胺化超高交联吸附树脂的制备及其对喜树碱和喜果苷的色谱分离

a,ba3aaaa(a,300071;b())(Rf18)(Rs3)N2(Rs4)(Rs5)(Rs6),,,(Rs6)2114Rf18Rs3Rs5,;Rs6,,80%(pH=4),,36,23,,,,:O647.3:A:100020518(2005)01200242062004203226,2004207216(20174017):,,1937,,;E2mail:[e-mail];:(CPT)(VCS2LT)[13],3,[46][7],(),2,,;,,,,,,ADS25[7],211.1,;();:(+)2camptothecin98%(ACROSorganics,);;ADS25()Waters510HPLC,486Waters,HL22,BSZ2100,DSHZ23001.28%,V()V()=11,,1d,2,,3d,,221Vol.22No.120051CHINESEJOURNALOFAPPLIEDCHEMISTRYJan.2005,0107401147mm,(Rf18)20gRf18,60mLNN2,40mL(),20%NaOHpH1112,503d,,Rs3(Rs5Rs6)15gRs3,50mL,10010h,,,5%3h,,N2(Rs4)Rs3Rs5Rs610%NaOH10%HCl,,10%NaOH,GB5757286[8],BET[8]1.3(HPLC)KromasilC18,5m,416mm150mm,30%,018mL/min,256nm1.4,ADS25[8]012g,100mL,25mLADS252524h,HPLC,,1.5(=019cm)7mL(),2BV/h,15BV(BV:),2BV,50%70%(1BV/h),,HPLC22.1,,N2,,11Table1PhysicalandchemicalparametersofsynthezedresinsResinImbeddedmoisture/%Functionalgroup/(mmolg-1)Specificsurfacearea/(m2g-1)Rf1848.58--395.9Rs357.08methylamine2.28319.0Rs455.92N2methylacetamido2.28369.2Rs560.34dimethylamine2.34210.2Rs661.09trimethylamine2.33174.1Note:Rf18:macroporoushypercrosslinkedresin;Rs3:methyiamine;Rs4:N2methylacetamido;Rs5:dimethylamine;Rs6:trimethylamine.1,,,,,,,2.22,(AmberliteXAD24XAD22)[9];[3],,2521:2Table2StaticadsorptionofcamptothecinandVincosideLactambysynthesizedresinsResinAdsorptioncapacity/(mgg-1)(drybeads)CPTVCS2LTc/vRf1811.0523.502.47Rs314.8733.223.82Rs411.4832.141.17Rs516.3531.014.46Rs620.3325.49114.0Notes:theinitialconcentrationofcamptothecin(CPT)andVincoside2Lactam(VCS2LT)were010231mg/mL,0.126mg/mLrespectively.2,,,,,(K),,(),,,Rs6,114,45,E(pH5),,()[10],,Rs6,,,,Rs62Scheme1Chemicalstructureof20(s)2camptothecinlactone,itscarboxylatesaltandvincoside2lactam2.3ADS25,50%60%,,,CPT,,,25%30%38%20%,Rf18121,20%,74BVVCS2LTCPT,38%,VCS2LT10BV,CPT24BV,,2,VCS2LTCPT,VCS2LT,CPT,VCS2LTCPT1050BV,VCS2LTCPT31025BV,VCS2LTRs6,,50%,3,(0BV),,25BV,025BV,VCS2LTRs3Rs5Rf18Rs62.4ADS25,,,Rf18Rs3Rs56222,50%,,70%,4,1VCS2LT,2CPT,Rs4,50%,,,5(c/v=1117)Rs6,50%,,,80%,2(Et2OH)80%,pH4,(6),,Rs6,pH=4,,,,,,721:5Rs4Fig.5ChromatographicseparationofCPTandVCS2LToncolumn:Rs41.CPT,(Et2OH)=50%;2.VCS2LT,(Et2OH)=50%6Rs6Fig.6ChromatographicseparationofCPTandVCS2LToncolumn:Rs61.CPT,(Et2OH)=50%;2.VCS2LT,(Et2OH)=80%(pH=4)Rs6,,Rs4233Table3ChromatographicseparationresultsofCPTandVCS2LTResinContent/%Recovery/%CPTVCS2LTCPTVCS2LTRf1815.044.19079.4Rs311.060.688.196Rs4canntseparateRs527.544.69874.4Rs69.3651.873.677.0Notes:ThecontentofCPTandVCS2LTininjectedsolutionwas4.18%and22.74%respectively.,36,23,73%98%1WallME,WaniMC,CookCE,etal.JAmChemSoc[J],1966,88(16):38882LINLong2Ze(),ZHAOZhi2Yuan(),XURen2Sheng().ActaChemSinica()[J],1977,35(3,4):2273LINLong2Ze(),SHENJi2Hui(),HEXiang().ActaChemSinica()[J],1988,46(12):12074LINLong2Ze(),SONGChun2Qing(),XURen2Sheng().ActaChemSinica()[J],1982,40(1):855LINLong2Ze(),SONGChun2Qing(),XURen2Sheng().ActaChemSinica()[J],1979,37(3):2076XURen2Sheng(),ZHAOZhi2Yuan(),LINLong2Ze().ActaChemSinica()[J],1977,35(3,4):1937WANGRui2Fang(),SHIZuo2Qing(),SHIRong2Fu().IonExchangeandAdsorption(8222)[J],2002,18(5):4128HEBing2Lin(),HUANGWen2Qiang().IonExchangeandAdsorptionResins()[M].Shanghai():ShanghaiScienceandTechnologyEducationPress(),19929MillerWL,KulltengMP.BiochemMed[J],1973,7(1):14510OLearyJ,MuggiaFM.EuropeanJCancer[J],1998,34(10):1500PreparationofAminatedMacroporousHypercrosslinkedResinsandTheirApplicationinChromatographicSeparationofCamptothecinandVincoside2LactamWANGRui2Fanga,b,SHIZuo2Qinga3,SHIRong2Fua,ZHANGJing2Zea,YANGWen2Honga,WUWeia(aStateKeyLaboratoryofFunctionalPolymericMaterialsforAdorptionSeparation,InstituteofPolymerChemistry,NanKaiUniversity,Tianjin300071;bSuntarMembraneTechnology(Xiamen)CO.,Ltd,Xiamen)AbstractMacroporoushypercrosslinkedresin(Rf18)wassynthesizedfromstyreneanddecoratedbyloadingmethyiamine(Rs3),N2methylacetamido(Rs4),dimethylamine(Rs5)andtrimethylamine(Rs6)respectively.TheadsorptionandchromatographicseparationofcamptothecinandVincoside2Lactam(VCS2LT)bythesynthesizedresinswerecompared.Theiradsorptioncapacityandadsorptionselectivityforcamptothecinandvincoside2lactamwerefoundtoberemarkablyincreased.Forquaternaryammoniumresin(Rs6),thesepara2tionimpact(c/v)was114.Camptothecinandvincoside2lactamcouldbeeffectivelyseparatedwithresinsRf18(Rs3,Rs5).ButcamptothecincouldnotbewashedoutfromRs6withorganicsolvent,itcouldbeeasilywashedoutwithacidicsolutionof80%ethanol2water(pH=4).Keywordscamptothecin,Vincoside2Lactam,aminated2macroporoushypercrosslinkedresin,adsorptionper2formance,chromatographicseparation921: