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1、13Solid-PhaseMicroextractionProtocolsa,baDajanaVuckovic,SanjaRisticevicandJanuszaPawliszynaDepartmentofChemistry,UniversityofWaterloo,Waterloo,Ontario,CanadabDonnellyCentreforCellularandBiomolecularResearch,UniversityofToronto,Toronto,Ontario,Canada13.1ProtocolforAut
2、omatedHigh-ThroughputSPME-LCusingtheConcept96RoboticSamplePreparationStationThisprotocoldescribesageneralisedsamplepreparationprocedureusingauto-matedsolid-phasemicroextraction(SPME)orthin-filmmicroextraction(TFME)andtheConcept96roboticstation(PASTechnology)fortheext
3、ractionoftargetcompoundsfromacomplexbiofluid,tissuehomogenateoranyothercomplex1matrixofinterest.Moregenerally,thisprocedurecanalsobeappliedforthedevelopmentofanyhigh-throughputmethodfortheanalysisofnon-volatiletargetanalytesusingConcept96.Thissamplepreparationtechniq
4、ueisideallysuitedforhyphenationwithliquidchromatography(LC)duetothenon-volatilenatureoftheanalytes.Anydetectionsystemcanbeused,butmassspectrometric(MS)detectionisrecommendedbecauseofhighsensitivityandselectivity.ThedesignandmainfeaturesoftheConcept96stationaredescrib
5、edinSection5.2.2.Thin-filmgeometryprovidesenhancedsensitivityandextraction2rates,andthisdesignisusedinthecommercialdevice.Therefore,fortheremain-derofthisprotocol,thetechniquewillbereferredtoasTFME.ThemainstepsofanautomatedTFMEprocedureare:(i)preconditioning,(ii)extr
6、action,(iii)washand(iv)desorption,asshowninFigure13.1.Priortotheuseofthisprocedure,SPME/TFMEmethoddevelopmentshouldbecarriedoutaccordingtotheproce-duresdescribedinChapter7and/orthegeneralmethoddevelopmentprotocollaid3outbyRisticevicetal.Themainparametersthatshouldbeo
7、ptimisedforthisapplicationare:(i)typeofcoating,(ii)coatingconditioningprocedure,(iii)extrac-tiontime,(iv)desorptionsolventanddesorptiontimeand(v)fastwashprocedurestep.Dependingontheparticularapplication,theusermayalsowanttoperformsamplepHadjustment(incorporationofsuc
8、hstepisrecommendediftheanalyteisionisable)and/orevaporation/reconstitutionstepinordertoenhancesensitivity.Figure13.2summarisesthepa