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離子液體在色譜中的應(yīng)用第1頁(yè),課件共16頁(yè),創(chuàng)作于2023年2月高效液相色譜法包括正相高效液相色譜法和反相高效液相色譜法。正相高效液相色譜法中流動(dòng)相的極性小于固定相的極性,也就是以及性鍵合相為固定相(常以氨基、氰基鍵合相等作為固定相)。反相高效液相色譜法中流動(dòng)相的極性大于固定相的極性,也就是以非極性鍵合相為固定相(常以十八硅烷C18、辛烷C8、甲基C1、苯基等作為固定相)。

離子對(duì)試劑是由強(qiáng)親水離子形成,反作用于樣品分子中的中性離心子對(duì)。因此,可用于同時(shí)分離帶電分子和非帶電分子。一般適用所有色譜固定相,流動(dòng)相含水至少達(dá)10%,否則就有產(chǎn)生沉淀的危險(xiǎn)(特別是在使用乙腈的情況下)。當(dāng)使用長(zhǎng)鏈的離子對(duì)試劑時(shí),如十六烷基硫酸銨或十二烷基硫酸鈉,色譜柱將選用反相色譜柱。2第2頁(yè),課件共16頁(yè),創(chuàng)作于2023年2月

抗衡離子:在離子型聚合反應(yīng)中,存在于增長(zhǎng)鏈末端活性離子附近的相反電性離子。

洗脫與洗脫劑:在洗脫色譜操作中,流動(dòng)相攜帶待測(cè)組分在色譜柱內(nèi)向錢(qián)移動(dòng)并流出色譜柱的過(guò)程稱為洗脫。所用流動(dòng)相稱為洗脫劑。3第3頁(yè),課件共16頁(yè),創(chuàng)作于2023年2月2.反相高效液相色譜法中離子液體作為流動(dòng)相添加劑對(duì)兒茶酚胺保留值的影響3.離子交換色譜法和反相高效液相色譜法分析選定的離子液體陽(yáng)離子4.1-烷基3-甲基咪唑離子液體作為洗脫劑對(duì)液相色譜法分離麻黃素的影響1.反相液相色譜法測(cè)定選擇性室溫離子液體陽(yáng)離子5.離子液體雙水相體系,高效液相色譜法測(cè)定鴉片生物堿的樣品前處理過(guò)程4第4頁(yè),課件共16頁(yè),創(chuàng)作于2023年2月6.使用四氟硼酸咪唑離子液體抑制液相色譜分析中游離硅羥基的不利影響7.離子液體在液體色譜法中減少硅羥基的相互作用

8.基于離子液體的液相微萃取-高效液相色譜法測(cè)定水中有機(jī)磷農(nóng)藥9.液體作為高效液相色譜分析的添加劑:分析胺和離子液體的相互作用機(jī)制10.離子液體液液萃取-高效液相色譜測(cè)定水中酚類(lèi)化合物5第5頁(yè),課件共16頁(yè),創(chuàng)作于2023年2月1.Reversed-phaseliquidchromatographicmethodforthedeterminationofselectedroom-temperatureionicliquidcations

Abstract

Theseparationofselected1-alkyl-and1-aryl-3-methylimidazolium-basedroomtemperatureionicliquidcationshasbeenperformedusingreversed-phasehigh-performanceliquidchromatographywithelectrosprayionizationmassdetection.TheRP-HPLCmethoddevelopmentstartedwiththeselectionofacolumntakingintoaccountespeciallytheresolutionoflowmolecularcongenersoftheselectedgroup.Mobilephasecompositionwasoptimizedforpeakresolution,sensitivityandhighreproducibilityofretentionvalues.Theresultsofthemethoddevelopmentwereappliedtothedeterminationofexemplaryionicliquidspeciespresentinthemediumusedincytotoxicitystudies.6第6頁(yè),課件共16頁(yè),創(chuàng)作于2023年2月2.EffectofIonicLiquidsasMobilePhaseAdditivesonRetentionofCatecholaminesinReversed-PhaseHigh-PerformanceLiquidChromatography

Abstract

Ionicliquidsorroomtemperatureionicliquidshavebeenwidelyinvestigatedasnewsolventsforcatalysisinthepastseveralyears.Becauseofsomespecialpropertiesofionicliquids,interestofusingthemindifferentchemicalprocessesisincreasing.Thisworkreportsontheuseof1-alkyl-3-methylimidazoliumsaltsandN-butyl-pyridiniumsaltsasnewmobilephaseadditivesforseparationofcatecholaminesinreversed-phasehigh-performanceliquidchromatography.Thegoodseparationisachievedbyusingtheseadditives.DifferentpHvaluesofthemobilephase,concentrationofionicliquids,anddifferentalkylsubstituentsonthecationsordifferentcounterionofionicliquidswereinvestigated.Theseparationmechanisminvolvesmolecularinteractionsbetweenionicliquidsandcatecholamines.

7第7頁(yè),課件共16頁(yè),創(chuàng)作于2023年2月3.Analysisofselectedionicliquidcationsbyionexchangechromatographyandreversed-phasehighperformanceliquidchromatography

Abstract

Thechromatographicbehaviorofionicliquids-homologuesof1-alkyl-3-methylimidazoliumand4-methyl-N-butylpyridinium-hasbeeninvestigatedwithastrongcationexchangeadsorbent.Inparticular,thedependenceoftheretentionpropertiesofthesesolutesonmobilephasecomposition,pH,andbufferconcentrationwasevaluatedwiththeaimofoptimizingandimprovingtheselectivityandretentionofsoluteseparation.WhileusingtheSCXstationaryphase,severalinteractionsoccurredwithvaryingstrengths,dependingonthemobilephasecomposition.Cationexchange,nonspecifichydrophobicinteractions,andadsorptionchromatographybehaviorwereobserved.Reversedphasechromatographyoccurredatlowconcentrationsofacetonitrile,electrostaticandadsorptioninteractionsathigherorganicmodifierconcentrations.Elevatedbufferconcentrationsloweredtheretentionfactorswithoutaffectingtheselectivityofionicliquids.Obtainedresultswerefurthercomparedtothechromatographicbehaviourofionicliquidsinthereversedphasesystem.Allanalyzedionicliquidsfollowreversed-phasebehaviorwhilebeingseparated.Muchlowerselectivityintherangeofhighlyhydrophiliccompoundsisobtained.Thissuggestspreferreduseofionchromatographyforseparationandanalysisofcompoundsbelow4carbonatomsinthealkylsidechain.

8第8頁(yè),課件共16頁(yè),創(chuàng)作于2023年2月4.Effectof1-alkyl-3-methylimidazolium-basedionicliquidsastheeluentontheseparationofephedrinesbyliquidchromatography

Abstract

Thechromatographicbehaviorofephedrines(norephedrine,ephedrine,pseudoephedrineandmethylephedrine)onaC18columnwasstudiedwithdifferentconcentrationsof1-butyl-3-methylimidazoliumtetrafluoroborateionicliquidsastheeluentatpH3.0.Theadditionofionicliquidhasgreateffectsontheseparationofthesebasiccompounds:decreasingbandtailing,reducingbandbroadening,andimprovingresolution.Theretentiontimesoftheanalytesincreaseatfirstandthendecreasewiththeincreaseintheconcentrationofionicliquid.Thiseffectmaybeattributedtothecompetitionbetweenimidazoliumcationsandthepolargroupsoftheanalytesforthesilanolgrouponthealkylsilicasurface,andalsototheformationofweakbilayerelectronicstructureontheC18column.Severalionicliquidswithdifferentalkylsubstituentsontheimidazoliumcationsorwithdifferentcounterionsastheeluentswerecompared.9第9頁(yè),課件共16頁(yè),創(chuàng)作于2023年2月5.Ionicliquid-basedaqueoustwo-phasesystem,asamplepretreatmentprocedurepriortohigh-performanceliquidchromatographyofopiumalkaloids

Abstract

Anionicliquid,1-butyl-3-methylimidazoliumchloride([C4mim]Cl)/saltaqueoustwo-phasesystems(ATPS)waspresentedasasimple,rapidandeffectivesamplepretreatmenttechniquecoupledwithhigh-performanceliquidchromatography(HPLC)foranalysisofthemajoropiumalkaloidsinPericarpiumpapaveris.Tofindoptimalconditions,thepartitionbehaviorsofcodeineandpapaverineinionicliquid/saltaqueoustwo-phasesystemswereinvestigated.Variousfactorswereconsideredsystematically,andtheresultsindicatedthatboththepHvalueandthesalting-outabilityofsalthadgreatinfluenceonphaseseparation.Therecoveriesofcodeineandpapaverinewere90.0–100.2%and99.3–102.0%,respectively,fromaqueoussamplesofP.papaverisbytheproposedmethod.10第10頁(yè),課件共16頁(yè),創(chuàng)作于2023年2月6.Suppressionofdeleteriouseffectsoffreesilanolsinliquidchromatographybyimidazoliumtetrafluoroborateionicliquids

Abstract

Silica-basedstationaryphasesarecommonlyusedinliquidchromatography,buttheirsurfaceaciditycausesknownproblems,especiallywhenseparatingbasiccompounds.Deleteriouseffectsoffreesilanolsarenotfullyremovedbystandardpreventionproceduresconsistinginaddingalkylaminesorotheraminoquencherstotheeluents.Wefoundthationicliquidsoftheimidazoliumtetrafluoroborateclass,addedtomobilephasesatconcentrationsof0.5–1.5%(v/v),blockedsilanolsandprovidedexcellentthin-layerchromatographicseparationsofstronglybasicdrugswhichwereotherwisenoteluted,evenwithneatacetonitrileasthemobilephase.Thesilanolsuppressingpotencyofimidazoliumtetrafluoroborateswasdemonstratedtomarkedlyexceedthatofthestandardmobilephaseadditives,liketriethylamine,dimethyloctylamineandammonia.Theproposednewmobilephaseadditiveswerealsodemonstratedtoprovidereliablelipophilicityparametersofbasedruganalytesasdeterminedbygradientmodeofhigh-performanceliquidchromatography.Byapplyingthereadilyavailableandenvironmentallyfriendlyimidazoliumtetrafluoroborateionicliquids,simpleandefficientmeansofimprovementofliquidchromatographicanalysisoforganicbaseswereelaborated.11第11頁(yè),課件共16頁(yè),創(chuàng)作于2023年2月7.Reductionofsilanophilicinteractionsinliquidchromatographywiththeuseofionicliquids

Abstract

Asuppressionofsilanophilicinteractionsbytheselectedionicliquidsaddedtothemobilephaseinthin-layerchromatography(TLC)andhigh-performanceliquidchromatography(HPLC)isreported.Acetonitrilewasusedastheeluent,aloneorwithvariousconcentrationsofwaterandphosphoricbufferpH3.Selectivityofthenormal(NP)andthereversed(RP)stationaryphasematerialwasexaminedusingaseriesofproton-acceptorbasicdrugsanalytes.TheionicliquidsstudiedappearedtosignificantlyaffectanalyteretentioninNP-TLC,RP-TLCandRP-HPLCsystemstested.Consequently,theincreasedseparationselectivitywasattained.Duetoionicliquidadditivestoeluentevenanalytescouldbechromatographed,whichwerenotelutedfromthesilica-basedstationaryphasematerialswith100%ofacetonitrileinthemobilephase.Additionofionicliquidalreadyinverysmallconcentration(0.5%,v/v)couldreducetheamountofacetonitrileusedduringtheoptimizationofbasicanalytesseparationsinTLCandHPLCsystems.Moreover,theinfluenceoftemperatureontheseparationofbasicanalyteswasdemonstratedandconsideredinpracticalHPLCmethoddevelopment.12第12頁(yè),課件共16頁(yè),創(chuàng)作于2023年2月8.DeterminationofOrganophosphorousPesticidesinWaterSamplesUsingIonicLiquid-basedLiquidPhaseMicroextractionCoupledwithHighPerformanceLiquidChromatographyXie

Abstract

Anovelmethodforthedeterminationofthreeorganophosphorouspesticides(phorate,parathionandpoxim)inwatersampleshasbeendevelopedusingionicliquid-basedliquid-phasemicroextractioncoupledwithhighperformanceliquidchromatography.Theinfluenceofextractionparametersincludingextractionsolvent,thevolumeratioofextractionsolventtosampleaqueous,extractiontime,extractiontemperatureandstirringratewasinvestigated.1-butyl-3-methylimidazoliumhexafluorophosphatewasusedasextractionsolventanddisplayedparticularadvantagescomparedwithvolatileorganicsolventssuchasbenzene,hexaneandacetone.Theproposedmethodprovidedenrichmentfoldsof665,630and553forphorate,parathionandpoxim,respectively.Themethodhadgoodlinearrangeof0.01-0.1μL/Landthelimitsofdetectionofthethreepesticideswereintherangeof0.001-0.01μL/L.TheRSDofmatrixspikedsampleswere3.4%,10.5%and2.4%forphorate,parathionandpoxim,respectively.13第13頁(yè),課件共16頁(yè),創(chuàng)作于2023年2月9.Ionicliquidsasadditivesinhighperformanceliquidchromatography:Analysisofaminesandtheinteractionmechanismofionicliquids

Abstract

Asnovelsolvents,ionicliquidshavemanyapplicationsinsynthesis,catalysisandanalyticalseparation,i.e.extractionandchromatographyseparation.Inthispaper,someaminesincludingbenzidine,benzylamine,N-ethylanilineandN,N′-dimethylanilineareseparatedusingionicliquidsasadditivesforthemobilephaseinhighperformanceliquidchromatography(HPLC).Theeffectsofthelengthofalkylchainorcounterionsondifferentionicliquidsandtheirconcentrationsontheseparationoftheseanalytesareperformed.Thedifferencesbetweenionicliquidsandtetrabutylammoniumbromide(TBA)ontheseparationofo-,m-,p-phthalicacidsarecomparedandtheresultsshowthationicliquidsareion-pairreagentsinessence,althoughtheirhydrophobicityandhydrogenbondingalsoplayimportantroles.14第14頁(yè),課件共16頁(yè),創(chuàng)作于2023年2月10.AnalysisofPhenolicCompoundsbyIonicLiquidBasedLiquidLiquidExtractionCoupledwithHighPerformanceLiquidChromatogra

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