Sephadex-LH-20-层析原理和应用基础

HansHenkePreparativeGelChromatographyonSephadexLH-20SephadexLH-201.SephadexLH-20HPLCGPC1000SephadexLH-20-SephadexLH20/1HPLCGPCSephadexLH20HPLCGPC1(hydroxypropylateddextrangel)SephadexLH20HPLCGPCSephadexLH20HPLC+HPLC11t0AHPLCHPLCB(MSC)CABSephadexLH-20Vads()V0V0+ViC=A+BV0ViV0+Vi+Vads------AHPLCt0HPLC,RPCNNH2B=SECVi()V01)W.Winkle,QuantitativeAnalysisintheV0-Zone,AQuantitativeAprpooachbyCouplingHPLCwithGPC”inChromatographiaVol.29.(1990)530.DataFilesTCM-2003-02AA1HansHenkePreparativeGelChromatographyonSephadexLH-20ViV0+ViCMSCSephadexLH-20G-MW1000SephadexLH-20A+BV0+Vi2.2.1SephadexLH-20SephadexLeuconostocmesenteroidesP.Flodin,PhDThesis,Uppsala1962:MW1DataFilesTCM-2003-02AA2HansHenkePreparativeGelChromatographyonSephadexLH-20SephadexGSephadexG-10SephasorbHP,G-25G-50SephadexLH-20LH-60SephadexLH-20SephadexGSephasorbHPSephadexLH-20LH-605SEM4SephadexLH-204SephadexLH-2027012.2V0ViMSCViV0DataFilesTCM-2003-02AA3HansHenkePreparativeGelChromatographyonSephadexLH-20V0+Vi2**b12)anD20Cp20()*/b)N--2--1.4700-5.0-5.381C1.3330-4.0-4.41000.951.32900.603.9-4.365d)0.401.44600.573.8-4.1610.421.42400.443.6-3.9400.451.4070-3.3-3.6670.561.35900.322.4-2.6560.581.37200.451.6-1.877(10)a)LCL.R.Snyder:PrincipleofAdsorptionChromatography”Hildebrandtscale.M.Dekker.b)SephadexLH-20-ChromatographyInOrganicSolvents”NMPc)0.95d)1%5.SephadexLH-20.PharmaciaBiotechcompanySephasorbTMHPUltrafine,Chromatographyinorganicsolvents.DataFilesTCM-2003-02AA4HansHenkePreparativeGelChromatographyonSephadexLH-20SephadexLH-2040004000V0SephadexLH-20SephadexLH-20G-2SephadexG-10G20070200000V0ViV0Vi//V0Vi5=25/26N-125SephadexLH2012966DataFilesTCM-2003-02AA5HansHenkePreparativeGelChromatographyonSephadexLH-203.3.1SephadexLH-20SephadexLH-20/SephadexLH-20/116-1-2-216-PU52/16-2RP3070SephadexLH-2015181430|18246002DataFilesTCM-2003-02AA6HansHenkePreparativeGelChromatographyonSephadexLH-2019931135152/νR21≈2.5R32≈2V0+ViDataFilesTCM-2003-02AA7HansHenkePreparativeGelChromatographyonSephadexLH-202.32.42.53.2Hildebrandt2/II.4.2.,-,SephadexLH-201DataFilesTCM-2003-02AA8HansHenkePreparativeGelChromatographyonSephadexLH-20PBA54/ω52/2DGTMGTDMT1=V0+Vi351,DataFilesTCM-2003-02AA9HansHenkePreparativeGelChromatographyonSephadexLH-204,,16--217815C16C12C254/ω15RP84X250HPLCC2-C690101/16-1315-6C8-C16C18-C226TMP8704/1→22→38705*HPLC/6535SephadexLH-20DataFilesTCM-2003-02AA10HansHenkePreparativeGelChromatographyonSephadexLH-20-851.SephadexLH-20(1=25+2X2=26=25)()4/851∑=1615/2.5SephadexLH-204/867SephadexLH-202-3-12-13-14-12-13--OH23--OH14--OH1,213-23-14-DataFilesTCM-2003-02AA11HansHenkePreparativeGelChromatographyonSephadexLH-208623-14-523-14-8SephadexLH2054/128770205.58794/t51=/170-OH2=8153=/3103-OHDataFilesTCM-2003-02AA12HansHenkePreparativeGelChromatographyonSephadexLH-2020104-54/t(2)1H-NMR88140351=3.6%R=-11PTGPTG(MEK)5588:,,,(MEK)MEK2.7%PEG52/13125200115NN.-NN.-3DataFilesTCM-2003-02AA13HansHenkePreparativeGelChromatographyonSephadexLH-20892001154/870125901335015090870=258/2.4----HPLCHildebrand2/II.,4.2SephadexLH-20TCLRf100-350100TCL-NH2-NH-,SephadexLH-201373TMP-DataFilesTCM-2003-02AA14HansHenkePreparativeGelChromatographyonSephadexLH-20--/--1M695CH3OH→1CH2Cl223502551916878671291.5%THFTHF67927280711471.4%150-20025X3502/522173-NH-7-3--NH-7--NH-3--NH-DataFilesTCM-2003-02AA15HansHenkePreparativeGelChromatographyonSephadexLH-20-3-9212712711325X8702/100-150/44-5•2/93210:2354184:25516.7%CD2Cl2=V0+Vi400/5DataFilesTCM-2003-02AA16HansHenkePreparativeGelChromatographyonSephadexLH-205936-14--14-350III.519104/318702.5-HildebrandtLC2/II.4.2.SephadexLH20,,SephadexLH201.72.5/ViVi3V0+Vi1A4NO71GDSGMS1/32-HPLCRP/185-94%DataFilesTCM-2003-02AA17HansHenkePreparativeGelChromatographyonSephadexLH-20drawback”--12-13-/GMS4.395315=25/26/233951112-535046/12/305092/9649015007665062900424X35048/DataFilesTCM-2003-02AA18HansHenkePreparativeGelChromatographyonSephadexLH-20975125.1258--6097126.31--SephadexLH-2056251-68NB1-C22H45-OH1-C20H41-OH10331+2X225/26οSephadexLH-202/50455050DataFilesTCM-2003-02AA19HansHenkePreparativeGelChromatographyonSephadexLH-201CH3-CH216-CH2-OH2703102CH3-CH214-CH2-OH2423523CH3-CH212-CH2-OH2144004CH3-CH210-CH2-OH186502=V0+Vi745CH3-CH28-CH2-OH1586006CH3-CH26-CH2-OH1306767CH3-CH24-CH2-OH1028058CH3-CH22-CH2-OH74905414/7a26/7b87025X10005997a25X8704/9912--,22-7b25X8704/TLCTLC2--2-Rf,0.880.760.380.74TLC5MEKN-1.4%8705/-CH2--NH--NH-281040170DataFilesTCM-2003-02AA20HansHenkePreparativeGelChromatographyonSephadexLH-2064/SephadexLH-20SephadexLH-2081008.MEKN-1X258702/2.6N--2-NMPHPLCN--2-NMPNMP2021.67N--2-(NMP),(DMSODMF)NMP81-82/0.1101912VADSViV0MSC+V08500=804V0+Vi:84=1950Vi=1146910128500Irganox1010?11762-4-3262SephadexLH20NMP2/II.4.2V0ViII.4.2.5SephadexLH20NMPViNMP952/DataFilesTCM-2003-02AA21HansHenkePreparativeGelChromatographyonSephadexLH-2095V0+ViVi741-Vi25NMP5-6,45504PVC21Quickfit2.7SephadexLH-20SephadexLH-20/52/tR()()2000=V02X1066241801340*921545901630CH3-O-CH2-CH2-O-CH3761630CH3-O-CH2-CH2-OH621630HO-CH2-CH2-OH581742CH3-OH=V0+Vi3218:12CH3CN()411824H2N-CO-NH2601839H2N-CN4227481263654*2.2%SephadexLH-20-1DataFil