《文献读书报告》PPT课件.ppt

,Molecularlyimprintedcoatedgrapheneoxidesolid-phaseextractionmonolithiccapillarycolumnforselectiveextractionandsensitivedeterminationofphloxineBincoffeebean,AnalyticaChimicaActa,ImpactFactor:4.517,PhloxineBaninsecticidegastrictoxicityandcelltoxicitydetect：HPLCCZESPEMIPshighselectivityandspecificrecognitionphysicochemicalstabilityandapplicability,Introduction,MISPE,MISPEmonolithiccolumnhigherchemicalstability,selectivitymorefacilepreparationPreparation:insitupolymerizationusingnanostructuredimprintedmaterialsGOGO-MIPshigherloadingcapacityfasterassociation/dissociationkineticsimprovingtheaccessibilityandsensitivitytotargetspecies,PreparationoftheGO-MISPEmonolithiccapillarycolumn,GO,porogenmethanoltoluenedodecanol,30min,ultrasonication,phloxineB(template)MAA(functionalmonomer),mechanicallystirred1h,roomtemperature,EDMA(crosslinker)AIBN(initiator),purgedwithN2fill5min,(capillarytube),polymerization,5h60oCinawater-bath,wash甲醇-乙酸(90:10,v/v),washmethanol,theGO-MISPEmonolithiccapillarycolumn,PreparationoftheGO-MISPEmonolithiccapillarycolumn,ThecorrespondingGO-NIPsmonolithiccapillarycolumn-withouttemplateMIPsmonolithiccapillarycolumn-withoutGO,PreparationofphloxineBcoffeebeansamples,Thesamplesolutions咖啡豆研磨后过20目筛，转移至广口瓶于50C保存。咖啡豆粉末(1.0g)2.0mL甲醇萃取离心phloxineB标准溶液超声15min10,000rpm,10min重复两次。萃取液合并，用甲醇稀释至4.0mL。溶液过0.45m滤膜备用。加标浓度为1.0和20ng/mL,theGO-MISPEmonolithiccapillarycolumn1.分别用100l甲醇和水活化活化2.样品溶液以0.02ml/min流速通过毛细管整体柱进样3.用40l甲苯以0.02ml/min流速洗涤去除杂质4.用40l甲醇-乙酸(90:10,v/v)0.1mL/min洗脱洗脱收集洗脱液，氮气吹干，残留物溶解于0.2ml甲醇HPLCLIF,ProcedurefordeterminationofphloxineBcoffeebeansamples,Fig.1.ThechemicalstructureofphloxineB.,Resultsanddiscussion,Fig.2.SEMimagesof(a)thecolumnpreparedwithAM,(b)thecolumnpreparedwithMAA,(c)MIPs,(d)GO-MIPsand(e)themagnificationis20,000foldsford,Synthesisandmorphology,Fig.3.FT-IRspectraof(a)GOand(b)GO-MIPs.,methanoltoluenedodecanolpermeable,theflowrateof0.15ml/mintolueneanddodecanol3040%keeptheporesizevoidlessstructureMethanolaugmentedthesolubilityofGOandphloxineB,porogen,T:M:C,Capacityofthecolumn,Fig.4.BreakthroughcurvesofphloxineBonGO-NIPs,MIPsandGO-MIPscolumnandbreakthroughcurvesofrosebengalonGO-MIPscolumn.Loadingconcentration:1.0mg/mL;Sampleflowrate:0.02mL/min,capacity,0.006g/mg0.029g/mg0.040g/mg0.012g/mg,Selectionofeluentandwashingsolvent,Methodvalidation,A=1.620107C+262792over0.0012.0mg/mLR2=0.9995,themethodhadgoodprecisionevenatlowconcentrationsLOD=0.075ng/mL(S/N=3);LOQ=0.25ng/mL(S/N=10)LOD(0.3ng/g)HPLC(7.5ng/g)andCZE(10ng/g)coupledwithtraditionalSPEthismethodwasmoresensitive,Enrichmentsandimpurityremoval,Fig.5.Illustrativechromatogramsforthesampleenrichmentandimpuritiesremoval.(a)1.0ng/mL.phloxineBsamplebeforeloadedontothecolumnand(b)1.0ng/mL.phloxineBsampleafterloadedontothecolumn.,Conclusion,Insummary,anovelphloxineBmolecularlyimprintedmonolithiccapillarycolumnwaspreparedusingGOasthesupportmatrix.GO-MIPspresentedhighercapacityandaffinitythanthoseoftraditionalMIPs.TheGO-MISPEmonolithiccapillarycolumnasextractionapproa