USP 35阿司匹林原料药质量标准.pdf

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1、Accessedfrom128.83.63.20bynEwp0rt1onMonNov2122:19:00EST2011USP35OfficialMonographs/Aspirin2245W=weightofSample(mg)·USPREFERENCESTANDARDSá11ñAcceptancecriteria:98.5%–101.5%onthedriedbasisUSPAsparticAcidRSIMPURITIES·RESIDUEONIGNITIONá281ñ:NMT0.1%·CHLORIDEANDSULFATE,Chlorideá221ñ.Samplesolut

2、ion:Dissolve0.7gofAsparticAcidin10mLAspirinofdilutednitricacid,anddilutewithwaterto15mL.Acceptancecriteria:TheSamplesolutionshowsnomorechloridethancorrespondsto0.20mLof0.020Nhydrochloricacid(NMT0.02%).·CHLORIDEANDSULFATE,Sulfateá221ñSamplesolution:Dissolve0.8gofAsparticAcidin4mLofhydrochl

3、oricacid,anddilutewithwaterto15mL.Acceptancecriteria:TheSamplesolutionshowsnomoreC9H8O4180.16sulfatethancorrespondsto0.25mLof0.020NsulfuricacidBenzoicacid,2-(acetyloxy)-.(NMT0.03%).Salicylicacidacetate[50-78-2].·IRONá241ñ:NMT10ppm»Aspirincontainsnotlessthan99.5percentand·HEAVYMETALS,Metho

4、dIIá231ñ:NMT10ppm·CHROMATOGRAPHICPURITYnotmorethan100.5percentofC9H8O4,calcu-Systemsuitabilitysolution:10mgeachofUSPAsparticlatedonthedriedbasis.AcidRSandglutamicacidin2mLofammoniaTS.Dilutewithwaterto25.0mL.PackagingandstorageÐPreserveintightcontainers.Standardsolution:Transfer5mgofUSPAsp

5、articAcidRStoa100-mLvolumetricflask,dissolvein2mLof17%USPReferencestandardsá11ñÐammoniasolution(preparedbydilutingammoniumUSPAspirinRShydroxide,6in10),anddilutewithwatertovolume.IdentificationÐSamplesolution:Transfer0.1gofAsparticAcidtoa10-mLA:Heatitwithwaterforseveralminutes,cool,andadd1

6、orvolumetricflask,dissolvein2mLof17%ammoniasolution2dropsofferricchlorideTS:aviolet-redcolorisproduced.(preparedbydilutingammoniumhydroxide,6in10),andB:InfraredAbsorptioná197Kñ.dilutewithwatertovolume.Lossondryingá731ñÐDryitoversilicagelfor5hours:itChromatographicsystemlosesnotmorethan0.5

7、%ofitsweight.(SeeChromatographyá621ñ,Thin-LayerChromatography.)Mode:TLCReadilycarbonizablesubstancesá271ñÐDissolve500mginAdsorbent:0.25-mmlayerofchromatographicsilicagel5mLofsulfuricacid:thesolutionhasnomorecolorthanmixtureMatchingFluidQ.Applicationvolume:5mLResidue