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1、7Solid-PhaseMicroextractionMethodDevelopmentaabLucieKudlejova,SanjaRisticevicandDajanaVuckovicaDepartmentofChemistry,UniversityofWaterloo,Waterloo,Ontario,CanadabDonnellyCentreforCellularandBiomolecularResearch,UniversityofToronto,Toronto,Ontario,Canada7.1IntroductionThisch
2、apterdescribestheanalyticalmethodsusedfortheisolationofanalytesofinterestfromvarioustypesofmatrices,withaspecialemphasisonsolid-phasemicroextraction(SPME)technique.Theoptimizationandvalidationstepsrequiredforthedevelopmentofvariousapplicationsaredescribedandthoroughlydiscus
3、sed.Thesamplingandsamplepreparationstepisoneofthemostimportantandfre-quentlythemosttime-andlabour-consumingstepsintheentireanalyticalmethod.Obtainingarepresentativesampleisabasicprerequisiteforobjectiveanalysis.Foragoodsubsequentextraction,solidsamplestypicallyneedtobeprope
4、rlyhomoge-nised,whichoftenrequireseitherdryingthesampleinanovenorblendingitwithwater,iceordesiccant(e.g.Na2SO4),dependingonthetypeofapplication.Theisolationofthetargetanalytesfromsamples(sampleextraction)isthenextstepoftheanalyticalmethod,andcarefulselectionofanappropriatee
5、xtractionmethodatthebeginningoftheanalysisisveryimportantforobtainingreliableanalyticaldatainareasonabletime.Consideringthatfastseparationanddetectionsystemsaremoreandmoreavailableinanalyticallaboratories,theisolationofthetargetanalytesoftenbecomesthetime-limitingstepofthew
6、holeprocedure.Solventextraction(liquidliquidextraction,LLE,orliquid-phasemicroextrac-153,4,69tion,LPME),supercriticalfluidextraction(SFE),solid-phaseextraction13,6,7,9(SPE)performedinthecolumn,cartridge,discormicrowellplateformat,33,4,10,11stir-barsorptiveextraction(SBS
7、E),ultrasonicextraction(USE),Soxhlet3,4,124,1314extraction(SOX),steam/solventorvacuumdistillation,cryo-extraction,pressurisedliquidextraction(PLE),suchasacceleratedsolventextraction3,4,9,10,123,4,7,911(ASE)andmicrowave-assistedextraction(MAE)arethemostcommonlyusedandwell-e
8、stablishedextractiontechniquesdescribedorreviewedintherespectivecitedpublications.