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Ionic

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IonicIonic,ionic,IONIC

    Ionic

Availableonlineatwww.sciencedirect.com

    ;?

    ;:,ScienceDirect

    ;ChineseChemicalLetters19(2008)985-987

    ;CHINE5E

    ;CHEMICAL

    ;LETTER5

    ;www.elsevier.com/locate/cclet

    ;Ionicliquidbaseddispersiveliquid-liquidmicroextractionOf

    ;aromaticalYllnesinwatersamples

    ;YunChangFan,ZhengLiangHub,

    ;MeiLanChencChaoShenTucYanZhu’

    ;DepartmentofChemisXixiCampus,ZhefiangUniversity,Hangzhou310028,China ;.TheZhej~angUniversityNationalSciencePark,Hangzhou310013,China ;BiologyandEnvironmentEngineeringCollegeofZhejiangShurenUniversity,Hangzhou310015,China

    ;Received7March20O8

    ;Inthiswork.anowmicroextractionmetllodtermedionicliquidbaseddispersive1iquid-1iquidmicroextraction(IL.DI,I)

    ;wasdemonstratedfortheextractionof2.methylaniline.4.chloroaniline.1-naphthylarnineand4.aminobiphenylinaqueous

    ;matrices.Afterextractiontlleionicliquid(IL)phasewasinjecteddirectlyintothehighperformanceliquidchromatography(HPLC)

    ;systemfordetermination.Someparameterstllatmightaffecttheextractionefficiencywereoptimized.Undertlleoptimum

    ;conditions,goodlinearrelationship,sensitivityandreproducibilitywereobtained.Thelimitsofdemction(LOD,S/N=3)forthe

    ;fouranalyteswereintherangeof0.45_2.6gL

    .Therelativestandarddeviations(R.S.D.,n=6)wereintherangeof6.2.-9.8%. ;T}lismethodwasappliedfortheanalysisoftllerealwatersamples.Therecoveriesrangedfrom93.4to106.4%.Themain

    ;advantagesofthemethodarehighspeed,highrecovery,goodrepeatabilityandvolatileorganicsolvent.free.

    ;?

    20o8YanZhu.PublishedbyElsevierB.VonbehalfofChineseChemicalSociety.lrightsreserved.

    ;Keywords:IonicHquid(m);Dispersiveliquid-liquidmicroextracfion(DLLME);Highperformanceliquidchromatography(HPLC);Aromatic

    ;amines

    ;Thedeterminationofaromaticaminesinenvironmentalwaterisveryimportantbecausetheyarewidelyusedin

    ;chemicalindustry

    1,2]andmanyofthemaresuspectedcarcinogenicandarehighlytoxictoaquaticlife3].High

    ;performanceliquidchromatography(I-IPLC)isoftenusedforthedeterminationofaromaticamines,andsample

    ;enrichmentisusuallyrequired.Inthepastextractiontechniquessuchasliquid_-uquidextra

    4],solidphase ction(LLE)

    ;extraction(SPE)57],microporousmembraneliquid_-uquidextraction

    8],solidphasemicroextraction(SPME)

    ;9,10]andliquid-liquid-liquidmicroextraction(LLLME)11,12]wereusedfortheextractionofaromaticamines.

    ;Oneofthemajordisadvantagesofthesemethodsistheneedofusingasubstantialamountofvolatileorganicsolvents.

    ;Therefore,severaleffortshavebeenreported,suchasionicliquidbasedheadspaceliquidphasemicroextraction(IL.

    ;HSLPME)13,14],coldinducedaggregationmicroextraction(CIAME)15]andtemperaturecontrolledionicliquid

    ;dispersiveliquidphasemicroextraction(TC?,DLME)

    16].However,boththesemethodsaretimeconsuming

    ;processes.

    ;Correspondingauthor.

    ;E-mailaddress:zhuyan@zju.edu.ca(YZhu)

    ;1001-8417/$seefrontmatter?

    2008YahZhu.PublishedbyElsevierB.VonbehalfofChineseChemicalSociety.Allfigh~reserved.

    ;doi:10.1016/j.cclet.2008.05.024

    ;

    ;

    ;YC.Faneta1./ChineseChemicalLetters19f2008)985-987

    ;Somerecentarticleshavereportedanewliquidphasemicroextractionmethod. ;dispersiveliquid.hquid

    ;microextraction(DLLME)whichisbasedontheuseofaternarycomponentsolventsystem.Rapidityandsimplicity

    ;ofoperationaresomeoftheadvantagesofthismeth0d17191.

    ;TheaimofthisstudyistoinvestigatethepotentialityofILinsamplepreconcentrationusingtheDLL]ME

    ;technique.UnliketheDLLMEtechniquedescribedinreferences,theIL.DLLM

    methoddemonstratedinthepresent

    ;work,isabinarycomponentsolventsystem(waterandIL,nodispersersolventwasused),notaternarycomponent

    ;solventsystem.Theeffectsofvariousexperimentalparametersontheextractionofaromaticamineswereinvestigated

;andoperatingconditionswerealsooptimized.

    ;1.Experimental

    ;TheprocedureforILDIfI

    wassimilartothatdescribedinNagarajuandHuangwork[19].Briefly,a1.8mL ;portionofsamplesolutionand50L0f1_butyl3

    methylimidazoliumhexafluorophosphate([Bmim][PF6])as

    ;extractionsolventwereplacedina2.2mLglasstesttubewithconicalbottom.1mLoftheabovemixturewas

    ;aspiratedintoa1mLsyringe(Agilent),thenthesyringeplungerwasdepressedrapidlytoinjectthecontentsintothe

    ;remainingsolution.TheaboveprocedurewasrepeatedtwiceinordertoentirelydisperseILintotheaqueousphase,

    ;thusinducingtheformationofacloudysolution.Themixturewassubsequentlycentrifugedfor2minat3000rpm.

    ;Accordingly,thedispersedfinedropletsofILweresedimentedtothebottomoftesttube.Thesedimentedextraction

    ;phasewascollectedusinga50Lmicrosyringe(Agilent)andinjectedintotheHPLCsystem. ;TheanalysisofaromaticamineswasperformedbyanAgilent1200system.AnAgilentEclipseXDB.C18column

    ;f4.6mln×150mm)andaVWDdetectorsettingat240nlrlwereusedfortheseparationofaromaticaminesextracted

    ;intheIL.

    ;ThemobilephasewasamixtureofacetonitrileandwaterdeSveredataflowrateof1.0mLmin.Thegradient

    ;programwasasfollows:keepingconstant30%acetonitrileduring0_1lmin.thenincreasingto55%acetonitrilein

    ;11-16millandkeepingconstantuntil21min.thereafterrestoredto30%in1minfollowedbya3minre.equilibration

    ;time.

    ;2.Resultanddiscussion

    ;Inthepresentwork,extractionconditionssuchasextractiontime,concentrationofNaC1,pHofaqueoussolution

    ;andvolumeofILwereoptimized.InIL.DLLM

    .extractiontimewasdefinedasanintervaltimebetweenthe

    ;formationofcloudysolutionandbeforecentrifugation.ExperimentsdemonstratedthattheextractionemciencykeDt

    ;constantforallthestudiedanalytesin_5min.furtherincreasingoftheextractiontimeresultedinthedecreasingof

    ;extractione

    ciency.Therefore.0minwasadoptedastheoptimalcondition.Acomparisonoftheextractiontimeof

    ;aromaticaminesfromwatersamplesusingIL.DLLM.SPMEandIL.HSLPM

    issummarizedin11ab1e1.

    ;OtheroptimalparameterswereasfoUows:concentrationofNaCl12%(w/v),pHofaqueou

ssolution7,ILvolume

    ;50.

    ;Undertheaboveselectedconditions,therepeatabilitywasstudiedbyperformingsixtimesusingaqueousstandard

    ;solutionwitll40gL

    9.8%. ofeachanalyteandtherelativestandarddeviations(R.S.D.)wereintherangeof6.2

    ;Excellentlinearrangeswerefoundintherangeof2200gL

    for4.chloroanilineand1-naphthylamine,5

    ;200gLfor2.methylanilineand10_200gL

    for4.aminobiphenylwithg0odcorrelationcoefficient()

    ;rangingfrom0.9985to0.9998.Theproposedprocedurehasadetectionlimitandenrichmentfactorof1.00gL.|l

    ;and45for2.methylaniline,and0.68gLand31for4.chloroaniline,and0.45gL

    and269for1.

    ;Table1

    ;ComparisonoftheproposedILDLLMEwithILHSLPMEandSPMEforextractionof

    aromaticaminesfromwatcIrsamples

    ;Centrifugingtime

    ;

    ;YC.Faneta1./ChineseChemicalLetters19I2oo8)985-987

    ;024681012141618

    ;Time(min)

    ;Fig.1.Atypicalchromatogramofthefouraromaticaminesafterextractionfrom100L

    workingsolution.Peaksidentifiedas:(1)2

    ;methylaniline,(2)4-chloroaniline,(3)1-naphthylamine,(4)4-aminobipheny1. ;naphthylamine,and2.60gL

    and84for4-aminobiphenyl,respectively.1hedetectionlimitsarecomparableto ;thosementionedinliteratures13,14].

    ;Totesttheapplicabilityandaccuracyoftheproposedmethodinrealsamples,suchastapwater,fiverwaterand

    ;wastewater,wereanalyzed,respectively.Beforeuse,allthewatersampleswerefilteredthrough0.45Ixmmicropore

    ;membranes.eresultsindicatedthatthecontentsofthefouraromaticaminesinthethreesampleswereundertheir

    ;detectionlimits.I’hespikedrecoveriesdeterminedbyspildngthesampleswith40gL

    ofaromaticamineswerein

    ;therangeof93.4-106.4%.AtypicalchromatogramisshowninFig.1.

    ;Acknowledgments

    ;ThisresearchwasfinanciallysupportedbytheNationalNaturalScienceFoundationofChina(Nos.20375035,

    ;20527005,20775070)andbyZhejiangProvincialNaturalScienceFoundationofChina(Nos.Z404105,Y507252).

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    ;m5O

    ;《昌.)uowqJ0呐《

    ;嘲删圳嘲

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