琥珀酰明胶的制备

2710201010JournalofShenyangPharmaceuticalUniversityVol27No10Oc.t2010p767:2009-11-02:(1971-),(),,,[e-mail];(1962-),(),,,,,Tel.[phone],[e-mail]:1006-2858(2010)10-0767-05郝艳茹,高亦鲲,姜同英,王思玲(,110016):,,IR1H-NMRUV,,:200mgL-1,10mgL-1,pH10,90,2h1H-NMRIRUV50mgL-1,288mmolL-1,pH719,50mgL-1,,pH:;;:R94:A(succinylatedgelatin),,40mgL-1,[1],[2],,,,,,,1DF-101S(),DM-18(),MDF-U32V(SANYOElectricBiomedical),FDU-1100(),IFS-55(Bruker),AVANCE-600(Bruker),WFZUV-4802H(),SD-1000(),KS017(),WESCORVapro-5520(),PB-10pH()(),(),()(),(),(),()221,,,1Fig.1Syntheticpathwayforthepreparationofsuccinylatedgelatin10g50mL,37mL(26%)200mgL-1(22),,90,10molL-1pH1005g,,pH,pH102h20%pH6,[3-4]12h,3L,,0512482448h,72h22,,,2212mL,-708h,16h20Pa22210mg,KBr,GelatinReferenceFreeze-drying,22320,10mLDMSOH2OCH3OHCHCl3CH3COCH301g,,(DMSO,),D2O10mg,,GelatinReferenceFreeze-dr-ying,D2O1H-NMR(300MHz)22420mg,8mL,GelatinReferenceFreeze-drying,200~400nm2320mL,,1Table1Parametersofspraydryingofsuccinylatedgelatinp(atomizing)/kPaqv(blower)/(m3min-1)(inlet)/qv(pumpspeed)/(mLmin-1)2010307011020,,22,Spray-drying243050gL-1,:331mL,33311,,30gL-1530mg,50gL-1550mg,22111,2mL,,257682725120mL,1g,221,,40gL-1252,,3,253pH,pHpH,3,331,3232122,,,C=O(I)NH(II)C-N,;CH2CH2,CH2CH2Fig.2IRspectraofgelatin(a),reference(b),freeze-drying(c)andspray-drying(d)Table2IRspectradataofgelatin,reference,freeze-dryingandspray-drying[5-6]/cm-1GelatinReferenceFreeze-dryingSpray-dryingVibrationtypeGroup34428342133419433980N-HNH293392932229312C-HCH216374164411644716452C=OCONH-(amideIband)154551545715457N-HCONH-(amideIIband)145081451114510C-HCH213842138431384213843SC-HCH3124171240612421C-NGe-lNH32233,,,12,232~233236~237CH2CH2323,,COn-*230nm[7],,76910:Fig.31H-NMRspectraofgelatin(a),reference(b),freeze-drying(c)andspray-drying(d)Table3Identificationofthelinesinthe1H-NMRspectra[8]No.oflineAminoacidTypeofprotons1084-086Va,lLeu,I-Leu-and-CH32113-116Thre-CH33131-133AlaCH34158-160Arg;Lys-and-CH2;-,-and-CH25194-196Pro;Meth-,-and-CH2;-CH2andCH36219-222Glu;Hypro-and-CH2;-CH27262-265Asp-CH28291-293Lys-CH29312-315Arg;Hys-CH2;-CH210355-357Pro-CH211381-387Gly;Hypro-CH2;-CH12726-727Phen,TyrAromaticC-2,6x232-233Succinyl-CH2y236-237Succinyl-CH233,43,(d)(b),12,2;22,(d)(b)C=O(I)(27,5),110,,10077027,,Fig.4Micrographofspray-drying(1000)34324,50gL-1,,,50gL-135288mmolL-1,298mmolL-1pH719,pH74Table4EffectsofvariouskindsofprotectiveagentsGroup/(gL-1)Appearancet(averagedissolving)/sPuredrugAtrophicandfissured265Mannitol30Bulkyandplump88Mannitol50Bulkyandplump80Lactose30Bulkyandplump120Lactose50Bulkyandplump118Glucose30Bulkybutshriveled236Glucose50Bulkybutshriveled215NaCl30Atrophicandporous320NaCl50Atrophicandporous295Sucrose30Glass-like348Sucrose50Glass-like3204,,,,50gL-1,,pH,:[1]DEJONGEE,LEVIM.Effectsofdifferentplasmasub-stitutesonbloodcoagulation:acomparativereview[J].CritCareMed,2001,29:1621-1627.[2].[J].,2001,12(9):9-10.[3],.[J].,2002,10(3):17-19.[4]ROBERTSJS,BRATTONSL.Colloidvolumeexpand-ers-problems,pitallsandpossilities[J].Drugs,1998,55(5):621-630.[5],,,.[M].3.:,1986:243-272.[6],.-[J].,2001,14(1):100-106.[7],.[J].,2003,20(6):900-902.[8]RODINVV,IZMAILOVAVN.NMRmethodinthestudyoftheinterfacialadsorptionlayerofgelatin[J].ColloidsandSurfaces,1996,A:95-102.(776)77110:Abstract:ObjectiveToinvestigatetheeffectsofO-acylmentholderivativesoninvitroskinpermeationofpiperinefromPiperislongiextractumpatchandpredictthepotentialcapabilityofPiperislongiextractumtobeformulatedinapatch.Methods2-Chamberdiffusioncellswereadoptedastheapparatusforinvitroskinpermeation,excisedratabdominalskinasbarrier.HPLCwasusedtodeterminethecontentofpiperineinre-ceiverdiffusioncel.lResults2-Isopropy-l5-methylcyclohexylpentanoate,2-isopropy-l5-methylcyclohexylhexanoate,2-isopropy-l5-methylcyclohexylbutyrateand2-isopropy-l5-methylcyclohexy-l2-hydroxypanoateproducedsignificantenhancingeffectsonpiperinepermeation.Ofthese,2-isopropy-l5-methylcyclohexylpen-tanoatehadthegreatestenhancingeffec.t2-Isopropy-l5-methylcyclohexylheptanoate,2-isopropy-l5-methy-lcyclohexyltetradecanoateand(E)-2-isopropy-l5-methylcyclohexyloctadec-9-enoatehadnoeffectonpiper-inepermeation.Mentholproducedaninhibitiveeffectonpiperinepermeation.ConclusionsThecumulativetransportandthefluxofpiperineincreasemarkedlywhenchemicalenhancersareaddedinthepatches,allo-wingarationalapproachfordesigninganeffectivePiperislongiextractumpatch.Keywords:Piperislongiextractum;patch;piperine;O-acylmentholderivative;skinpermeation(771)PreparationofsuccinylatedgelatinforinjectionHAOYan-ru,GAOY-ikun,JIANGTong-ying,WANGS-iling(SchoolofPharmacy,ShenyangPharmaceuticalUniversity,Shenyang110016,China)Abstract:ObjectiveTopreparesuccinylatedgelatinforinjection.MethodsSuccinylatedgelatinwassynthe-sizedandthencharacterizedusingIR,1H-NMRandUV.Succinylatedgelatinforinjectionwaspreparedbyspraydryingandfreeze-drying.Theredispersionpropertiesofsuccinylatedgelatinforinjectionwereinvest-igated.ResultsSuccinylatedgelatincouldbesynthesizedundertheconditionsasfollows:theconcentrationofgelatinwas200mgL-1,theconc