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24中英文双语高效压液相色谱外文文献翻译基于共价有机框架的磁性吸附剂的多环芳烃固相萃取及其HPLC

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外文标题：

Acovalentorganicframework-basedmagneticsorbentforsolidphaseextractionofpolycyclicaromatichydrocarbons,andanditshyphenationtoHPLCforquantitation

外文作者：

RongWang,ZilinChen

文献出处:

《MicrochimicaActa》,2017（5751）:

1-8（如觉得年份太老，可改为近2年，毕竟很多毕业生都这样做）

英文4589单词，24889字符（字符就是印刷符），中文7792汉字。

Abstract

Anovelcovalentorganicframeworkbasedmag-neticadsorbentwasdevelopedformagneticsolidphaseex-traction（MSPE）ofpolycyclicaromatichydrocarbons（PAHs）.Covalentorganicframework-LZU1（=LanZhouUniversity-1）wascovalentlyimmobilizedontopolyethyleneimine-functionalizedmagneticnanoparticles（COF-LZU1@PEI@Fe3O4）,andtheresultingmaterialwascharacterizedbytransmissionelectronmicroscopyandFouriertransforminfraredspectroscopy.TheeffectsofthepHvalueofsamplesolution,percentageofacetonitrile,ex-tractiontimeandsamplingvolumeonMSPEofsixPAHswereinvestigated.TheCOF-LZU1@PEI@Fe3O4displayshighextractionefficiencyforthePAHssuchaspyrene,benzo[a]pyrene,fluoranthene,benz[a]anthracene,benzo[a]fluoratheneanddibenz[a,h]anthracene.Followingdesorptionwithacetonitrile,thePAHswerequantifiedbyHPLC.TheMSPE-HPLCmethodshowslowlimitofdetec-tion（0.2–20pgmL−1）,widelinearrangeandgoodreproduc-ibility（relativestandarddeviations<4.4%forintra-dayandinter-dayprecision）.ThemethodwassuccessfullyappliedtodeterminePAHsinenvironmentalsamples.Goodrecoverieswereobtained,rangingfrom90.9to107.8%forwatersamplesand85.1to105.0%forsoilsamples.

KeywordsCovalentorganicframework.COF-LZU1.Magneticsolidphaseextraction.Environmentalanalysis.Traceanalysis.HPLC

Introduction

Covalentorganicframeworks（COFs）areaclassofcrystallineporousmaterialsthatconsistoflightelements（C,H,B,N,Oetc.）andareconnectedthroughstrongcovalentbonds[1–7].Thesematerialspossessmuchfascinatingpropertiesincludinghighspecificsurfacearea,excellentthermalstability,highporosity,andlowdensity.Withtheseuniqueproperties,COFshavearousedintensiveinterestofscientistsforthegreat

potentialapplicationindiverseareas[2,4],suchasgasstorage[8–10],gasadsorption[11,12],photoelectricity[13,14],ca-talysis[15,16]andchromatographicseparation[17–19].However,therearestillfewreportsfocusingontheirperfor-manceinthefieldofsamplepretreatment.Metal–organic

frameworks（MOFs）areanothernovelclassofporousmate-rialssimilartoCOFs,whichhaveshowntobepromisingmaterialsassorbentsforsamplepreparationinmanypioneerworks[20–24].AstheanaloguesofMOFs,COFsshouldpossessgreatapplicationpotentialinsamplepreparation.

Hydrazonecovalentorganicframeworkshavebeensynthe-sizedandappliedtothesolid-phasemicroextraction（SPME）ofpyrethroids[25]andpesticides[26]invegetables.Therefore,itispossibletodeveloptheapplicationofCOFsaspromisingadsorbentinsamplepretreatment.

SincethefirstdiscoveryofCOFmaterialsin2005[1],avarietyofCOFshavebeenreported.Imine-linkedCOF-LZU1（LanZhouUniversity-1）wasfirstdesignedandsynthesizedbyWang’groupin2011[15],whichwasconstructedwith1,3,5-triformylbenzeneand1,4-diaminobenzenethroughSchiffbasereaction.COF-LZU1hasatwo-dimensional（2D）layered-sheetstructureandpossesseslargenumberofbenzeneringsandiminegroups.Unlikeboron-containingCOFsthatlinkedbyboroxineorboronate-estergroups,COF-LZU1ishighlystableinwaterandmostorganicsol-vents[15].Niuetal.exploreditsperformanceasthestationaryphaseofcapillaryelectrochromatographyforseparatingor-ganicmolecules[19].TheresultsindicatedthatCOF-LZU1canofferstrongπstackinginteractionandhydrophobiceffectwiththeanalytes.Thissuggeststhatitmaybeanexcellentenrichmentmediaforcompoundswithabundantπsystem.

Samplepreparationisacriticalsteppriortoanalysis,espe-ciallywhencomplexsamplesarepresent.Overthepastfewdecades,manynewsamplepretreatmenttechniqueswithlowsolventconsumptionandlowsamplehandlinghavebeende-velopedandappliedtoextracttargetcompoundsfromdifferentmatrices[27,28].Amongthesetechniques,magneticsolid-phaseextraction（MSPE）hasattractedincreasingatten-tionduetoitslargeadsorptioncapacityandhighextractionefficiency[29].Additionally,magneticnanoparticles（MNPs）canberapidlyseparatedfromsamplematrixviaanexternalmagnet,whichwouldsimplifyoperationprocedureandshort-enanalysistime.ConsideringofthefeaturesofCOF-LZU1andMSPE,weattemptedtoprepareaCOF-LZU1functionalizedMNPsandapplytomagneticsolid-phaseextraction.InordertoachievetheimmobilizationofCOF-LZU1,polyethyleneimine-functionalizedFe3O4nanoparticles（PEI@Fe3O4）[30]werechosenasthemagneticsupport.WiththenumerousactiveaminogroupsinthestructureofPEI,COF-LZU1canbecovalentlybondedtothesurfaceofPEI@Fe3O4throughSchiffbasereaction.

Polycyclicaromatichydrocarbons（PAHs）arewell-knownenvironmentpollutants,whichareconsideredtobecarcino-genicandmutagenictohumanbeings.Itisofgreatimpor-tancetomonitorandcontroltheamountofPAHsinenvironment.SincetheconcentrationofPAHsinenvironmentalsamplesisusuallyintracelevels,itisnecessarytoenrichPAHsbyefficientsamplepretreatmentmethodbeforeinstrumentalanalysis[31–34].ConsideringthepropertiesofCOF-LZU1andPAHs,COF-LZU1basedMSPEmethodwasexpectedtoexhibithighextractionefficiencyandcapacityforanalysisofPAHsinenvironment.

Herein,inthiswork,wereportedthefabricationofanovelCOF-LZU1functionalizedMNPs（COF-LZU1@PEI@Fe3O4）anditsapplicationfortheMSPEofPAHs.Fe3O4nanoparticleswerefirstcoatedwithPEI,thenCOF-LZU1wasgrownonthesurfaceofMNPsattributingtothecovalentbondingbetweenthePEIlayerandCOF-LZU1.Themorphologyandsurfacepropertiesofnanoparticleswerecharacterizedbytransmissionelectronmicroscopy（TEM）andFourier-transformedinfraredspectroscopy（FT-IR）.COF-LZU1@PEI@Fe3O4wereusedasmagneticadsorbentforextractionofPAHsfromenvironmentalsamples.Theextractionperformancewassystematicallyinvestigated.Tothebestofourknowledge,itisthefirsttimethatCOF-LZU1isimmobilizedonsolidsupportforsamplepreparation.

Experimental

Chemicalsandmaterials

1,3,5-Triformylbenzene,1,4-diaminobenzene,pyrene（PYR）,benzo[a]pyrene（B[a]PY）,phenanthrene,anthracene,naph-thalene,1-naphtholwerepurchasedfromSigma–Aldrich（MO,USA,www.sigma-）.Fluoranthene（FLU）,benz[a]anthracene（B[a]AN）,benzo[a]fluorathene（B[a]FL）,dibenz[a,h]anthracene（D[a,h]AN）wereobtainedfromTCI（Shanghai,China,）.4-Phenylphenol,4-vinylbiphenyland1,4-dioxane,polyethyleneimine（PEI,Mw70,000gmol−1,50%（w/v）aqueoussolution）wereboughtfromAladdinReagent（Shanghai,China,www.aladdin-）.MethanolandacetonitrilewereHPLCgrade（Tedia,OH,USA,）.Otherreagentswereanalyticalgrade.PurifiedwaterwasobtainedfromaMilli-Qsystem（MA,USA,US/en）.

Instrumentation

ThechromatographicanalysiswasperformedbyaShimadzu20AHPLCsystem（Tokyo,Japan,.cn）,whichequippedwithtwo20Apumps,asix-portvalve,a20AUVdetector,anda10Afluorescentdetector.ThechromatographicseparationwascarriedoutbyaC18column（150mm×4.6mmi.d.,5μmparticlesize,GLScience,Tokyo,Japan,www.shimadzu-）.Themobilephase

consistedofmethanolandwater（89/11,v/v）andtheflowratewas1.0mlmin−1.Thedetectionwavelengthoffluorescentdetectorwassetat290nm（exitingwavelength）and430nm（emissionwavelength）,whilethedetectionwavelengthofUVdetectorwassetat254nm.ThecolumntemperatureforHPLCseparationwassetat30°C.

Fourier-transformedinfraredspectroscopy（FT-IR）charac-terizationwasperformedonThermoNexus470FT-IRsystem（MA,UAS,）.Thetransmissionelectronmicroscopy（TEM）imagewasobtainedbyaJEM-2100（HR）transmissionelectronmicroscope（TEM）（JEOL,Tokyo,Japan,https:

//www.jeol.co.jp/en/）.

PreparationofCOF-LZU1@PEI@Fe3O4

PEI@Fe3O4waspreparedfollowingAmal’smethod[30].Briefly,FeCl2∙4H2O（0.7g）wasfirstlydissolvedin80mLofdistilledwater.Then10mLofKNO3（2.0M）,10mLofNaOH（1.0M）andPEI（1.7g）wereaddedtothissolutionsequentiallyundernitrogenatmosphere.Afterbeingstirredfor2hat90°C,thesynthesizednanoparticleswerecollectedbyamagnet,followedbywashingwithwaterforseveraltimes.

1,3,5-Triformylbenzene（3mg）,1,4-diaminobenzene（3mg）weredissolvedin3mLof1,4-dioxaneandfollowedbytheadditionof60μLof3Maqueousaceticacid.PEI@Fe3O4（100mg）weresuspendedinabovesolutionwithultrasonication.FormodificationofCOF-LZU1,thetemper-aturewasroseto150°Candreactedfor24h.Finally,theCOF-LZU1@PEI@Fe3O4werewashedwithethanolthor-oughlyanddriedintheoven（60°C）.

COF-LZU1@PEI@Fe3O4basedMSPEprocedures

PAHsstandardweredissolvedin20mMphosphatebuffer（pH9,containing1%acetonitrile,v/v）atcertainconcentra-tion.COF-LZU1@PEI@Fe3O4（5mg）werecarefullyweighedandmixedwith20mLofsamplesolution.Themix-turewasstirringfor30minwiththeassistantofamagneticstirringapparatus（twobottlescontainingthemixtureandstirringbarwereplacedtogetherandstirring）.Beforecollectionofnanoparticles,thestirringbarwasremovedbyamagnetunderstirring.Afterthat,thenanoparticleswereseparatedfromthesolutionbyanextern