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1、湖南大学博士学位论文生物碱的分离分析及其液相色谱保留机理的研究姓名:罗旭彪申请学位级别:博士专业:分析化学指导教师:姚守拙;陈波20060714生物碱分析方法学和液相色谱保留机理的研究碎片离子,同时高锥孔电压技术能有效降低仪器的噪音,从而把维生素B12的检测限降低到ng/g。把这个方法应用到21金维他和牛奶食品中维生素B12的分析检测,取得非常满意的结果。关键词:液质联用;气质联用;制备色谱;“绿色”色谱;高锥孔电压;离子液体;挥发性离子对试剂;生物碱II博士学位论文AbstractDuetotheexcellentbiological
2、diversity,chemodiversity,andbioactivediversity,alkaloidsarepaidattentionverymuchallovertheworld.Thestudyontherapid,sensitive,reliable,qualitativeandquantitativeanalysismethodofalkaloidsincomplicatedmatricesiscontinuouslypopular.Inthepresentpaper,theseparationandanalysism
3、ethodsofdifferentkindsofalkaloidswithhighperformanceliquidchromatographycoupledwithmassspectrometry,gaschromatographycoupledwithmassspectrometry,“green”chromatography,andpreparativehighperformanceliquidchromatograhyhavebeensystematicallystudied.Thedetailsaresummarizedasf
4、ollows:1.Aporphinealkaloids,N-nornuciferine,O-nornuciferine,nuciferine,androemerine,havebeenisolatedandpurifiedfromtheleaveofNelumbonuciferaGaertnusingsilicagelcolumnchromatographyandpreparativehighperformanceliqudchromatography.Thestructuresofabovefouralkaloidshavebeenc
5、onfirmedbyanalyzingtheirspectraofUV,IR,113ESI-MS,H-NMR,andC-NMR.WithN-nornuciferine,O-nornuciferine,nuciferine,androemerineastargetcompounds,high-performanceliquidchromatography-photodiodearraydetection-electrospraymassspectrometryandgaschromatograpgy-massspectrometryhav
6、ebeendevelopedforthesimultaneousdeterminationofaporphinealkaloids.AndtheproposedmethodshavebeenappliedsuccessfullytothedeterminationsofN-nornuciferine,O-nornuciferine,nuciferine,androemerineinleavesofNelumbonuciferaGAERTNandhealthfoods.2.α-Naphthaphenanthridinealkaloids,
7、sanguinarineandchelerythrine,havebeenisolatedandpurifiedforthefirsttimefromthefruitofMacleayacordata(Willd)R.Br.usingmacroporousadsorptionresin.Thestructuresofabovetwoalkaloidshavebeenconfirmedby113analyzingtheirspectraofUV,IR,ESI-MS,H-NMR,andC-NMR.Withsanguinarine,chele
8、rythrine,protopine,andallocrytopineastargetcompounds,theisocratichigh-performanceliquidchromatographicm