中華人民共和國出入境檢驗檢疫行業(yè)標(biāo)準(zhǔn)進(jìn)出口動物源食品中克倫特羅、萊克多巴胺、沙丁胺醇、特布他林殘留量的檢測方法液相色譜-質(zhì)譜/質(zhì)譜法Determinationofclenbuterol,ractopamine,salbutamoland2007-05-23發(fā)布I本標(biāo)準(zhǔn)的附錄A和附錄B為資料性附錄。本標(biāo)準(zhǔn)由國家認(rèn)證認(rèn)可監(jiān)督管理委員會提出并歸口。本標(biāo)準(zhǔn)起草單位：中華人民共和國上海出入境檢驗檢疫局、中華人民共和國河南出入境檢驗檢疫局、中華人民共和國湖南出入境檢驗檢疫局、中華人民共和國江蘇出入境檢驗檢疫局。本標(biāo)準(zhǔn)系首次發(fā)布的出入境檢驗檢疫行業(yè)標(biāo)準(zhǔn)。1進(jìn)出口動物源食品中克倫特羅、萊克多巴胺、沙丁胺醇、特布他林殘留量的檢測方法液相色譜-質(zhì)譜/質(zhì)譜法本標(biāo)準(zhǔn)規(guī)定了動物源性食品中克倫特羅、萊克多巴胺、沙丁胺醇、特布他林殘留量的制樣和測定本標(biāo)準(zhǔn)適用于動物源性食品肌肉和內(nèi)臟中克倫特羅、萊克多巴胺、沙丁胺醇、特布他林殘留量的檢測。2試樣制備與保存2.1試樣制備從所取全部樣品中取出有代表性樣品約500g,充分絞碎，混勻，均分成兩份，分別裝入潔凈容器內(nèi)。密封作為試樣，標(biāo)明標(biāo)記。在制樣的操作過程中，應(yīng)防止樣品受到污染或發(fā)生殘留物含量的變化。2.2試樣保存將試樣于—18℃保存。試樣中的藥物殘留采用pH5.2的乙酸銨緩沖溶液提取，同時加入β鹽酸葡萄糖醛甙酶-芳基硫酯4試劑和材料4.3乙酸銨。4.5氫氧化銨。4.8冰乙酸。4.9β鹽酸葡萄糖醛甙酶-芳基硫酸酯酶：含β鹽酸葡萄糖醛甙酶134600U/mL,芳基硫酸酯酶4.10乙酸銨緩沖溶液：0.02mol/L,pH=5.2。溶解1.54g乙酸銨于900mL水中，用冰乙酸調(diào)節(jié)pH到5.2±0.1,最后用水稀釋到1L,于+4℃貯存，使用期為1個月。4.11乙酸乙酯-氫氧化銨(97+3,體積比)。使用前攪拌，同時用超聲波水浴超聲使成均相。4.12鹽酸溶液：0.03mol/L。取30mL,1mol/L的鹽酸溶液用水稀釋到1L。2萊克多巴胺(分子式C?H??NO?CAS號：97825-25-7)、D?-萊克多巴胺純度≥98%。4.14標(biāo)準(zhǔn)儲備液的配制(1.0mg/mL):分別稱取約50mg(±0.1mg)的特布他林、萊克多巴胺、克倫特羅、沙丁胺醇標(biāo)準(zhǔn)品于50mL容量瓶中，用少量甲醇溶解，然后用甲醇配成1.0mg/mL標(biāo)準(zhǔn)儲備溶液。低于5℃保存，有效期為1年。4.15同位素內(nèi)標(biāo)標(biāo)準(zhǔn)儲備液的配制(1.0mg/mL):分別稱取約50mg(±0.1mg)的D?-克倫特羅、D?-沙丁胺醇、D?-萊克多巴胺標(biāo)準(zhǔn)品于50mL容量瓶中，用少量甲醇溶解，然后用甲醇配成1.0mg/mL標(biāo)準(zhǔn)儲備溶液。低于5℃保存，有效期為1年。4.16混合標(biāo)準(zhǔn)中間溶液的配置：用甲醇分別稀釋標(biāo)準(zhǔn)儲備液至終濃度約為1.0μg/mL和100.0ng/mL,低于5℃保存，有效期為6個月。4.17混合同位素內(nèi)標(biāo)標(biāo)準(zhǔn)中間溶液的配置：用甲醇分別稀釋同位素內(nèi)標(biāo)標(biāo)準(zhǔn)儲備液至終濃度約為100.0ng/mL,低于5℃保存，有效期為6個月。4.18標(biāo)準(zhǔn)工作液的配置：根據(jù)需要，臨用時吸取一定量的混合標(biāo)準(zhǔn)中間溶液(4.16)和混合同位素內(nèi)標(biāo)中間標(biāo)準(zhǔn)溶液(4.17),用水稀釋配制成適當(dāng)濃度的混合標(biāo)準(zhǔn)工作溶液(參考線性濃度范圍為0.5ng/mL~10ng/mL),每毫升該混合標(biāo)準(zhǔn)工作溶液含有同位素內(nèi)標(biāo)各1.0ng。低于5℃保存，有效期為6個月。5儀器和設(shè)備5.1液相色譜-串聯(lián)質(zhì)譜儀：配有電噴霧(ESI)離子源。5.2渦旋混合器。5.4旋轉(zhuǎn)蒸發(fā)器。5.5感量天平(0.1mg和0.01g)。5.6超聲波發(fā)生器。5.7恒溫箱。5.8真空過柱裝置。5.9吹氮濃縮裝置。5.10粉碎機。6.1提取稱取10g(精確至0.1g)試樣，于50mL塑料離心管中，加入20mLpH為5.2的乙酸銨緩沖溶液(4.10),在2000r/min下渦旋混合2min。添加200.0μL同位素內(nèi)標(biāo)物(4.17)于待測樣品中。加50μL的β鹽酸葡萄糖醛甙酶-芳基硫酯酶，加蓋后超聲提取15min。在恒溫箱中于37℃酶解16h。以3800r/min離心10min后，將上清液過0.45μm濾膜(4.21)取5mL濾液于10mL帶刻度的玻璃將C小柱(4.19)和SCX(4.20)小柱按從上到下的次序裝好。依次用5mL水、5mL甲醇和5mL0.03mol/L鹽酸(4.12)溶液以1.0mL/min的流速過柱活化。轉(zhuǎn)移過濾后的提取液至固相層析柱的頂部，以0.5mL/min流速過固相層析柱，此步操作至少需要10min。用5mL水、5mL甲醇淋洗小柱，在較強的負(fù)壓下抽10min。取下Cg小柱。用12mL混合均勻的乙酸乙酯-氫氧化銨溶液(4.11),洗脫SCX柱子上的待分析成分并收集洗脫液，并在吹氮濃縮裝置上于40℃±5℃的溫度下蒸干。加入31.0mL乙腈+水(1+9)振蕩溶解殘渣后過0.45μm濾膜。濾液供液相色譜-質(zhì)譜測定。6.3.1高效液相色譜條件a)色譜柱：Cg柱，150mm(柱長)×2.1mm(內(nèi)徑),粒度5μm;b)流動相：A:乙腈+0.1%甲酸，B:2mmol/L乙酸銨水溶液+0.1%甲酸；流速：200μL/min,梯度洗脫程序見表1。表1梯度洗脫程序表梯度時間/min流動相比例/(%)05786.3.2質(zhì)譜條件a)離子源：電噴霧ESI,正離子；b)掃描方式：多反應(yīng)監(jiān)測MRM;c)霧化氣壓力(GS1)、氣簾氣壓力(CUR)、輔助氣流速(GS2)均為高純氮氣或其他合適氣體；使用前應(yīng)調(diào)節(jié)各氣體流量以及離子源溫度(TEM)使質(zhì)譜靈敏度達(dá)到檢測要求，詳細(xì)條件參考附錄A;d)電噴霧電壓(IS)、碰撞電壓(CE)、去簇電壓(DP)、碰撞室入口電壓(EP)、碰撞室出口電壓(CXP)應(yīng)優(yōu)化至最佳靈敏度，監(jiān)測離子對和定量離子等詳細(xì)條件參考附錄A。6.3.3定量測定根據(jù)試樣中被測物的藥物含量，選取響應(yīng)值相近的標(biāo)準(zhǔn)工作液(4.18)同時進(jìn)行分析。標(biāo)準(zhǔn)工作液和待測液中四種藥物的響應(yīng)值均應(yīng)在儀器線性響應(yīng)范圍內(nèi)。如果含量超過標(biāo)準(zhǔn)曲線范圍，應(yīng)用乙腈十水(1+9)稀釋到合適濃度后分析。在上述色譜條件下的待測藥物的參考保留時間分別為3.0min(沙丁胺醇)、3.1min(特布它林)、9.4min(萊克多巴胺)和9.9min(克倫特羅),標(biāo)準(zhǔn)溶液的選擇性離子流圖參見附錄B。6.3.4定性測定按照液相色譜-串聯(lián)質(zhì)譜條件測定樣品和標(biāo)準(zhǔn)工作溶液，如果檢測的質(zhì)量色譜峰保留時間與標(biāo)準(zhǔn)品一致，定性離子對的相對豐度，是用相對于最強離子豐度的強度百分比表示，應(yīng)當(dāng)與濃度相當(dāng)標(biāo)準(zhǔn)工作溶液的相對豐度一致，相對豐度允許偏差不超過表2規(guī)定的范圍，則可判斷樣品中存在對應(yīng)的被測物。表2定性確證時相對離子豐度的最大允許偏差土30土506.4空白試驗除不加試樣外，均按上述操作步驟進(jìn)行。7結(jié)果計算和表述用色譜數(shù)據(jù)處理機或按式(1)計算樣品中待測藥物殘留量。計算結(jié)果需扣除空白值。4………………(1)式中：X——樣品中待測組分殘留量，單位為毫克每千克(mg/kg);c——標(biāo)準(zhǔn)工作溶液中藥物的濃度，單位為納克每毫升(ng/mL);c?——樣液中內(nèi)標(biāo)物的濃度，單位為納克每毫升(ng/mL);A——樣液中藥物的峰面積；Aw——標(biāo)準(zhǔn)工作溶液中內(nèi)標(biāo)物的峰面積；V——樣品溶液最終定容體積，單位為毫升(mL);cy——標(biāo)準(zhǔn)工作溶液中內(nèi)標(biāo)物的濃度，單位為納克每毫升(ng/mL);A;——樣液中內(nèi)標(biāo)物的峰面積；A,——標(biāo)準(zhǔn)工作溶液中藥物的峰面積；m——最終樣液代表的試樣質(zhì)量，單位為克(g)。8測定低限、回收率8.1測定低限(LOQ)本方法肉和肝的測定低限為0.0005mg/kg。8.2回收率8.2.1肉中克倫特羅、萊克多巴胺、沙丁胺醇、特布他林添加濃度及回收率試驗數(shù)據(jù)見表3。表3肉中克倫特羅、萊克多巴胺、沙丁胺醇、特布他林回收率數(shù)據(jù)表藥物名稱添加濃度/回收率范圍/(%)藥物名稱添加濃度/回收率范圍/(%)克倫特羅73.4～96.4沙丁胺醇80.8～91.698.5～126.5104.7～110.986.5～102.073.5～78.5萊克多巴胺90.6～98.8特布他林80.6～108.091.7～108.990.0～97.390.6～98.880.6～108.08.2.2肝中克倫特羅、萊克多巴胺、沙丁胺醇、特布他林添加水平及回收率試驗數(shù)據(jù)見表4。表4肝中克倫特羅、萊克多巴胺、沙丁胺醇、特布他林回收率數(shù)據(jù)表藥物名稱添加濃度/藥物名稱添加濃度/回收率范圍/(%)克倫特羅94.6～100.8沙丁胺醇77.2～89.878.3～98.477.3～92.090.5～99.073.5～80.0萊克多巴胺96.4～100.4特布他林77.2～90.695.5～122.080.5～94.992.0～108.573.0～79.55(資料性附錄)質(zhì)譜參數(shù)a)電噴霧電壓(IS):5500V;b)霧化氣壓力(GS1):50Pa;c)氣簾氣壓力(CUR):20Pa;d)輔助氣流速(GS2):30Pa;e)離子源溫度(TEM):550℃;f)碰撞電壓(CE)、去簇電壓(DP)見表A.1所示。碰撞室入口電壓(EP)為10V、碰撞室出口電壓(CXP)為13V。表A.1β-興奮劑及內(nèi)標(biāo)碰撞電壓、去簇電壓參數(shù)表母離子(Q1)m/z子離子(Q3)m/z碰撞電壓/V去簇電壓/V克倫特羅277.3203.0*259.2萊克多巴胺302.3284.3沙丁胺醇240.2222.1特布它林226.2D??-克倫特羅286.3204.0D?-萊克多巴胺307.2D?-沙丁胺醇243.2a為定量離子對。6(資料性附錄)標(biāo)準(zhǔn)品MRM圖譜pairs):277.3/259.2XICof+MRM(13Max.2.7e43)pairs):277.3/259.2XICof+MRM(13Max.2.7e4■XICof+MRM(13pairs):277.3/203.0amufromSamplc3(std3)ofData061120.wifT(TurboSpray)Max.9.le4cps■■XICof+MRM(13pairs):286.3/204.0amufromSample3(std3)ofData061120.wiff(TurboSpray)Max.3.7e4cps■■XICof+MRM(13pairs):302.3/284.3amufromSamplc3(std3)ofData061120.wiff(TurboSpray)Max.3.1e4cps.■XICof+MRM(13pairs):302.3/164.2amufromSample3(std3)ofData061120.wiff(TurboSpray)Max.2.le4cps■XICof+MRM(13pairs):307.2/167.2amufromSample3(std3)ofData061120.wiff(TurboSpray)Max.3780.0cps圖B.1克侖特羅、萊克多巴胺標(biāo)準(zhǔn)品的多反應(yīng)監(jiān)測(MRM)圖譜7■XICof+MRM(13pairs):226.2/152.1amufromSample3(std3)ofData061120.wiff(TurboSpray)Max.3.4c4cps.■XICof+MRM(13pairs):226.2/107.1amufromSample3(std3)ofData061120.wiff(TurboSpray)Max.7840.0cps.■XICof+MRM(13pairs):240.2/222.1amufromSample3(std3)ofData061120.wiff(TurboSpray)Max.2.0e4cps.■XICof+MRM(13pairs):240.2/148.1amufromSample3(std3)ofData061120.wiff(TurboSpray)Max.6.4c4cps.■XICof+MRM(13pairs):243.2/151.1amufromSample3(std3)ofData061120.wiff(TurboSpray)Max6810.0cps圖B.2特布他林、沙丁胺醇標(biāo)準(zhǔn)品的多反應(yīng)監(jiān)測(MRM)圖譜8AnnexAandBofthisstandardareinformativeannexes.Thisstandardwasproposedbyandisunderthechargedofcertificationandaccreditationadminista-tionofthePeople'sRepublicofChina.ThisstandardwasdraftedbyShanghaiEntry-ExitInspectionandQuarantineBureauofthePeople'sRepublicofChina,HenanEntry-ExitInspectionandQuarantineBureauofthePeople'sRepublicofChina,HunanEntry-ExitInspectionandQuarantineBureauofthePeople'sRepublicofChina,JiangsuEntry-ExitInspectionandQuarantineBureauofthePeople'sRepublicofChina.ThestandardwasmainlydraftedbyDengXiaojun,ZhuJian,GuoDehua,LiBo,YangJizhou,DaiHua,ChenHuilan,GuoJunfeng,WangMeilin,ChenMolian.Thisstandardisaprofessionalstandardforentry-exitinspectionandquarantinepromulgatedforthefirsttime.Note:thisEnglishversion,atranslation9Determinationofclenbuterol,ractopamine,Thestandardspecifiesthemethodsofsampleprepafationanddeterminationofclenbuterol,racto-pamine,salbutamolandterbutalinresiduesinfoodstuffsofanimaloriginbyHPLC-MS/MSThisstandardisapplicabletothedeterminationofclenbuterol,ractopamine,salbutamolandterbutalinresiduesinmeatandvisceraofanimaloringinbyHPLC-MS/MS.Thecombinedprimarysampleisreducedto500gwhichistocourseofsamplingandsamplepreparation,precautionshouldbetakentoavoidcontaminationoranyfactorthatmaycausesthechangeofresiduecontent.Thetestsampleshouldbestoredat-18℃.Clenbuterol,ractopamine,salbutamolandterbutalinresiduesareextractedfromthetestsamplewithpH5.2ammoniumacetatebuffersfollowedbyhydrolysiswithglucosidase.TheextractiscleanedupbySCXandCisolidphasecolumn.FourresiduesaredeterminedbyHPLC-MS/MS, isotopeinternalstandardmethod.Unlessotherwisespecified,allthereagentusedshouldbeanalyticalgrade,waterisdeionizedwater.4.1Methanol.4.2Acetonitrile:HPLCgrade.4.3Ammoniumacetate.4.4Aceticether.4.5Ammoniumhydroxide.4.6Hydrochloricacid.4.8Aceticacid.4.9β-glucuronidase:100U/mL.4.10Ammoniumacetatebuffer:0.02mol/L,pH=5.2.Weigh1.54gAmmoniumAcetatein900mLwater,adjustpHto5.2±0.1withaceticacidandaddwatertofinalvolumeof1L.4.11Aceticether-ammoniumhydroxidesolution(97+3,V/V).Mixtohomogeneousphasebeforeuse.4.13Clenbuterol(Ci?H??Cl?N?OCAS:37148-27-9),ractopamine(CigHz?NO?CAS:97825-25-7),salbu-tamol(C?H??NO?CAS:18559-94-9)andterbutalin(Ci?H??NO?,CAS:23031-25-6),D?-Clenbuterol,D?-ractopamine,D?-Salbutamolstandards:purity>98%.4.14Stockstandardsolutionofclenbuterol,ractopamine,salbutamol,terbutalin(1.0mg/mL):ac-curatelyweigh50mg(±0.1mg)standardinvolumicflask,addtothebottlesaknownamountofwatertoproduceasolutioncontainingcompoundsallat1.0mg/mLandstoassignashelflifeof12months.4.15StockinternalstandardssolutionofDg-clenbuterol,Ds-ractopamine,D?-salbutamol(1.0mg/mL):accuratelyweigh50mg(±0.1mg)standardinvolumicflask,addtothebottlesaknownamountofwatertoproduceasolutioncontainingcompoundsallat1.0mg/mLandat<5℃,assignashelflifeof12months.4.16Mixtureintermediatestandardsolution:dilutestockstandardsolutionofclenbuterol,racto-pamine,salbutamol,terbutalin(1.0mg/mL)to1.0μg/mLand100.0ng/mLinmethanol,storerefrig-eratedat<5℃,assignashelflifeof6months.4.17Mixtureintermediateinternalstandardsolution:dilutestockstandardsolutionofDg-clen-buterol,D?-ractopamine,D?-salbutamol(1.0mg/mL)to100.0ng/mLinmethanol,storerefrigeratedat<5℃,assignashelflifeof6months.4.18Workingstandardsolutions:Torequireasuseful,dilutethemixtureintermediatestandardso-lutions(4.16)andmixtureintermediateinternalstandardsolutions(4.17)withwaterfreshly(Thereferencecalibrationregionis0.5ng/mL~10ng/mL).Andtheconcentraperworkingstandardsolutionis1.0ng/mLandstoreref4.19SCXcolumns:LC-SCXSepPak,500mg,3mLorequivalent.4.20Ccolumns:LC-18,500mg,3mLorequivalent.4.210.45μmhydrophilicfilm.5.1Liquidchromatograhycombinedwithelectrosprayionizationmassspectrometry.5.2Vortexmixer.5.3Centrifuger:4000r/min,andequippedwith250mLpolyethyleneorpolypropylenebottles.5.4Rotaryvacuumevaporator.5.5Balances(0.1mg,0.01g5.6Ultrasonicapparatus.5.8ApparatusofSPE.5.9Nitrogenevaporator.5.10Pulverizer.Weigh10(0.1g)samplein50mLplasticcentrifugetubes,add20mLpH5.2ammoniumacetatebuffer(4.10)and20.0nginternalstandardofD?-clenbuterol,Ds-ractopamine,D?-Salbutamol50μLandβ-glucuronidaserespectivelytosamplematrixandvibratefor15minfollowedbyhydrolysisfor16hat37℃.Thetubesiscentrifugedat3800r/minfor10min.Tra0.45μmfilm(4.21)toget5mLsamplesolutionforSPEcleanup.Load5mLfilteredsolutiontoCig(4.19)andSCX(4.20)SPEcartridge(CisandSCXcolumnswereattheflowrateof1.0mL/min).Then,thecolumnwasrinsedwith5mLwaterand5mLmethanolandremovetheCgSPEcolumn.Afterpurgethecartridgesatvacuum,elutewith12mLaceammoniumhydroxide.(4.11),Theeluateswasconcentratedtonearlydrynessbygentlenitrogenandadded1mLacetonitrile/water(1+9)toresolvetherea)Column:C,5μm,150mm×4.6mm(i.d),ortheequivalent.b)Mobilephase:A:Acetonitrile+0.1%formicacid,B:2mmol/LAmmoniumacetatesolution+0.1%formicacid.Flowrate:200μL/min.Gradientprogramislistedastable1.Time/minRatio/(%)MobilephaseAMobilephaseB0578c)Columntemperature:35℃.d)Injectionvolume:30μL.6.3.2Massspectralacquisitionb)Monitormode:multiplereactionmonitoring,MRM;c)Nebulizergas(GS1),curtaingas(CUR),auxiliaryheatergas(GS2)andcollisiongasarehighpuritynitrogenorequivalent,optimizetheflowrateofeachgasandionsourcetemperaturetoreachtherequirementofthesensitivityofmassspectrometry.DetailedparametersarelistedasannexA;d)Collisionenergy(CE),deculsteringpotential(DP),collisioncellexitPotential(CXP),collisioncellentrancepotential(EP)andelectrospraycapillaryvoltage(IS)shouldbeoptimizedtothebestsensitivity.RelatedparametersandqualifierandquantifierMRMarelistedasannexA.6.3.3QuantitationofLC-MSAccordingtotheHPLC-MS/MSoperatingconditionabove,determinethesamplesolutionandthestandardworkingsolution(4.16)simultaneously.Theresponsesoftheanalyteinthestandardwork-ingsolutionandthesamplesolutionshouldbothbewithinthelinearrangeoftheinstrumentdetec-tion.Quantifiedbyinternalstandard.UndertheaboveHPLC-MS/MSoperatingcondition,theretentiontimeofsalbutamolisabout3.0min,terbutalinisabout3.1min,ractopamineisabout9.4min,andclenbuterolisabout9.9minrespectively.SelectedionchromatogramsofthestandardsseeFigure6.3.4ConfirmationofLC-MS/MSDeterminatedundertheestablishedLC/MS-MSconditions,andcalculatedtheintensityratiooftwoselectedionpairsofthesamplesolutionandthestandardworkingsolution.Iftheretentiontimesofsamplechromatogrampeaksareconsistentwiththatofworkingsolution,Andtherelativeabundanceratiotoleranceissameaslisted(table2)itissafetoconcludethatthiscompounddoexitinthesample.Theoperationoftheblanktestisthesameasthedescribedinthemethodofdetermination,butwithoutadditionthesample.Calculationthecontentofclenbuterol,ractopamine,salbutamolandterbutalinresidueinthetestsam-plebyHPLC-MS/MSdataprocessororaccordingtotheformula(1).Theblankvalueshouldbesub-SN/T1924—2007tractedfromtheaboveresultofcalculation.……………whereX—theresiduecontentofβ-agonistinthetestsample,mg/kg;c—theconcentrationofβ-agonistinstandardworkingsolution,ng/mL;c,—theconcentrationofinternalstandardinsamplesolution,ng/mL;A—thepeakareaofβ-agonistinsamplesolAsi—thepeakareaofinternalstandardinstandardworkingsolution;V—thefinalvolumeofthesamplesolution,mL;cs?—theconcentrationofinternalstandardinstandardworkingsolution,ng/mL;A,—thepeakareaofinternalstandardinsamplesolution;A?—thepeakareaofβ-agonistinstandardworkingsolution;m—massoftestsampleoffinalsamplesolution,g.(Annotation:Allβ-agonistemploythecorrespondingisotopeastheinternalstandardrespectivelyexceptthatterbutalinusesD?-salbutamolastheinternalstandard)8.1Limitofquantification(LOQ)Thelimitofdeterminationofthemethodforliverandmeatis0.0008.2.1Accordingtotheexperimentaldata,thefortifiedconcentrationofclenbuterol,ractopamine,salbutamolandterbutalininmeatanditscorrespondingrecoveryareshowedinTable3.8.2.2Accordingtotheexperimentaldata,thefortifiedconcentrationofclenbuterol,ractopamine,salbutamolandterbutalininliveritscorrespondingrecoveryareshowedinTable4.ChemicalsConcentration/ChemicalsConcentration/ClenbuterolRactopamineTerbutalinMainMassParametersa)Electrospraycapillaryvoltage:5500V;e)lonsourcetempeture:550℃;f)QualifierandQuantifierMRM,CollisionEnergy(CE),DeclusteringPotential(DP)areshowedinTableA.1.CollisionCellExitPotential(CXP)andCollisionCellEntrancepotential(EP)are10Vand13Vrespectively.D?-clenbuterolD?-ractopamineD?-salbutamol1)theequipm