毛細(xì)管電泳-電化學(xué)發(fā)光用于含胺類藥物的檢測.pdf_第1頁
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1、廣西師范大學(xué)碩士學(xué)位論文毛細(xì)管電泳電化學(xué)發(fā)光用于含胺類藥物的檢測姓名:李林秋申請學(xué)位級別:碩士專業(yè):分析化學(xué)指導(dǎo)教師:鄧必陽200804022005級分析化學(xué)研碩士論文IITheapplicationofcapillaryelectrophesiswithelectrochemiluminescencedetectionftheanalysesofaminecontainingpharmaceuticalsPostgraduatestu

2、dent:LinqiuLiSupervis:ProfessBiyangDengSpecialty:AnalyticalChemistryResearchdirection:pharmaceuticalanalysisEntranceyear:2005ABSTRACTElectrochemiluminescence(ECL)whichcombinestheacteristicsofelectrochemistrychemiluminesc

3、enceisprovedtobeapowerfulanalyticaltoolwithadvantagesofsensitivityinsituwidelinearrangegoodivityetc.Capillaryelectrophesis(CE)hasbeengreatlyevolvedsince1980snowithasbeenprovedtobeaneffectivetechniquefseparationwithshtana

4、lysistimehighresolutionsmallsamplevolume.Thecombinationofcapillaryelectrophesiswithtris(22’bipyridyl)ruthenium(II)basedelectrochemiluminescencedetection(CEECL)showsmanyadvantagesfinstancehighivitygoodefficiencyfastanalys

5、isspeedeasyoperationetc.Nowthemethodhasbeenwidelyusedfthedetectionofnitrogencontainingcompoundsithasbeensuccessfullyapplyzedtopharmaceuticalsaminoacidsnarcoticsenvironmentalsamplesetc.AsamethodofanalysisCEECLwillbemewide

6、lyuseinmedicalscienceenvironmentalsciencelifescience.ThisthesisisconcentratedontheapplicationofCEECLftheanalysesofaminecontainingpharmaceuticals.Itscontentswereintruducedasfollows:1.AnovelsimplepharmacokiicsofPefloxacinm

7、esylate(PM)intheurineofahealthyadultwasdeveloped.TheproposedmethodologywasbasedontheECLintensityofruthenium(II)tris(bipyridine)ataplatinumelectrodewasgreatlyenhancedbyPM.Undertheoptimalconditionsthecalibrationcurvewaslin

8、earovertherangefrom0.05to10mgLwithadetectionlimitof0.006mgL(σ=3).Therelativestarddeviationofthepeakheightwas2.4%(n=6).Therecoveryinhumanurinewasbetween92.9%112%.Thehighestexcretionratewasobservedduring1.5hto2hafteraladmi

9、nistration.TheurinaryexcretionratioofPMwas13.5%within48h.2.Basedonelectrochemiluminescence(ECL)intensityofruthenium(II)tris(bipyridine)ataplatinumelectrodewasgreatlyenhancedbyBuflomedilhydrochlide(BUF)Verapamilhydrochlid

10、e(VER)thesimultaneousdeterminationofBUFVERinhumanplasmahasbeendevelopedusingcapillaryelectrophesiswithECL.Indertoincreasethesensitivity0.1mmolLaceticacidwasedassamplesolvent.Undertheoptimalconditions,thelinearrangeswere0

11、.001~3mgLfBUF0.01~12mgLfVER.Thedetectionlimits(3σ)fBUFVERwere0.00070.0047mgLrespectively.Therecoveriesofthetwodrugsatdifferentconcentrationswerebetween85%92%fBUF85%to93%fVER.Plasmaconstituentsdidnotinterferwiththedetermi

12、nationofBUFVER.3.Anovelmethodfthedeterminationofephedrinehydrochlide(EP)wasproposed.IndertoimprovethesensitivitytheprecolumnderivatizationofEPwithacetaldehydewasproposed.UndertheoptimalconditionstheECLintensityobtainedab

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