.1515m）弃长水层，析二氧平焙溶液市：六碳酸氢钠落液收三次（册次用量2m.），收崇水层合并装.并用ml/1.SN 0347:- 95
蓝酸调作水游夜pH约1. 5后,再用三能中惊三次反些取事系(用址依次火25,15,15 mL>.合卡三达-氯中爆层，升低温冰箱内一%心冷冻，滤去冰水）然全格人能转发器于~心下然千，哦法用乙腾1.5片乙接55十45>溶解，井定客至1.心-nl.经0.45m滤膜滤至样品瓶内：世微机负谱仪定。
3.4.2谢定
3.1.2.1色谱案性
免些柱;34 mm.:2. 1 m内径),5μm 固定相：JJVPD1silD统动相，之-1.乙酸（+，整器剂过诺能然，超波脱h.
c.流理：0,2ml./min
d，荧光验测器激发读长：333Trml发射波长；4rr。3.4.2.2色谱测宽
待上述许条件稳是片分别将标准作液依次以，,自到进样相当于棕曲每套索AG.2.0.4.0.6.G.5.1.0吨到降面积与进样成的标准工作准0.2~1.G线性转因比），分别将标确工作波和样等车秘参插过样定：以外标法走虽。上述件，探零每考A的保轻时约为.40n，
3.5空白试验
不加试样，传用不台格山举每案A的豆拍粉，上米粉或菜杆动粉接上述源定步媒进行。3.6给果的计弃和录最述
用单谐数增处理机或责止计算试样综曲解率责A的含站：A.c.v
武市，，
试样中棕曲需需惠A的含量g/kg；A
液你素的峰积
x 1 000
标准！作商中核曲要毒享的睡面！地标准作被中偿曲每京A的依度·鸿/mL：量终体L
3，录然样滤所扣当养样品质量·。4、测定低限、国收率
1.1到宗低限
本方法测定低根为降/kg
4.2可改
回收主实验数据：棕曲需事案A依度弃20-50/kg化币内.收净；93.%95.9%附加说明：
本标准士中华人民头和国国家过出南品检验局提。本标雅由中华人民未和国东选出口商品愉验质和深圳进商品检验尺负责超学本控布上要起草人李寅家、潘坤水、张艺吴、志辉。Prafcssional Standard of the People's Kepublic ofChina for Impori and Export Commodity InspectinnMethod for the determination uf orhraloxin in fudders fur expori
1 Nope and field nf applicatinSN 0317—95
Tlis :tindly:dl +Erriles the mcthod of zampling, ear:ple prepuration un:l delerr:natinn by higlFe:tormance 'iguid cbromog:apn f orkraroxin A in indd-r: for cxport.1 his s:anderd 1g yaalier.ble to tbe uraniu,'ra. uf ixh.xin A in atsle 1 nal awder,mviztl pwwde uml -pp npr.d -' pnwder For expnrt.2 Stcupling and sampte urepanatinn2. 1Telir h
Fec.n mepcction knt shtuld not extteu s=c ton (50o tana at harhou:).The caaraeln:iariea nf the catgo wthin the st.me insrtusu. Jut,nu-l, u nkinu.irirk, ruigin.spee:ficarios rnd r-ude +stwu.d b thr rrnt..2-2Qt.intily nf ample Takcn
Tte scuare ruoi of the toial nuimber af brgs in a lry shall be ruken s tia tumbur ul hag lo arameler..
winere
A .. r.:al aunber of haks in a Inat?rutnber f hugs1o be sanpled.Nle: If value e, is witlh dee.ual, rounc off thr incima. pa,whica is addet an witv I, ibt iuegral pa -. o. ..2.3Sumplietols
2. 3.1 Mh : lite sempler: [enpth, 5.1. 77 cn; leagth ed grove: 5t 55 cru; wicth o: groave: ]-1. cra: sha.pe ol gruove tip:shar2; mnaximun autar daneter rzu 2, b cmsor utter c.tivaln. upi-r2. 3.2Sarpliay shovel
2- 3. 3R ifl- -iampirr,iinh ahee1 for sarplz nuixing,table and place for cuarerirgtl:2.3.4 San:pl can bag?.which can he sealcd.2.Sampling grocccurc
2. 4. 1 Sipli-g fr:srt - lag5Toras the: araples tru tt:e uumber o bags aperiied in 2. 2 (nurua thc number of thc si.ruplucbags by eraplyisg ca? ar followssAlnng the sine wavu ef the gilu,d:uw -aplin frsrv ili- inigy f .lh.Apprtved by te Stafe Abmlnistrallom ofImportandKxporCommadityInspecilon ofthe People's Reublle of China on May.29.1995Implemenled from Nw. [1.1995sN 0347—95
mpu.r,rnilir und luwer purty uf cae pile at rendom. Insert the sanpier,with :ta groove facirg duwn-ward,diagonalty inin Hecl, ug.ilnr luru ilug hurpler by Iu',cirt.w out the semplcr,end prosplypour the samp.c into a container. The quanticy of ihe kanupin. ilawn frsr: wiurh hug shall he basiuilythe same.Mix all the aaruples frcm diffetem baga to lurm d gross zample.2.4.2Saruplig by rajtying uucTras 1o percent of the nunler sl hiagn kprcifin-il in 2. 2 [rut Irsy hen 3 bags?,ungcam end opehile bag -arul lay it onl a clean cloth sheet (or other clean aheet), Grasp tiyhl :wr: trrltrs rf the luig l.atom and raigc up to ea EC cra,tug baclkwhyd far ca I.5 m, Aller all contert ot the bag is cmptied ut.Pnrk .s ap:narint:uduur uf th guods and whethr: the goods are moldy,:ollen etc, Alsu ctnuckwhether tle qcal:ty of the knnda ig irmfonin within al lelwew, ilu luags. Aftur cunfirmiag thc goodsare in noraal cunditior..scup up ac randon. the sample frant differen: par.s nf ilr um-umrr.l unntwich a ahovel. The quantiry af the sample drawn from euch bag zhocld be baxica.ly thc sanle.2.4.3Rih.ticnt of gruss sattudePon.r the 5snple frnm 2. 4. I aad 2. 4. 2 ran a elrun nheu far quitering atnd iasx.reduce to nat ieaathan J kg with a plate by quarering, Place in a sarple ronta.ner,nesl,Inbei rinil seml lu tin. laburaturyintim
2. 5 Pre[ralicn r.f Igal warpleReduce the 6anple in ca I ky -l'nd thnrtuglily iul lei pann thruugh tush sicve,m.dvidin:o :wa equal pariigas .and place in clean containerz seai and label.2. 5Storagu of rst asmple
T'inet I-sl sitnjrl. shall ba. ssural bulow C and kcyt away from light.3 Metlol uf determinntiun
3. 1 Principle
The s:lnalixin A in ilm sampl: ik kitacicd+jurified and conceneraree,and whih acetonitrile1, 5 zcctit acid as raosile phase,dererminated hy HPl.c wil, Jlmurunr diglestur, using cxtcrnalsiandard method.
3.2Rcugunts atid r.ateiala
Tinleea niherwne xperifinit,all thr Trgent% xhall be wua.yticully pare,watcr :a the redianilled watet.
Aceroninrite.
3. 2.2 Calurofurm.
3.2-3Prirrilumi rihr(3:gisc:1.3.2.4 Hydrochtoric acid.
3. 2. 5 sulfuric aeid,G, K.
3.2-6 Aeuic id.
3. 2.7 Sadinm bicarhemale xrimtinrn,50 g/l. Wuigh bl: g of sodium bieeroonace ,dssolve tr. 1 ca5 rel.of water
3.2.8 Potaaium caloride solunion:40 g/L. Weigh z0 g of yotassium chlnrice.disnnle in I hun ml.sifwiter,
3. 2. 9 Sulfuric acid-pntat.um chlorile nelutirut Arlid 4sb mL uf suifuric tcied to 6u3 ml. of ecrassiumcaloride olulig (3. 2. 8.
3. 2.tExtraction aoluron.Acetonit-ile-u.furic wcid-putussium caloride slatinn (.2.) (9-lo)S
SV0347-95
3.2.11 (ehrataxin A standard,Purity 95%3.2. 12Ochratuxin A Rtangaro Rtock scl ation, Acruraicly weigh an udequate amoane of sendurdochratoxin A Kaceurate to U.oo 1 g)ediswolve in acetomitrile and ururaurr a soiuticn f 5—lU ng/rml. igche stlulurid stusl, snluim. Ihdrrmne r'se uencentiation with u'traviolet epectropaotometer (maxi-rme ahorptien Peak is at 333 tm.molecsle weigtt is do3,mulzl exinglio. coeffiecieal is 555c?.3. 2.13 Uchratuxir: A standarl worang salution,Tilure tne ochratuxin A standerd stock aolueic toO. 2 ug/mL uich Bceturtiiri's as tha, f'umk ntantlarrl working sululiein.All ilnwe ximlaid rolulions sihosld be kept in browr. scaled via: and rcservec in a ireezer-18.
3.3Apparatusandeguipmenr
3. 3. tIligh perfurmuru liquid crriztrilngtuph.riupphil witis lucreeeue deleelnr arid allesaraple.
3.3.2Girinde:.
3. 3. 3 Shaker.Www.bzxZ.net
3. 3.1 Rotary evaparatur.
3. 3.5 Glusi vneumn, litratinu rlevire fnr organic 5clvente.3.3.6Disensablefiltration rm.branet.45p3.3.?Glass rechatilatros ceeipment.3.3.8Micu syringu,l nt,lG ml..50 gt.lotul..3.4Pncednre
3. 4. 1Extraztic
Waigh abour lo. C g(aesurare to U. I g) l thr: grurned test surmpl. in 2ho rt. Fr'entyur Il.r-kwits gtujur,udd Iol:, l: mf.wxraraiox ro.ntwonJ. 4- 2 Jererttir:ation
3.4.2. 1HPL uptrai,r 1oreitiuna.luar.ngapiaiccolum.:otmmx2.1mm(id).pmrn.Scable phanetHyporwil (MS, Mebiie ptase,Acezoarda -.5% rcre neid (G-t.S5?.f:lterzdluider vscuum through 0. 45 μn menbreneanc. tir.gaxu:rl with: suanr>srin: ileviisft.Flw rate.t.e m:f.fruirg
Fluarescencedeteclor:Excitatioawavelcngth333nmemisxiouwavelengih 46ti m,3- 4. 2.2 HP1 lriermin: licirnSN034/95
Wheu the work:ng condicior. is Atable .auamatinally feel ir: ilm Nluml: ril wi,rkieg suuricr! 2 pL l.6 jμL.s rL, lu peL rwspectively (corresponding to octratoxin A,0. 2,0, ,0. fi,G. s, I. n up),l..Frcrrc Estandsrd workiur curve of oshrntoxin A contentsaghiasi ihe Feak areas.The tundard w! ling su!utiur shoall be injared randumly in bct en rge injeasicrs of he kamiple sslutirn nf ejual visinmn in the lineal enngm isf o. g-l.n rg,t:ning rxirrual xtenclatd.Lnder the alave caruretugrephic roaditian,tae retention time oi ochrrtoxin A is hrril f. 4tm:n
3-5Blarik le
Tle operation of the blank test is tte eame ae that descilber. in ihe meihn. af lelrrra.ulng-s wihCul zrdition of tesl sanple.but with tae xoybean neal powder; or maize meai powdet.nr rape seemeal zowder which ia dcrerinaced ro be free fram achraLrxia A,3. 6Culeulalioni arrl pxpriss'rst r.f dhe risulThe ralenlatinn of coents of ochraloxin A can he enirial ut liy bmunalagraphic tli ta xucessingsystem sor by the feliowing tormela:X
Crterut cl ochratuxin A in test wumple.rg/kg:A rk irca of ochratexin A in samp.e aolution.mml, Pr.k area of ur hratcxi:a A i tanderd wurking olutiul,rr;CozruutratinnsufurhrtuxinAinundnrdwurkingsulutiuntpa/kgVFinal volume ol 1enl aamplr nlution,mi.FmCorrcsponding mass of ciae sample in the final test saragle bo.uricr n.4Limit of determinatipn aad recveryA.1 Eimit nf determinatirn
The linit ot determiuztiun ot this method is 20 mg/kgA.2keery
Aceorliag te thu exprrincurel datt.,whes the forilving unentratien of chratnxir A ts in ihrrany nf 26i—52 /kg,lhe :avery i, 90. 4—98. 9%:.Adititioan explanatinns:
This etanda:d wa: prspased y the Stete Adrinietratiog af import and Expnrt Cnmmodiiy luxiettion of the Penple's Republic of Chirs.This :tulprul w cr:.fiel hy the Shanduag timl Shenzhen Imyor: nd Export Cemmrdits Inspeelinn 15ureans- :f ih Perol-s Rapelln: n: Chinit.Tinis xtandard was rns:nly drafted by Li Yinbin,Par. Kunyang.Zharp Yibing.Cai ZhipuiNirr::Ihn: Fnpish wrsi:n
rmisl:rnni fron: -hi t'hincir: rnx:,is nlrly fnr Reidancr
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