液相色谱_质谱联用技术在检测食品中兽药残留的应用

2007,15(2):34240ChineseJournalofVeterinaryParasitology:2005211209:(1981),,:[e-mail]21,2,2,3,1,1(1.,200232;2.,201103;3.,200031):2(LC2MS):2;;;;:S859.79:A:100520868(2007)0220034206THEAPPLICATIONSOFLIQUIDCHROMATOGRAPHY2MASSSPECTROMETRY(LC2MS)INTHEDETERMINATIONOFDRUGRESIDUEINANIMALFOODYANFeng,HUANGShi2xin,YUKun,XUMei2qian,HEGuo2sheng(1.ShanghaiVeterinaryResearchInstituteCAAS,Shanghai200232,China;2.ShanghaiSnpervisoryStationofAnimalDrngsandFeed,Shanghai201103,China;3.XuhuiDistrictCentralhospital,Shanghai200031,China)Abstract:Thesecurityofanimalfoodhasbeenaglobalproblem.Theproblemsofthedrugresidueinani2malfoodandthepoorsecurityareveryobvious.Sotofindamethodwhichcanprecisely,sensitivelyandcrediblyanalyzethedrugsinanimalfoodisveryimportant.TheapplicationsofLiquidChromatography2MassSpectrometry(LC2MS)inthesecuritydeterminationandanalysisofanimalfoodwereintroducedinthepaper.Keywords:LiquidChromatography2MassSpectrometry(LC2MS);animalfood;drugs;residue;determi2nation,,,:(BSE)(FMD)(AI),,,,1,:,,,,,(FIA)(RIA)(ELISA)(FIIA)(ELISA),ng/mLpg/mL,ELISA,,,,,,,()()(),,,,()(22)(LC2MS)LC/MS:(TSP)(PB)(ESI)(APCI)LC2MS,,2(LC/US)22222:(Clenbuterol)(Salbutamol)(Cimaterol)(Mabutaline)(Ractopamin)(Carbuterol)(Turbutaline),,,22,2,,22,10:,,,():,,;,,GC/US,,,,,,,2:277.0/203.1,240.1/148.2PinnacleC18(2.1mm150mm,5m,Restek),0.05%5%-0.05%(5050,V/V);:200L/min;:10L,0.05ng/g0.2ng/g,0.150.6ng/g,103,,1.5ng/g70%,(RSD)9%,0.999[1]53152:2ESI/MS/MS2,m/z2772592032mg/L100mg/L;0.75mg/L;95%98%[2]ESI(SIR)(M/Z):203,259,277:WatersC18,150mm2.1mmI.D.,5m0.1%2(9010):20L;:0.2mL/min0.0010.01mg/kg,71.2%98.6%0.001mg/kg[3](MS/HS)(MRM),,m/z277259,C18,Inertsil5ODS22(2.1mm50mm,5m,MetaChemTechnole2gieslnc.),300L/min,20L243nm:Y=4336.07X(r=0.99985),0.14g/L60.0g/L90%;0.07g/kg[4]FesserAC2(LC2APCI2MS),22,2,OasisHLB23%76%,34%76%[5]3(sulfonamides,SAs),:(SM2)(SMM)22,62SAs,,0.3mg/kg,0.1mg/kg,252(HPLC)2(GC2MS)(CE)(TLC)HPLCCE,,,,GC2MS,TLC,(ESI2MSn):Hypser2silC18,25cm4.6mm,5m;0.2%=8884,:1.0mL/min,:263nmm/z289,(MRM),m/z203,m/z156:2.540.0g/L,0.99957,76.5%88.3%,5g/L[6]17213C62,:CAP2CELLPAKC8DD(150mm210mm,5m);:20,:4;:10LA0.2%,B0.2%;ESI+0.021g/kg,1752.3%124.9%,1.0%17.6%[7]44.1,,32222(32amino222oxazolidinone,AOZ)1995,2002,,,6320073,,4AOZAMOZSEMAHDHPLC2MS,2222:IntersilODS,150mm4.6mm,5m(GLScienceJapan);-0.1%,:0.6mL/min,:30L:API2ES(SIM),22AOZAMOZSEMAHD:m/z225227;m/z324326;m/z198200;m/z23824022AOZAMOZSEMAHD:m/z335m/z236m/z209m/z24985%90%;0.5g/kg[8],(ESI+)(MRU)A,B0.1%(0.5mmol/L),;0.2mL/min,30489.5%110.3%(3S/N)AMOZAOZ0.05g/kg,SEMAHD0.1g/kg,[9](LC/MSn)4F,:ZORBAX80AExtendC18150mm2.1mm,5m(Agilent):(B)(A),:20L;:0.2mL/min(ESI+),64%79%,(LOQ)0.11g/kg,(LOD)0.050.5g/kg[10]PPMulder2(LC2MS/HS)3,52(3,52dinitrosalicylicacidhydrazide,DSH)NPDSHNPHBH,,NPDSHNPHBH[M2H]m/z374,NPD2SHm/z182226,NPHBHm/z1830.04mg/kg,0.025mg/kg,0.10mg/kg,0.05mg/kg[11]4.2(Quinolones,QNs)1,4224223,42232,DNA(Fluoroquinolo2ne,FQs)(Noffloxacin,)(Pefloxacin,)(Enoxacin,)(Oflox2acin,)(Ciprofloxacin,),(Enrofloxacin)(DanofloxacinMesylate)(Marbo2floxacin)(SoraflaxacinHydrochlo2ride)(Orbifloxacin)(Di2floxacinHydrochloxride),,,LC2MS,,,FQs()7(PQs)LC2ESI2MS/US7:NORCIPENROOFLDANODIFSARA:LichroCART(r),Pu2rospher(r)STARRP218e,1252mm,5m;:(A)0.1%(B),:0.2mL/min;:30;:10L::(HRM),71.0ng/mL200ng/mL(LOD)0.52.9g/kg,(LOQ):9.6(NOR)6,8(CIP)1.8(ENRO)2.8(OFL)8.2(DANO)5.4(SARA)2.4(DIF)g/kg,,(HRL)[12]HatanoK/(LC273152:2ESI2MS/MS)(SRM),7()0.2%,5mmol/LIPCC2MS3,5mmol/LIPCC2MS2ODS60%,2ng/g,1ng/g[13]4.3(Chloramphenicol,CAP),,2002,,,,,GClCLC/MSGC/US(RIA),RIA(ELISA),1g/kgELISAGC/ECD()CAP,0.15g/kg,CAP,,HPLC/UVD,UVD,,HPLC/UVDGC,510g/kg,,LC/MS,,MasahikoTakino2(LC2APPI2MS),ZorbaxEclipseXDBC181503mm,5m,10mmol/L2;:,0.05mL/min;;:40;:20l;:0.5mL/min(SIM):m/z321[M2H]-0.12ng/g,89.3%102.5%87.4694.8%LOD0.07ng/ml(=3)0.27ng/g0.10ng/g[14](ESI),,m/z:321/152C18Inertsil5ODS22(5m,2.1mm50mm,MetaChemTechnolegiesInc.);,300L/min,20L0.2828g/L,r=0.999910.07g/kg[15]/(Q2Trap):InertsilODS23(2.1mm15cm,5m):0.01mol/L,0.5mL/min,5L;40;278nmMS:(2)API2ES,,m/z321MS20.120g/L0.99953;201000g/L0.99803,70%116%[16]m/z321.0,m/z152.1257.0194.1,(HRM):BDSC18,2.1150mm,3.5m;:30L;:30;:300L/min;:2(V/V1090),0.010g/kg(S/N3),0.10g/kg,0.1001.00g/L,74.3%84.0%[17],2:XDBC18(150mm2.1mmi.d.,3.5m);:30L;:30;:2,:300L/min,(MRU),m/z152.1257.0,m/z185.1290.1,m/z185.1336.1,m/z321.0/152.1,354.0/185.1356.1/336.183200730.010g/kg,0.100g/kg,0.0501.00ug/L,69.0%92.8%[18]4.422:,2GGDMHolstege225p(GV)2()/(1%)[M+H]+,GV[M+Na]+FDA5ng/ml2.5ng/mL(=10)0.2ng/mL(),0.4ng/mL(),0.8ng/mL(),1ng/mL(G),2ng/mL(V)[19]CKFagerquist(spersive2SPE)2,,102:DCCDGDCCD58%,70%[20]5LC2MS,,,:[1],,,.HPLC/MS2[J].,2004(04).[2],,,.2[J].,2004(06).[3],,,.2[J].,2005(1):3638.[4],.[J].,2005,26(1):187.[5]FesserAC,DicksonLC,MacNeilJD,etal.Determina2tionofbeta2agonistsinliverandretinabyliquidchroma2tography2tandemmassspectrometry[J].JAOACInt,2005,88(1):6169.[6],,,.[J].,2004(02).[7],,,.217[J].,2005(04).[8],,,.2[J].,2005,33(5):707710.[9],,,.2[J].,2003,13(6):2328.[10],,,.2[J].,2005,37(3):1215.[11]PPMulder,TZuidema,NGKeestra,etal.Determina2tionofnifursolmetabolitesinpoultrymuscleandliver