【商检行业标准(SN)】 出口肉中喹乙醇残留量检验方法

中华人民共和国进出口商品检验行业标准SN 0197
出口肉中喹乙醇残留量检验方法Method for determination of olaguindnxresidues in meat far expnrt
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喹乙醇残留量检验方法Method far delerminatian pr ulacquindoxresidues in meat for export
主题内容与适用范围
SN0197-93
本标难规定了出内中唑乙事残留后检验的冶样，制样和液相色谐测定方法。本标准适了出口鸡肉中噬艺酵残留的检验。2抽样和制样
以不随过2503件商品检验批，
同一检验批的商品度具有拒的特征如包装、标记，产池，制护报等级等，2.2抽详数量
（件）
26--1no
101-250
5G:--1 000
1CG1~2
2.3拍详方法
最低油烂效（件」
按3.2规定的拍详件数预机抽取，逐件下启，每件至少取一包，从每包中划取肉样不少于，其总盘人俘少于1kg。放人将污容内，划均后，明际记，及时遂实学京，2.4试样制备
将所取原始详品缩分出.5，取可含部分.经组织码降机据碎，均价成两伦，装入洁净零器内，密封为试择，并标哦系记。
2.5试样保弃
将试样于。亡冷冻保存，
过：在抽利详的操栏让理中些乐的样出受到染成实出物含的化，中华人民共和国国家进出口商品检验局1993-06-04批差1993-08-01实
3测定方法
3.1活提要
SN 0197: 93
将陶栏用之时提取用无永炭酸脱水，正己烷洗李。特乙随层热发至干，用平醇溶解残造，用液相色造仪选行测定，外标法定垫。3.2试新和材料
3.2、1乙确：分折绝重获瘤。
3.2.2正己烧，分折纯，瓶糊，用7服均和3.2.3中，外纯。
3.2.4期滤外，.elim545.传用前再甲酵洗涤，干，3.2.5无水限醒评：分开统.200心干燥4h，冷本后贴一密封容靠巾3.2.6呢乙醇标需品，纯度99%，32.7乙尊标准落液，精维称取唑艺醇原清品10.0mg，以少盘水将释，用甲醇择鲜至100m，取此滚0E，压甲醇带释1m..此领年我升食吃乙酵5B。上逆标准诺减击于色容量瓶内避光冷获保存，保存期--个为。
3.3发器部设备
3. 3. 1肢砂芯漏
3.3.2高速质器。
3. 3. 3转蒸发器，
离心机
33.5高效液相色谱仪,配案外检频器。3.4刚定步强
喹乙穿竭光易分解，国比要求在测定逆程中通开光綫的直接射，3.4.3提晚
标取试样约10g（物确到0.1g）+250m均质析中，加入助德剂1及乙100r:L，为质1aim，以30mo-%500z/mz高心5Tin。将上清波例人25ml.维形瓶中，再向残留物户加人50mL乙睛同洋均质、离心后，合并上活液。3.4.2净化
间上述z.堤取被中加入元水碳酸卵20，源控并放置30min，用鼓璃砂芯漏斗滤.然后向滤渣中人元己烷10nn振据n置分层，将乙临房转铭乳范形能中，在40C水中能转蒸发次除法箱荆。月中醇2mL将解然期物，供高效演祖色说翘定.。3.4-3阅定
3.2.2.1免路条件下载标准就来标准下载网
a.诺：-BoadpakC18.10m.3.9mm)X320m流动相：甲款/水（10-90)，1.5mL/min；h
色带柱溢度：5$5C；
1.抢进密长：680m
3.4.3.2也测定
根据样凌中虚之醇合实背况，送定浓度相的标准工作留液，标座工作溶减新液中吨乙醇响应值均应在仅器控测线烂困内，标准下作海商伴液等怀积参插进样满定，在上述色谱系件下，嚏乙翻保留时间约为4.8min。
3. 4.3.3空血试验
卧不加试样外，强上述德定步骤进行。2
3.4.4结果计算和表述
SN 0197—93
用色诺数据处理机或按下列公式计X
式：X——试样中坚乙略的残留盛，mg/kg—样我中噬乙醇的蜂高，mm
一标准工作落液中唑无哗的峰离，机m：—标准工作南避中乙醇防浓度能/m州称取的试样既·4
V样接采警定暨依积，ml..
注：计算结术需扣际空白他
4方法的测定履、回收率
4.1定低限0.05x/，
4.2回收率
收常的实险数据,吨2.等的凝加浓度在5. 02~.0. 15mg/kg范围,回收求为8U%～89%。附加说明：
本标准由中华人民兴和国国家走出商品验腔局提出。本标准断中国进出口商品检验技本研究所，中华人民共和国河北进出口商品登验局更交起卓本标准主要起常人庄无忌，主凤池,段交主要龄考文献：
“声水产食品中の残留物质位查法生举生活卫生写乳内卫生课编地，P185—186.Japan.
Frofessional Standard of the People's Republic of ChinaforImport and Export Cummodity InspectionMethod For determination of olaguindoxresidues in meat lor expor!
1 Sept aod ticld uf μpplicationSN0197—93
This standari specif:es the methocs of supling sample preparation and dutertninarion by highFerlnr.aner liruiel :-li-mmelugri.jhy (FPLC) of olaguindox reaiduea in mcat Eor cxport.This starcard is apzliceble tc, tiam ilelermirn li:un f ulagainkix rmvil.s in rhieken ue:l fu.: rx.port.
2Samplingand sampleprtparation2-1 Inspaerion loT
Th yuantity of en inspceron lat should nor h more than 2 5oc packages.The charaeer.nlirx yf thu cargo within the ame inapeetion lot,suzh as pecking.mark,crigingrade and sperificationsliotld be t'be smr.2-2 Qansty of sample taken
Nnles cf suckegcs n
each inspeeior: lel
1—25
26—10m
1G=—231)
25-500
sr=—1 ouu
1 cc::-2 5co
2.3Sunpling proced.are
Minimum number of
pa:k:gstobetake
A numbar of packaa* speeificd ir. 2. 2 arc takra at iaadam ar.d opened one by one. A, ieast onebag slhulu bu tascn from caca packnge, The sacaale weigh: taken aa ac primsry sampl- frorn cach bagssould be al lea+' Sll g. The total wcikh: of al p:irary san.ples shauld nut be le+ :ina: I kg-whichsaall be sealed,labeled and szn: n lantuzratiry ir linn2.4 Paeparerign uf teut samsizAiproved hy the State Admiaisiration urIniporl and Expori Lummodlly lspectlon orthe Penple's Repuulic ut Chint ua Jun.4,19931
lmplementetramAug.1.1993
SN 019793
The rurrbincd pzitnary aample ia teduced to O, 5 kg ,the edible portion is blended .and :hea dividedintn Iwr erual portiana. Eac-h rworlion i placed in a clcan eantaincr os test samplc+which ig gealed andlabeled.
2. 3Storage cl sample
he test gamples saauld be stored andet. ls cMele : In :ht courge of sapipling Snd aatape pre;iaratiuat pracaukiut musr he ttken ts avnid cnntamina.inn ar nzy fae-tei whicl utsy au'ywe lie ehange uf rerilue cun'ett.3Method of determlnation
3.1 Princisle
The sanple is extricted withs acetunitrile vand washed wi-n hexane after watzr is remnved hy anhyd:o.a pocessium carbanata,tlen evaporated to dryegs, The residue is lissoived in methanpl. The fi-ual spolutin in uus.lyuel by HPLC with UV detcetor,using exterral standard method.3.2 Regents and materials
3.2.1 Acetouitrile,A.R. -redistilled3.2.2 n-Hexare:. R. redigtilled.3.2.3Mthunl,V grade.
3. 2, 4Filter zid,Celice :-ti,washed with me-hann. anil Jriril.3.2. E Potassium carbonaie(anbycrous):A. R..heat ar 2oc C for 4b,and ksep in: a tighily alvseilcontaincr sfter cooling
3 2.6Cluquirtiox standard solutien;Prrity>s%.3.2.7 Oluuieriox Neruurd ulutin:Accuraely weigh 10. 0 nug af sLandard olajuinrlnx ial< a flink. Dinsol ve ir Fle wg-it unl diucsto loc ml, with methaao..
Trirsfur 5mL of the abavementaned soletian into 10o mL brawn volametric flask and akeup1n mark with methanil.Thr ruacrntrution ui the solution is 5 ag/mL. Storc in B rcfrigeratar t be useawithin cne month.
3.3Apparatus and equipmert
3- 3- 1 Sintcree glass fuanel.3. 3.2 Horingenicer.
3.3.3 Ratars evaaratar,
3.3-4 Certrifege
3.3.5High parformence liquid ehroraaragraph withUy detcctor.3.4Praredare
Claujimelkix Iianutin I's darampose iander liruet light, whichs chus shosld be evaided during the pro.cesses of do'erminaior.,
3.4.Extracion
Weigh ce 25 g o the test sample (aueurate to o.1 g>into a 250mL homogea:zer cup-tomogcaizeEor 1 mia witi I & uf Celile 545 ul l00 mL of ureturlitrile. Centr:fuge the maxrure at S 000-3 500I/min far min,rlunr ihn aupernatani iata s ronical [lausk,Extruse thc reaidue with 5o mL, of scetoni.criie.hortogcrize and cen-rifuge as in the above mentioued prexrilurr.(urnlin: the supernetancs ia chcrurical f.ast.
3.4.2 Clenn up
SN 0197-93
Add 2o g of anhydrous potassjum carbonate inlo the ahove exiracr,shake anc lel stand fnr 30min,tilter the mixture with zintered glass [unnel by suction. Add 2oo mL of n-hexane inta the filr-ate,shake for min and lrt stand until the layer separare. Tranafer the layer of aceron:trile into flaakre-vepurate thr s:lvunt in Fatary evaporatur at 40 C. Dissalve the rcaidue with 2 m oi mcthenol, The 5a-lution is csed for chramatoxrephy deterrainatiaa.3.4.3Determination
3. 4. 3. 1 FPLC ogcreting coudicioaga.Coiurnsμ-[kondapak Clg,io pm,a.s mm(it)Xsoo rmrn Irniglin;bMobil phase:Methanol+water(1o+go).1.5 mL/minec-Column temperarure,35C
d.Wavelegth f UV rlielreter:ss n3.4.3.2 IIF1.C determinatior.According to the appreximate corcentration of al-quindox in the sample ealu-ion,select the et:andaid workirg solucion with gimilar peak height ro that of samp'e walution. T'he reaponses of olaquindoxi.s ihe nla:lard wurkirg ialutir and sarrple sulutiun shuuld br in the lincar rurgc of the ingtrurucnzelderecion, The standard warking solucicr. alculd be injecied ta-beiwuen occasinnally with ibe sinsplesolutious of enual vol ane. Linder the above hromotogtaphis conditiors.the retensiun cime f alaquin-dux is elwu: 4.8 ica.
3. 4. 3. 3 N.ank test
Tae operatioa of -ae blank test is the zamc as that dcseribed in the mett.od af determintiau,huwith amisgion o: gample additian.3-d. 4Ca:eulatipn and cxpresaion of regal-The eaieulaulinn od reanli i: tarrieri nut by elearategriplhis lnla procesnur ur asuru:ng to the zol.lowingformula:
X = (+ ×rX V)/(h. Xm)
X-Resid.le euritrat uf uluguietinw in tus hist suaule g/kgli—Peak beigl ni aliarjuiatiox in cse aample snlalinn,mntth,['eak keight oi olaguiadox in tne staaldard workirg solutisConcentratign of olacuindox ia the ztandard working soiution,μg'mL:m-The mass of test sample-g;1—Final yulume uf aample solution,ml.Not= Tie blaak va.ue siwouid be subtrachec Erodt zhe sbove -esult of ca:sulazior..4Limit of determination and recovery4.1 Eimit af dererzinazion
Th- linit uf d-rrrimalioni is to. os ng?g4.2Recnvery
According ta the experimenta! data when the fortified sontentration of olaquirdex is in the rangeo: 0. 02-0. 15 mg/kg .he :ecovery La 83%—89%.5
Addliaul ezpiunalions
SN019793
This standard wan prupared by the State Administration of Irmpcr and Eappre Commcdi-y ln-6peraian af the Peaple's Republic of China.This standard was drafted by the China Import and Ex[url Contundity Tnspection Technalogy In-stirute ard Hcbei Impprt and Exuati Curmmmidliy Irspectinn Dureau of the Peop'e's Republic of ChinsThis s1nnilard wins nuainly drafted by Zhung Wuji.Wang F'engchi and Juen Wenzhong.Rererence:
套水产食品中の残留物质检法生省生活工生局乱肉卫生识编策。23，才牛下，P18985.Jigan.
Xote: Tnia English versionra iraraletion Ercm rha thinein text i Holely Jer gu.dance.
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