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1、JournalofChromatographyA,1081(2005)145155Residuedeterminationofglyphosate,glufosinateandaminomethylphosphonicacidinwaterandsoilsamplesbyliquidchromatographycoupledtoelectrospraytandemmassspectrometryMar´ıaIba´nez,OscarJ.Pozo,JuanV.Sancho,FranciscoJ.L´opez
2、,F´elixHern´andez´∗ResearchInstituteforPesticidesandWater,UniversityJaumeI,E-12071Castell´on,SpainReceived11February2005;receivedinrevisedform3May2005;accepted17May2005AbstractThispaperdescribesamethodforthesensitiveandselectivedeterminationofglyphosate,g
3、lufosinateandaminomethylphosphonicacid(AMPA)residuesinwaterandsoilsamples.Themethodinvolvesaderivatizationstepwith9-fluorenylmethylchloroformate(FMOC)inboratebufferanddetectionbasedonliquidchromatographycoupledtoelectrospraytandemmassspectrometry(LCESI-MS/
4、MS).Inthecaseofwatersamplesavolumeof10mLwasderivatizedandthen4.3mLofthederivatizedmixturewasdirectlyinjectedinanon-linesolidphaseextraction(SPE)LCMS/MSsystemusinganOASISHLBcartridgecolumnandaDiscoverychromatographiccolumn.Soilsampleswerefirstlyextractedwit
5、hpotassiumhydroxide.Afterthat,theaqueousextractwas10-folddilutedwithwaterand2mLwerederivatized.Then,50Lofthederivatized10-folddilutedextractwereinjectedintotheLCMS/MSsystemwithoutpre-concentrationintotheSPEcartridge.Themethodhasbeenvalidatedinbothgrounda
6、ndsurfacewaterbyrecoverystudieswithsamplesspikedat50and500ng/L,andalsoinsoilsamples,spikedat0.05and0.5mg/kg.Inwatersamples,themeanrecoveryvaluesrangedfrom89to106%forglyphosate(RSD<9%),from97to116%forAMPA(RSD<10%),andfrom72to88%inthecaseofglufosinate(RSD<1
7、2%).Regardingsoilsamples,themeanrecoveryvaluesrangedfrom90to92%forglyphosate(RSD<7%),from88to89%forAMPA(RSD<5%)andfrom83to86%forglufosinate(RSD<6%).Limitsofquantificationforallthethreecompoundswere50ng/Land0.05mg/kginwaterandsoil,respectively,withlimitsofd
8、etectionaslowas5ng/L,inwater,and5g/kg,insoil.TheuseoflabelledglyphosateasinternalstandardallowedimprovingtherecoveryandprecisionforglyphosateandAMPA,whileitwasnotefficientforglufosinate,thatwasquantifiedbyexternalsta
