【行业标准】 进出口蜂王浆中11种有机磷农药残留量的测定 气相色谱法

华人民和出人检骏检疫行业标准5%/T 2577-2019
进出口科有机磷
汽相色谱法
农药残留量的测定
TDetrmaaiae r ebwak goosp u hestiefela resixlts itrpyal iey ft ingari aint napracris ciraaaleyrtphy2010-05-27 教布
微码弱伪
金品伙伴网ht
201012-01 2:
本标准按照G，T1.-20C9给比的规洲放本标雅中国家认证认可监督性率瓷负象究中平师。本标滩出中华人低洪和浙江出大途编店市品超学。本你游主要超草人，点义订慧资、英商鸡韩留，张避被，http：//foodmate.netSN/T 2577--2010
二科磷
最阁意制航相的普诺
SN/ 257---2010
本标准视可进中口虾「浆！种在须避承药然留测定的制祥和气相色谱测笑方法：不标翟三州丁蜂峰下聚山段恢畏、中酸滋兴线溝、中拌楼、系架、甲基对硫磷、百拉筛微、对蔬磷、喹梳磷、二唑磷、频奇磷农药残留量的检测。2规范性强用文件
下列义件对于本文件闪应用步必小少的，州是注川期的兆节文件仅注！期的版木适用下本支件，凡是不注石满的用文件，其赢教最本（心指所有的修改单）站用于本文性。（1/T6682分新实验用水规络彩威验方读3#游擦装
与7脂提联样品中有机磷衣药，最限液还微按价谐在净化，片断有火焰光度检测器的气杆色谱仪测流外标法完常：
4试剂和材料
除见有规定外，研有试剂为分断，术次T682规定的级水，1.17.峻二酷，高效色谐级，
有名肺：高效液相！色游效
1.不已烷高效液剂色谱领
4、1两酬：高效涨色谱波。
4包化钠。
6无小碗酸钟：购烧在烘我密温，价密封瓶中备用，心洗脱激：酸书坏出
4.3·收做线，早滋麟、灭经磷、中料消、乐4送对硫减、4拉确剂硫磷、嗪硫磷、三咚磷、烧舞磷标雅品纯度大干等下染您附求A表。4.311种有磷标准器备落波：分制称61予价能品（4.8）：分鼎用内阴落解定容至10m溶液浓保效：
4.1种有机油企标准作整：临新市托出密用内酮能解全适当浓，作为混合标滩1作液1%4冰箱渠存。石效法3个月，款准1作润液浓度，0008/mL，0.01/mlo.n5ug/ml..o.1pg/mL.o.3ag/mt..4.谢腔净化成品（心r：.n内格：质料：BioBcadsg-x3.38um~7um微前整川标准液先假淋洗市！，
12小确搬钠在：80×m（内形落斗底部垫m脱棉再装50X水确httn
SN/T 2577.- -2010
酸钠。
4.13N为基之一胺露介神晚！PRA15
投器和设备
51相色仪，配有火炸光安检（离来5分大平，感.0
5.微软热发器：
5.4新揭混个器。
5.5良心机大于等于6occm
6试样制备与保存
取500代装性降一装祥州4我品下单车，年与部证化店将试举均分成两份分别装入樽品靓，时，并标明标证，份为试器样弱心8保存．制样的染作过程中成院山样品污染或发生线留物含壶变化：7测宽步骤
7.1提取
称安战样精确到理潮料心人求银静5加瞻至刻度ml，旅涡混介器以?送心m：mm.以5/mn离心5in移取1游液置于男一个50mL塑料肉心件中m人4以t然，量个器上以2000/mm，混句1mm以6000m离心5mr将点溶湾开本，：收！浓练瓶加人m水和20z精至残酒，币复！述操作自并将玛房液”以下水济微压游缩金诞于待净化：7.2净
残渣用落剂4.7)定咨至51aL源询.、，上清液过GPC法、J1），流速1nL/min，用落剂4.7)洗魔，弃前15m1.萍洗液，收条：1：.的洗悦激在0以下水济减乐浓练至进下人两阴滚解在以水当中爆急气款收个车准确加人m内耐，游勾加0.05018S4，湿创热套以式降淘定7.3测定
7.3.1色谱条件
价谱性，细管0t内）1um（膜感），惑机半者我气氮气度大.慢下.6：吹线流速30m/mm：氧s）
气流速：5mL/mix.室流速.，
漏：初始度120保#1n：科#2以2℃℃/n争270保持12.min;
样口湿度20;
检测器湿度：250（：
班斌：脉冲小分路证样冲活：脉冲时0.75m2
雪品伙伴欧ht
讲详：
阁时前m
色灌测
BN/T 25//-2010
限据性品中设有机读农药的高，连量略积讲为徐准二作溶液、标准作落液利祥液中名种有机磷的制道低动成在仪靠的续性草学，小作性落液和样陵等你狼等独别样测定。也述的谱聚件散敬恩、甲股瞬、火发半禄、异乐甲式资遇流微、刘，唯确鞘、呼磷、烟毒磷的贫保时间分约为2.us， i/mixo 0 mnj3mmin214.6mi，2r标准的e多陶录中图17.3.自诚验
除个加就样外与接课作安紧量行苏酷架计算和滚递
百谱数据处机或按武，兴试书中备种机避的残留今降，计筑缩集带扣除空自值：R.y
就鲜中机磁资农商磁科量单代准维工克样液中有机象头发药商用测
标准工件液中有机涉类药的降理一析雅作液中有机满膜然的密典单位微克每意开（m）样减教终定体视，总位为还！
能悠样漫礼在的诚证量，单行
京汉的测实低限和创收率
9.1方法的测定低限
种名机磷戏留密新究低限为
8.装回收率
可收密的实验数据(在不同添可度和司的)娠表。神移机确趣国顺密款间（）
教微所
徐川得//
httn
tnnrmn+e
回收率，英
82. 6-..67.
88 5-8,6
SS/T 2577--2010
中其测硫税
马拉硫磷
对硫群
培研露
三醚磷
种有动磷容添加回收减宽围（）（续）htt
回设率
6. 6--:10.
3. F.-. 10.
20. 8.90.0
0%,R---59. 3
85,8. 90.8
97. 3~. 110. 6
71 2---78. 6
16. 0...1. 5
95.8106,1
73. 2--$5. 8
70.8 -- 78. 6
88. --198.2
.110.n
标准物款
敌做展
灭线漆
激硫磷
峰酸微
中·a想端额希品
表、1
m.th::n.tloubs
Hrtet.o.te
pa:thiun-me.tyl
alathict
http
新机游标准器响息
18285 82 4
13194·48-
295 03-2
631·5
139303-8
24:15 47-8
53-2 4
C,u.o,C,r
C:JI,N Ps
C, Hi. O PS.
C Ft .o.Ps.
CH: NO.PS.
C H. No.JE
Tetno, Pe
C-hNO: Ps
C..H:N.O.P3
. HeN.O. PbzxZ.net
G.II CHO PS
tonrmnte
SN/ 2577..-2010
机对分下资尿
220,98
SN/1 2577-2010
数收摄.xin)；
-单股麟(,y n):
火綫磷(7.3 min):
甲伴碰(7.9 mimn);
牙果。min)
中流臀：11.0m);
马拉滑微门11.3min：
对辨(11.3 min):
哮磷（12.2价示）；
三唑供(14.5 mia):
呢等情（1.？tu）
烧科性树录
标法色谱
11种有机磁混含标游品落微（0.0/ml.的气相包谱图httn
NN/9 2577.-2010
\nis srandrd was Drpostd hy t.sksst the charger: ef cerifiation and acareditarionacministrion i the Peapio's terautils: t iisu.This sranuard wata tdrattec by Zhejin rririv sin hieticr art Cuaramine burea.The wiandard was nairly draiteas by Xle ie pir Hi. vlra Huyang eifurg.Han Chao.Znang Huinir.http：//
foodmate.net
NN/T2577-20110
Determinaticn ot eleven rrgaroppesphorus pesticidesresidues in royal jelly for imrort and export-Gas chrtamatouraphy
1 Scope
Tne standard specifies the mothods ct aampie sxaration and determnination by gas thrematography(Gc) of nlaven orgenophesphorus pesticides esicuas in rcyal jely samgios for expsrt anu impat.This stardard is applicaole to the determination nt dishlervus, metharnidpras, ethopraphes,pharate,dinethoate,paruthion-methyl.rnalatttion.paratnici,uinalphos,triazoanas anu cetsmspncs nroyal jally somples.
Normat:vereferances
Tae following normative docurnents contrin grovisions which, through reference in ilis text.crnstituta provisions cf this Professional Standard. For dated references, subsequent amiendrssrts:To.or revisinns of.any af these pub!icaticrs rie not apoly. Hewever.parties to agreenents bases inthis Professional Standard are encouraga to .nvestigate rik possibility cf aaplying the most raon:sditions rst the nernative cocuments indicated peiow. F:tr undated relererices, tre latest editier ctthn normativedocurrent referred toapplies.GR/T 6682Watei for analyticel labaratory use---peifirstion and test melfads3Princinle
Crgancphasphurus pesticides are extrarred ttn Fhe searnzls hy aceteonitrile. The rezidus ars cleanedLe wh (pc aalumn. Finally it is determner by ttp,uwinsgi exterrn! standard miethod.4Feagerits and materials
Unless orherwise specified.all the reaffent lsed srcule ht analytical yrade,\water\ is GB/T eGB2dcabls distilled water.
htt
A, 1 mihyl acoare:Hrl uade
A.?Agatoritrile:hPiC grade
A. ?Gyalohexure: Hpi arare.
A. Arelono.Hrlc girade
. adiun chsride
SS/T 2577:: 2010
A. cAnhvd:sus sdinm sulfate:ignite for A h at fsu C .crul to rcom lemperature ir desiccaror cnskeoinatisghtiy slasad nainer.Elutenisolution af Gpniylacorarrytlxale(+:v/v)A. Standa d of dichlerycs. mcthunidophs, rhor-rsphs, omerare, dimothoate, pnrathicn-methyl.ralation paruthion tguiraiphow, thazophes ad xuriapks: purisy gs%.Other infematior s?a:nx A tas: A, 1.
4, R Gtark slarcard sniuitina.Accurtely wr'rl an erertate anmnvnt ef oach arandard(4. B),cissaly?wif:zcetcne and quentinativly ony\wninstric fiask irdiidualiy,tha toncentration essadutioneare100 /mt.It shoule oe storiC4 in relrigrraterSteakstanlarri soluticnis stsble tor thre morths.
a.lnWoricirg ataruard aolution; Arc rg te thn icentraticn reguired,the mixru nurdarworkiw soluticn is prepard Tror tha siork gnlulixrs by Rretore. The toncentratians are n. cos p/.rs co. o ag/ml .0.05 μg/mi..0. 1 ps/int.n. 5 ae/mh..t.1cacoluma:o0mnx15mnti.cj:ain.Eeads:S-X3.38gm/5um (elutad curveshould betiene efie asinc the titt cohimn.A. 12 Tl.umir of anhydrou? gorliam tau.lfat+, oh: + x s tpni ki. d) cylinder furinel pack wich ca 5 mmehorberi. cuitem Bt ehe botioiri ct sh csh. t+ a:et fI i so irm anhyarchs sodhurn suhate.4. 13 03A
5Apparatus anes wexsipr ngt
n.Gan chrorretograan eigipxen with Fiatinn gh.irrnetris deteeter (ghesphereus tilter.52B nr).G. 2 Falant:a:Accuracy o. oot 1 ty aici n. m ahtt
SN/T 2577---2010
s.aFotary vac:uurt evaorerir5. 4 Verrax mixer
、sCeriritugo 6 to) rinin
Preparaticn ot test aarnple
Fcyal jelly is aonut hoo g. The sariple melrar imetr rtn! tarnperaiure. Kcp tre prepared sameeintc twe sample bottles, Boal anr take : Fhe m snmple : toned at rosrn temperarure. The restsamaleis storod iniaCrofrirerateinhetts.f se nde preriaratim,precautinns she:l betakan toavoid nontaminatlon or eriy\aerors.wnicPey caisthe hange f iasictue conienr.7 Anavticai Procedire
7.1 Extrcter
Wghca 5g of the test sarnple tacruraten.( inic bi) ml cantrifuge tuhe.Add 5 rnLwaterare rmix it,sland Icra min.Acd thomi.wiib ti:iiln.Vrtoxfor 1 min unler2oo r/min.centrifuge fer 5 min tinder 6 ooo r/rin. Frans\er tarerretant iavsr irto a cereritune tube. Aad t. gsediurn chioride and vortex for 1 rnini trsim s so -/niis.renirifuge fot b min urader a oon t/nin. Thesupernatant layer was pisecd thitouigli ary.cous ninrn ghulfare colmn inte flask (4. 12). Aaa 5 rml.wter ar zo ml. acetonitrile to renmat thrr r:ncue. Gerrkir: acetonitrile extracted suiulisn ardsvaporate to nearly dryness in a water thatl: oelnw go e.7.2 Cleep up
A:d iuted soluton (4.2) te diosive he reiju: and guantisatively on 5 ml.vslumatrie flask.mixthe solution. Transfor 1. O inl the anye seittii in; ti Gpi: coiumn (a, 11).Flow rar of GPcesllmr: is 3 ml/min.eute with oiutard nal!tha 4.t;,rt wcard 1s mil elured soluraori,ce!lect elutedsalutiun is from s ml.to 30 irl.Tne ufec sniut n vaioiate tu nearly dryness ln a water bathheiaw ay C, Thko residues are terhissnlvsi in s irn. wemm,hhnr just diyness wi-h N? gas in n ware.bstn baiew 40 G. Tha reaidues 1s ectiltiritt: r 1 o itoitsmix ifr solution. dd o. te cO. 1 g FsA(4. l) vinix tte soluticn, Fr kolsrien s thasse: throuuh o. 45 yin Filtar. The soiuticn isroaty for GG determination.
z.Dererrnitiation
g. a. nc: opxrnting condisirisa)Calurn: fusad silica capilary rolurrin.y 1yo tat in * o. a mrn tt. : × 1. D gmi.er tre eguivaert:10
http
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。