SN/T 2574-2010
基本信息
标准号： SN/T 2574-2010
中文名称：进出口蜂王浆中双甲脒及其代谢产物残留量检测方法 气相色谱-质谱法
标准类别：商检行业标准(SN)
标准状态：现行
出版语种：简体中文
下载格式：.rar .pdf
下载大小：1057KB
相关标签： 进出口 蜂王浆 双甲 代谢 产物 残留量 检测 方法 相色谱 质谱法
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标准简介
SN/T 2574-2010 进出口蜂王浆中双甲脒及其代谢产物残留量检测方法 气相色谱-质谱法
SN/T2574-2010
标准下载解压密码：www.bzxz.net
标准图片预览
标准内容
人民土利国康检验检股行业标准SN/T 257A--20/0
及其代谢产物留#检测方法
相色滑·成谐法
eteagurtir axnina it Kasxnlrt resecnim roya ieiy f ippr eageMs
2010-12-01 9:2
微研药势
含品伙伴网httn
本标雅控照GB/卡U给主的电房
本象准出间家认证获山监督信理必员媒的并！本家泽起益华位中华大民共和国湖）出人务传意检境局。本称游十除起大：期美从产中腾清开影姐http：//foodmate.netSN/H2574-2010
进出斑藤
及其代谢产物网检树方法
汽村色港·谱漆
SN/n 2574. 2010
本标准规乐了屿王浆中双甲咪&其代确产物裂绍量的气和色谱所说测定及确证方法本源准活用了蜂工浆中双甲膝及其代谢产督然留最的测定和确证学法提装
栏品深俊水解，藏化店可卡已炼（2中外职法）液合路剂提取，酸碱液-液分净化：相件详质谱测定和确证，外标法定量。”试刻和材料
除易有说所外，所出的试剂均为分新、求为蒸留不或志离了尺：1正烷：色将纯
?酸，免谱纯。
3.3两现仰露纯。
34氯化锅购烧41在下烘带内冷非单空温清划瓶中备用3.5盐酸溶液：2.00)/书移液管移权1.折醒，证水稀群定容宝5c0m1.3。5复载化销溶液：）mo称最载计年，东深解完容至130mL2双巾咪（mir%1N。A8N：3306！1，对分手成量为293）标雅物质纯度人-f93.824-甲站单联（24-dimo+ntN.A5No5-681，格刘分了质量送121）标雅物质：纯度大丁99%，
3.开咪标准落液：确称二气的双件膝准物或，用耐配成浓度为/mL的标准储条瀛。银据而爱用内自稀释年活“浓度的标1作筱。甲基胺标滩落：控称于消基苯胺标雄物设，用内丽配成浓为08/mL的标拍储备液，根据需公比内型摄整心浓的标准作液，4仪和设
气相氢谱凝谱仪：有重车密源（）4.？能满误个器
.3离机:转速大下5c0/mt
25全破膚四流装臀：
http
$W/ 2574---2010
5诚样制备和保存
5.1制样制备
股代表性样品约将禁用原产装人严治带内，帮刘，计标明标记5、试样保存
于：以下媒行：在样程中让格品受到资或发诉测物留量的变化。6测定步骤
6、1水解
你取斌详（精痛到：8→，盐俊溶骏.）旋满器上流装回冷装置加热可流，遇座游十链续摄冷部水微称滋冰中冷都15 min。
6.2提取利离化
将水解液转移到mLH宰心十，正xL正熔（继（2「1，体积比）落合剂。可加1ml参微化销溶液（6）满施漫方求+等可：i以40min离心3i，将上层有机剂转移到另-52m其宠离心管中。太×7新2（2：1达供比）池合落剂举取2次。合并1层有机相。用2品离液（2欧·并提股液并定容节0m分感m站峻概服液一19m只寒离心管中，川体识出据合辫剂2化销辫液（3.6取1获，岛心分，「量自销秋纯相白普谱测审净标法延量，6.3测定
气概色谱·质谱条件
色谱柱B5英细宿社内科）或相当者a
色潜社湖变9保持2xin.以：mi的升品速率升靠160，保持nn.以30（mh
的温速率升举2保等：：
截氮，纯斑卡筝海mm
d）#样量：：
遇样式：脉冲不分盗游，球中户5：0in店开阀：）
溶剂延泥时sm
逃样11温度25“.
接鼠度280
离子鸿:电子轰击源(E1:;
j）心离能量： V
测定方式：选择高了临测方发：选择离子及对十贝
htt
选离m动
用影长发的设华离习和相对年度13 k
SV/T 2574~->010
根斯样液中二就果胺香微的肖流送与滋中二求只胺波度性现的标体作落液，部游下作溶液剂详游中2，4，中密间高应在仪器测定的线兰的衡内，标工落波粘样单联的保智时间药为10.m证标维品的离该擎体积穿帮册样测定：在1述单件中流图移见附法A中图A，
刘你雅游液及液均陈3「惠的茶件引弹款乐样液标证裕液在相同的保留用间有递出照，心对其进行质善证在扣商肾京品间举品量图中用谛择子全部出现，同时所选择的实学的离了您成标准品！美离了根对小心哦更用合表之的最大容许谢落之内（见），可判定样品中存在2甲求胺。被简的品出学器本胶阳性注。2，一中期求接标滩品的送谱图移品图求A市图A
来？喷管时降最大率体偏繁
机华度（英
降许的和对误整：
存3.42月试验
除不加式性外，沟按上测定守象进行流睾讨算
用负增数据处理软件或按武（计货谢单双中我的费留含Axrxy
1中2的意单游分惠换算x中微的转换系数最祥中双中兹留单，伴佳为率中：需（/）释渡中中基禁有理
称准1件液中4“中书思密，单待头微配筹魔（/m）最然样液定究体科单位升）
标！作液，-“底呼而想；
-最终样滚研代表的试款单色没。http
SV/T2574—-2010
方法测定低限和回收资
7.1测定低限
本方法的测汇低限为018：
7.2回收率
女率见3
化合物
态词随源
深州浓度gs）
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激环联我雅物质的服谱图
http
SF/T2574--2010
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3.gAmitraz,Accuratelyweighapprriaiu arrrni f Amitrastandards anddigsolvewith acetaneto preparo standard stock scluticns of 1oo un/rn. Acewidir: so the conaentration recuired: pigete?appropriate volurne of the ahove szandara sni.ttk:ta anct dilute lr psorsed working sciution with ac.one
3. ro 2, 4-Dimethyl aniline standarl r.k woi :s, Arsalralely weigh apprapriate armint cf 2.4.Dirnethyl aniline standards ard dissolun w\h feinn re peparg stardar stuck solutlars t soo pg/r Accrrding lo the ranerntmitior reuirm girnris ararorriate votume of the above ataridardsolurirns snc dilule to proposed wrrkirg srhutiot wih aeetene.4Amararus anc eguipmnts
A, 1G- Ms: eguipped with o.octrnirnent sauree:El.1.2Vortee mixer
4.3 Coritrifuge.5 000 r/min.4.&Thermostat,5o c~20nc.
Gnss reflux condensor.
sPrepararion and Starkge
5. 1Freparation cf test xampieTake aprropriately 5po g of topresentative sampie,mixerd thoroughly, Then the homagerizco samipiea placed in a cleari container as the test sanple,whish s ealed and lakeled.5. 2 Storage of tesi sample
The sample shauld be stored at - 1x , tr te rurso a the sample preparatinn,precautior shall betaken to evoic contaminatiori anu ary facir's whi may case the change of residue conlert.sProredure pf detarrination
6.1 Hydrolyze
Weigh 4 gteccurate to 0. (1 g of the test. sinple mitc a Joo rnl. tiask. Add 10 m.hydrochloric acid(3. 5) and the mixiure is refluxed frne approyirnatsfy h at 12n r:. After cooling it for 15 min at reum8
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iarnsfr\ thn warer pitanc ints tas: mi. a:rt. tigen t:atus ndid l) ini. n nerane ether(2+ 1. V/V) ardA irs.odiumhysrexideta.6).Vtx Tintatyandl cat i it water beth et 5 min.Ganift net trainfer the orsganic phase>teanrtor:r.riugsTuabe.Tre:residuois extrscted again with1n mi. hwatie-ethert2:,V/vMelgkgaaic nasas.wmrganie phase is extracied wiut mt. yoisrhiorie acid. ier twe timouttr t io Iyrchlrric anis phasos ar make it to mlwith hydiachioric xcid:a. E.Traister 5 nmt. astrairg salution ints lo nl. nrmitugo tube, ad ? r:r.haxane-auatno:2 -- 1: V/v) anc 2 imi nceiutn frydexide(3. G). eritrilupe it anx the ararigaxiraut deiermined y Gc Ms.
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h) courn temperature te min oh t mintpr2oc(s ruina)tarricrgas,Nitroman-purityeass.9a%,:lw raie:l.o mL/nin::t)Irjoion olnm.2 ul.:
e)Irjsctiof mode:splitlaseoper: the Vilveaftero./s mnins&tiynt deiay timoe mr:
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Tahic -erelactest lons tt relttor, inire iy cof s a airxthyl arilineSeierted ionstm/2)
Relative intensiy/x:
uahfcatnn
Aerordng lc tne approxirnate concertiatoige: , tirmaini aniline ir ssmple soluiion:select thestadaay workirig soiutian witn airiiar raxpose : tai if sgripie snluton.The respops f thesriaiyte in te standard wetrki soiu o dry in sa nie shuion wluul b witnin he limear range tfthe mstruimwnt detecition. Tho staridarci wurkin: snlliuor snoul! re irlectec before and between thsirjsrtions of sample solition of fguui vsiure sieot i sbva GcMs cperarina conditior, tneroteitim lirne ef 2.4.imethyl anine tca ot. l i: Tst.si ion chrematograrn is snerwn as figareA.? ir: snro A.
B.3.3Confi.mation
Urrar 6, , 1 G-Ms conixiuts, if th ily i ?e i sange nromatgten peeks ate conaisen.with: tas f the standard solutien. tc Vs cronfir r.rirn resr should t taken. All seleeled ions appearin the aubtracterd chruirerogran. Furthann re.t't. dir. ve incansities nf sample lons saall corraspirnd rse of ataneard soution icrs, The t rarr. s,r repatvt i inraitiex meet with table 2, andhar a positive result \or 2,4.birmethyl anilir ra ti.i: ar: he pinvidled, Mase spectrogran af 2.4.Dirriathyl anuine in the stanciard is sow: ts list e A irs arnex A.Table 2Reiarive ion riy nd galtre reerive rularanceHelartivo ln interisrtybzxZ.net
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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。
及其代谢产物留#检测方法
相色滑·成谐法
eteagurtir axnina it Kasxnlrt resecnim roya ieiy f ippr eageMs
2010-12-01 9:2
微研药势
含品伙伴网httn
本标雅控照GB/卡U给主的电房
本象准出间家认证获山监督信理必员媒的并！本家泽起益华位中华大民共和国湖）出人务传意检境局。本称游十除起大：期美从产中腾清开影姐http：//foodmate.netSN/H2574-2010
进出斑藤
及其代谢产物网检树方法
汽村色港·谱漆
SN/n 2574. 2010
本标准规乐了屿王浆中双甲咪&其代确产物裂绍量的气和色谱所说测定及确证方法本源准活用了蜂工浆中双甲膝及其代谢产督然留最的测定和确证学法提装
栏品深俊水解，藏化店可卡已炼（2中外职法）液合路剂提取，酸碱液-液分净化：相件详质谱测定和确证，外标法定量。”试刻和材料
除易有说所外，所出的试剂均为分新、求为蒸留不或志离了尺：1正烷：色将纯
?酸，免谱纯。
3.3两现仰露纯。
34氯化锅购烧41在下烘带内冷非单空温清划瓶中备用3.5盐酸溶液：2.00)/书移液管移权1.折醒，证水稀群定容宝5c0m1.3。5复载化销溶液：）mo称最载计年，东深解完容至130mL2双巾咪（mir%1N。A8N：3306！1，对分手成量为293）标雅物质纯度人-f93.824-甲站单联（24-dimo+ntN.A5No5-681，格刘分了质量送121）标雅物质：纯度大丁99%，
3.开咪标准落液：确称二气的双件膝准物或，用耐配成浓度为/mL的标准储条瀛。银据而爱用内自稀释年活“浓度的标1作筱。甲基胺标滩落：控称于消基苯胺标雄物设，用内丽配成浓为08/mL的标拍储备液，根据需公比内型摄整心浓的标准作液，4仪和设
气相氢谱凝谱仪：有重车密源（）4.？能满误个器
.3离机:转速大下5c0/mt
25全破膚四流装臀：
http
$W/ 2574---2010
5诚样制备和保存
5.1制样制备
股代表性样品约将禁用原产装人严治带内，帮刘，计标明标记5、试样保存
于：以下媒行：在样程中让格品受到资或发诉测物留量的变化。6测定步骤
6、1水解
你取斌详（精痛到：8→，盐俊溶骏.）旋满器上流装回冷装置加热可流，遇座游十链续摄冷部水微称滋冰中冷都15 min。
6.2提取利离化
将水解液转移到mLH宰心十，正xL正熔（继（2「1，体积比）落合剂。可加1ml参微化销溶液（6）满施漫方求+等可：i以40min离心3i，将上层有机剂转移到另-52m其宠离心管中。太×7新2（2：1达供比）池合落剂举取2次。合并1层有机相。用2品离液（2欧·并提股液并定容节0m分感m站峻概服液一19m只寒离心管中，川体识出据合辫剂2化销辫液（3.6取1获，岛心分，「量自销秋纯相白普谱测审净标法延量，6.3测定
气概色谱·质谱条件
色谱柱B5英细宿社内科）或相当者a
色潜社湖变9保持2xin.以：mi的升品速率升靠160，保持nn.以30（mh
的温速率升举2保等：：
截氮，纯斑卡筝海mm
d）#样量：：
遇样式：脉冲不分盗游，球中户5：0in店开阀：）
溶剂延泥时sm
逃样11温度25“.
接鼠度280
离子鸿:电子轰击源(E1:;
j）心离能量： V
测定方式：选择高了临测方发：选择离子及对十贝
htt
选离m动
用影长发的设华离习和相对年度13 k
SV/T 2574~->010
根斯样液中二就果胺香微的肖流送与滋中二求只胺波度性现的标体作落液，部游下作溶液剂详游中2，4，中密间高应在仪器测定的线兰的衡内，标工落波粘样单联的保智时间药为10.m证标维品的离该擎体积穿帮册样测定：在1述单件中流图移见附法A中图A，
刘你雅游液及液均陈3「惠的茶件引弹款乐样液标证裕液在相同的保留用间有递出照，心对其进行质善证在扣商肾京品间举品量图中用谛择子全部出现，同时所选择的实学的离了您成标准品！美离了根对小心哦更用合表之的最大容许谢落之内（见），可判定样品中存在2甲求胺。被简的品出学器本胶阳性注。2，一中期求接标滩品的送谱图移品图求A市图A
来？喷管时降最大率体偏繁
机华度（英
降许的和对误整：
存3.42月试验
除不加式性外，沟按上测定守象进行流睾讨算
用负增数据处理软件或按武（计货谢单双中我的费留含Axrxy
1中2的意单游分惠换算x中微的转换系数最祥中双中兹留单，伴佳为率中：需（/）释渡中中基禁有理
称准1件液中4“中书思密，单待头微配筹魔（/m）最然样液定究体科单位升）
标！作液，-“底呼而想；
-最终样滚研代表的试款单色没。http
SV/T2574—-2010
方法测定低限和回收资
7.1测定低限
本方法的测汇低限为018：
7.2回收率
女率见3
化合物
态词随源
深州浓度gs）
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孜率/
75. 7- 88. 7
73. 9 --89.0
78.4~ 90. 4
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自增价动速请图
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图A12微膜标准网的总阅于流色谱图（浓度为0.0#）Y
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激环联我雅物质的服谱图
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SF/T2574--2010
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9N/T 25743070
atrrrintic h rmita nd irs eralits reirasin royaljeily ee igwa r exrortMsSebra
Thie attra spoaifia ihe rmani i: rs wliin i cwitia al his rrearelies rsidasg ig ryeljaly fer inocrt and axpr by yae enot:o ary ms spec:eto.Ms)Tis standerd in apolicabe e dgtemmirniiom : rrtmiian cf arerez arud its metabclites reslocIn ruvai joily
2 rirepale
h: anmple hiydroyre inth cneifikn l as t j .: idua is rx artod with n hexane-ethe:(? lV/vurje akalinn condritn.Al't the lic :p: o:ti:n: wih atjbase.derertinsu wy toMsad guaifd by extnal stendrd neshr.aHearglerits sst ararules
Unisa saraiicd all ragonts sinutle t of na iasal gicn, water is the distlled or daionized water.3. erer:fl'L grecte
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3.gAmitraz,Accuratelyweighapprriaiu arrrni f Amitrastandards anddigsolvewith acetaneto preparo standard stock scluticns of 1oo un/rn. Acewidir: so the conaentration recuired: pigete?appropriate volurne of the ahove szandara sni.ttk:ta anct dilute lr psorsed working sciution with ac.one
3. ro 2, 4-Dimethyl aniline standarl r.k woi :s, Arsalralely weigh apprapriate armint cf 2.4.Dirnethyl aniline standards ard dissolun w\h feinn re peparg stardar stuck solutlars t soo pg/r Accrrding lo the ranerntmitior reuirm girnris ararorriate votume of the above ataridardsolurirns snc dilule to proposed wrrkirg srhutiot wih aeetene.4Amararus anc eguipmnts
A, 1G- Ms: eguipped with o.octrnirnent sauree:El.1.2Vortee mixer
4.3 Coritrifuge.5 000 r/min.4.&Thermostat,5o c~20nc.
Gnss reflux condensor.
sPrepararion and Starkge
5. 1Freparation cf test xampieTake aprropriately 5po g of topresentative sampie,mixerd thoroughly, Then the homagerizco samipiea placed in a cleari container as the test sanple,whish s ealed and lakeled.5. 2 Storage of tesi sample
The sample shauld be stored at - 1x , tr te rurso a the sample preparatinn,precautior shall betaken to evoic contaminatiori anu ary facir's whi may case the change of residue conlert.sProredure pf detarrination
6.1 Hydrolyze
Weigh 4 gteccurate to 0. (1 g of the test. sinple mitc a Joo rnl. tiask. Add 10 m.hydrochloric acid(3. 5) and the mixiure is refluxed frne approyirnatsfy h at 12n r:. After cooling it for 15 min at reum8
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torwrsra,tranter thes Flaaik intr: kut : rx i: for s ir.t. 2.Fxtrareicn aud cleon upSR/T 25742010
iarnsfr\ thn warer pitanc ints tas: mi. a:rt. tigen t:atus ndid l) ini. n nerane ether(2+ 1. V/V) ardA irs.odiumhysrexideta.6).Vtx Tintatyandl cat i it water beth et 5 min.Ganift net trainfer the orsganic phase>teanrtor:r.riugsTuabe.Tre:residuois extrscted again with1n mi. hwatie-ethert2:,V/vMelgkgaaic nasas.wmrganie phase is extracied wiut mt. yoisrhiorie acid. ier twe timouttr t io Iyrchlrric anis phasos ar make it to mlwith hydiachioric xcid:a. E.Traister 5 nmt. astrairg salution ints lo nl. nrmitugo tube, ad ? r:r.haxane-auatno:2 -- 1: V/v) anc 2 imi nceiutn frydexide(3. G). eritrilupe it anx the ararigaxiraut deiermined y Gc Ms.
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EN/n 2574 - -2010
Tahic -erelactest lons tt relttor, inire iy cof s a airxthyl arilineSeierted ionstm/2)
Relative intensiy/x:
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Aerordng lc tne approxirnate concertiatoige: , tirmaini aniline ir ssmple soluiion:select thestadaay workirig soiutian witn airiiar raxpose : tai if sgripie snluton.The respops f thesriaiyte in te standard wetrki soiu o dry in sa nie shuion wluul b witnin he limear range tfthe mstruimwnt detecition. Tho staridarci wurkin: snlliuor snoul! re irlectec before and between thsirjsrtions of sample solition of fguui vsiure sieot i sbva GcMs cperarina conditior, tneroteitim lirne ef 2.4.imethyl anine tca ot. l i: Tst.si ion chrematograrn is snerwn as figareA.? ir: snro A.
B.3.3Confi.mation
Urrar 6, , 1 G-Ms conixiuts, if th ily i ?e i sange nromatgten peeks ate conaisen.with: tas f the standard solutien. tc Vs cronfir r.rirn resr should t taken. All seleeled ions appearin the aubtracterd chruirerogran. Furthann re.t't. dir. ve incansities nf sample lons saall corraspirnd rse of ataneard soution icrs, The t rarr. s,r repatvt i inraitiex meet with table 2, andhar a positive result \or 2,4.birmethyl anilir ra ti.i: ar: he pinvidled, Mase spectrogran af 2.4.Dirriathyl anuine in the stanciard is sow: ts list e A irs arnex A.Table 2Reiarive ion riy nd galtre reerive rularanceHelartivo ln interisrty
Slgnk tesswill ha concucred sccordinej u trowtu s snove wituut sarnpia adaition.a. 4Gaiewemian
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