高速逆流色谱原理及应用.ppt

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1、高速逆流色谱原理及应用多级萃取技术离心分配色谱平面图离心分配色谱立体图同步行星式逆流色谱高速逆流色谱运行平面图分离区分离区混合区HSCCC系统连接工作图1、HPLC方法的建立尽可能使各峰得到良好的分离2、溶剂系统的选择根据样品的溶解特性选择溶剂体系测定分配系数，依据分配系数确定溶剂系统K2/K1:0.5-2.53、HSCCC分离条件优化色谱柱转速；固定相的保留；流动相流速；分离温度。4、HPLC测定收集组分的纯度HSCCC方法的建立过程:丁醇-醋酸-水丁醇-甲醇-水(缓冲液)丁醇-乙酸乙酯-水(缓冲液)乙酸乙酯-水(缓冲液)氯仿-甲醇-水(毒)甲基异丁基酮-

2、丙酮-水正己烷-乙酸乙酯-甲醇-水(石油醚-乙酸乙酯-甲醇-水)正己烷-乙腈正己烷-甲醇-水正己烷-乙酸乙酯-甲醇-水(石油醚-乙酸乙酯-甲醇-水)水溶性和强极性中等极性(氯仿)弱极性(正己烷)HSCCC常用溶剂系统（依据组分的极性和溶解性）PreparativeIsolationofSixMajorSaponinsfromPlatycodiRadixbyHigh-speedCounter-currentChromatographyYoungWanHaandYeongShikKimABSTRACT:Introduction–Platycosides,thep

3、rimaryconstituentsofPlatycodiRadix,areknowntohavenumerousandvariedbiologicalactivities,exertinganti-inflammation,anti-allergy,anti-tumour,anti-obesityandanti-hyperlipidemiaeffects.However,effectivemethodsforisolatingandpurifyingplatycosidesfromPlatycodiRadixarenotcurrentlyavailable

4、.Objective–TodevelopanefficientmethodforthepreparativeseparationofsixplatycosidesfromPlatycodiRadixbyhighspeedcounter-currentchromatography(HSCCC)coupledwithanevaporativelightscatteringdetection(ELSD)system.Methodology–Preparativeseparationwasperformedbywaterextractionusingreversed

5、-phaseC18columnchromatographyonanHSCCC-ELSDsystem.Atwo-phasesolventsystemcomprisedhexane–n-butanol–water(1:40:20,v/v)and(1:10:5,v/v)wasemployed.Twootherkeyparameters,revolutionspeedoftheseparationcolumnandflow-rateofthemobilephase,werealsoinvestigatedforoptimumHSCCCperformance.Each

6、peakfractionobtainedfromseparationoftheplatycosideswascollectedaccordingtotheELSDelutionprofileanddeterminedbyHPLC.Results–Usingthedescribedmethod,sixplatycosides,allwithpuritiesofover94%,couldbeisolatedfrom300mgoftheplatycoside-enrichedfraction.Theirstructureswerecharacterizedbyel

7、ectrosprayionisationmassspectrometry(ESI-MS),1HNMRand13C-NMR.IntroductionExperimentalApparatus.Reagentsandmaterials.Preparationofcrudesample.MeasurementofpartitioncoefficientsPreparationofthetwo-phasesolventsystemandsamplesolution.HSCCCseparationSelectionofthetwo-phasesolventsystem

8、andHSCCCconditionsResultsa