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纳升级高效液相色谱与电感耦合等离子体质谱联用在砷、汞形态分析(2)

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导读: 浙江大学硕士学位论文AbstractAbstractArsenicandmercurywidelyfromspeciestoarehumancarcinogens,andthetoxicityoft

浙江大学硕士学位论文AbstractAbstractArsenicandmercurywidelyfromspeciestoarehumancarcinogens,andthetoxicityofthemvariesspeciesinvolved.Hence,abetterunderstandingoftoxicmechanismofarsenicandmercuryissignificantlyimportant.However,biologicalexperimentsanditsspeciationanalysiscanleadtolimitedavailabilityofsample,andcollectionofsamplesintherangeof10-50nLisverycommoninthisfield.Nanohighperformanceresolutionliquidchromatography(NanoHPLC)showshighchromatographicandlowsolventconsumptionandisoftencoupledwithhighlysensitiveanddement-specificdetectors,amongwhichinductivelycoupledplasmamassspectrometry(ICP.MS)isnanoHPLConeofthebestchoicesforarsenicandmercuryspeciation.ThecouplingofisoftenproblematicduetoflowratewithICP.MSincompatibilities.HencethedevelopmentofdedicatednanoflownebulizersforsheathlesscouplingofICP-MSandnanoHPLCishighlydesirable.Theresearchwasbasedontheseaspects,includingtheprogressofarsenicandmercuryspeciationanalysisinthetracesamples,nanoHPLChyphenatedwithICP-MS,andnanoflownebulizersforinductivelycoupledplasmaspectrometries.TheresearchmainresearchpurposewastoachievethecouplingofnanoHPLCwithICP-MS,andtheworkwassummarizedasfollows:First.asimple.10W.costandsmall.dead.volumedemountablenanoflownebulizer(d-NN)wasfabricated,whichconsistedofanebulizerbody,asolutioncapillaryandanadapter.Thetipofthesolutioncapillaryofthenanonebulizerwasgroundwithgmthickand20gmsandpaperstoobtainathinindicatedthatthesimilartonebulizers.ornozzle(5i.d.).TheexperimentalresuRsperformancesbetteroftheproposednanoflownebulizerat500nL/minwereeventhanthoseobtainedwithd.CMNandothernanoflowThen,thedevelopednanonebulizerwasutilizedtoseparateasthesheathlessinterfacefornanoHPLC.ICP.MSarsenicspeciesonareversed—phasecapillarycolumnseparationofarsenicspeciesandananionexchangecapillarycolumn,respectively.The16f50nLsamples)wasachievedwithinminonahomemadereversed。phasecapillary2.0mmol/Ltetrabutylammoniumcolumnf150gmi.d.×450pmo.d.×15cm)withTV万方数据浙江大学硕士学位论文Abstracthydroxide(TBAH)aqueoussolution(pH6.58)asthemobilephase.Incomparisonwiththec11romatogrambythereversed—phasecapillarycolumn,moreeffectiveseparationandhighersensitivityoftheAs—analyteswereachievedonastronganionexchangec印illarycolumn(100gmi.d.×360gmo.d.×25cm),packedinthelaboratory,with10.0mmol/Lofsodiumtartrate-tartaficacidsolution(pH6.90)asthemobilephaseat620血|min.Last,theseparationofmercuryspecieswasperformedbyusageofthenanoflownebulizerforsheathlessinterfacingnanoHPLCwithICP-MS.Themercuryspecieswereseparatedwithin13minonareversed-phasecapillarycolumn(150gmi.d.×450gmo.d.×15cm)with10.0mmol/LofL-cysteinesolution(pH5.00)asthemobilephase.Theoriginalityinthisthesis:AlOW.costdemountablenanoflownebulizer(d-NN)wasfirstfabricated.Lowdeadvolume,ultra-lowself-aspiration,narroweraerosolsizedistributionandhigheranalytetransportefficiency(nearly100%)wereobtainedwiththeproposednebulizer.Furthermore,theICP.MSinstrumentcouldtoleratedirectintroductionof100%organicsolventsbyusingthedevelopednebulizeroperatingatnanoflowrates.Itwasutilizedtosheathl …… 此处隐藏:2045字,全部文档内容请下载后查看。喜欢就下载吧 ……

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