六味地黄丸(浓缩丸)质量标准英文版

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LiuweiDihuangPills(concentratedpills)六味地黄丸(浓缩丸)PinyinLiuweiDihuangWanIgredientsPreparedRehmanniaRoot120g;FructusMacrocarpii60g;CortexMoutanRadicis45g;RhizomaDioscoreaeOppositae60g;Poria45g;RhizomaAlismatis45gProcedureDistillateCortexMoutanRadiciswithwatervapoforabstractingvolatilityingredients;Decoctthegruffs,FructusMacrocarpii20g,PreparedRehmanniaRoot,PoriaandRhizomaAlismatiswithwatertwice,2hoursforeverytime,filter,combinethefiltrated,concentratedthemtoextract;pulverizeRhizomaDioscoreaeOppositaeandexcessofFructusMacrocarpiitofinepowder,sifting,mixthoroughly,addtheaboveextractandvolatilityingredientsofCortexMoutanRadicis,mixthotoughly,maketopills,dry,polishing.DescriptionBrownishtoblackconcentratedpills,taste,sweat,acid,slightlybitter.Identification(1)Microscopical:Epidermalcellsofpericarporange-yellow,polygonalinsurfaceview,withsomewhatbeadedanticlinalwalls.Starchgranulestriangular-ovoidoroblong,24-40µmindiameterhilashortcleftVshaped.(2)Pulverize5gofthepills,heatunderrefluxwith20mlofetherfor1hour,filterandexpelether.Dissolvetheresiduein1mlofacetoneasthetestsolution.DissolvepaeonolCRSinacetonetoprepareasolutioncontaining1mgperml.asthereferencesolution.Carryoutthemethodforthinlayerchromatography(AppendixⅥB),usingsilicagelGasthecoatingsubstanceandcyclohexaneandethylacetate(3:1)asthemobilephase.Applyseparately5-10μlofeachofthetwosolutiontotheplate.Afterdevelopingandremovaloftheplate,dryinair,spraywith5%ferricchlorideinethanolacidifiedwithhydrochloricacidandheattothespotsclear.Thespotinthechromatogramobtainedwiththetestsolutioncorrespondsinpositionandcolourtothespotinthechromatogramobtainedwiththereferencesolution.(3)Pulverize10gofthepills,dissolveitwith100mlofwater,heattoboil,allowtostandforcool,filterinabsorbentcotton,washthefiltratewithtwo-30mlquantitiesofacetidin,combinethefiltrate,evaporatethefiltratetodryness,dissolvetheresiduein1mlofmethanolasthetestsolution.Prepareasolutionof4gofPreparedRehmanniaRootreferencedrugand60mlwater,decoct30minutes,standforcool,filterwithabsorbentcotton,washthefiltratewithtwo-20mlquantitiesofacetidin,combinethefiltrate,evaporatethefiltratetodryness,dissolvetheresiduein1mlofmethanolasthereferencesolution.Carryoutthemethodforthinlayerchromatography(AppendixⅥ),usingsilicagelGasthecoatingsubstanceandthelowerlayerofamixtureofchloroform,xyleneandacetidin(1:1),asthemobilephase.Applyseparately3-5μlofeachofthetwosolutiontotheplate.Afterdevelopingandremovaloftheplate,dryinair.Sparywith2,4-dimethylethanolnitriletospotsclear.Thespotinthechromatogramobtainedwiththetestsolutioncorrespondinpositionandcolourtothespotinthechromatogramobtainedwiththereferencesolutionandthereferencedrugsolution.(4)Pulverize5gofthepills,dissolveitwith30mlofwater,coolandfilter,washtheresiduewith30mlofwater,andheatunderrefluxtheresidue,with50mlof30%hydrochloricacidfor1hour,coolandfilter,washthefiltratewithtwo-25mlchloroform,evaporatethefiltratetodryness,dissolvetheresiduein1mlofchloroformasthesolution.Dissolvethe0.3gofRhizomaDioscoreaeOppositaedrugin50mlof30%hydrochloricacid,andmakethereferencesolutionasthesamewayabove.Carryoutthemethodforthinthinlayerchromatography(AppendixⅥB),usingsilicagelGasthecoatingsubstanceandmixtureofchloroformandacetone(9:1.5)asthemobilephase.Applyseparately5μlofeachofthetestsolutionandthereferencesolutiontotheplate.Afterthedevelopingandremovaltheplate,dryinair,examineundertheultravioletlightat365nm.Thefluorescentspotsinthechromatogramobtainedwiththetestsolutioncorrespondinpositionandcolourtothespotsobtainedwiththereferencedrugsolution.(5)Pulverize10gofthepills,dissolveitin100mlofwater,coolandfilterinabsorbentcotton,washtheresiduewith50mlofpetroleumether(60-90℃)third,evaporatethefiltratetodryness,dissolvetheresiduein1mlofpetroleumether(60-90℃)asthetestsolution.Decoctthe2gofRhizomaAlismatisdrugwith50mlofwater,coolandfilterinabsorbentcotton,andmakethereferencesolutionasthesamewayabove.Carryoutthemethodforthinlayerchromatography(AppendixⅥB),usingsilicagelGasthecoatingsubstanceandmixtureofpetroleumether,acetidinandchloroform(2:2:1)asthemobilephase.Applyseparately10-20μloftestsolutionand10μlofreferencedrugsolutiontotheplate.Afterdevelopingandremovaltheplate,dryinair.Sparywith5%phosphomolybdicacidinethanolandheatat110℃tothespotsclear.Thespotinthechromatogramobtainedwiththetestsolutioncorrespondinpositionandcolourtothespotsobtainedwiththereferencedrugsolution.(6)Pulverize10gofthepills,heatunderrefluxitwith50mlofether,coolandfilter,evaporatethefiltratetodryness,dissolvetheresidueinn-hexaneasthetestsolution.Heatunderreflux2gPoriawith30mletherfor1hour,filter,evaporatethefiltratetodryness,dissolvetheresidueinn-hexaneasthereferencedrugsolution.Carryoutthemethodforthinlayerchromatography(AppendixⅥB),usingsilicagelGasthecoatingsubstanceandmixtureofpetroleumether(60-90℃)andether(3:2)asthemobilephase.Applyseparately20μloftestsolutionand10μlofreferencedrugsolutiontotheplate.Afterdevelopingandremovaltheplate,dryinair,examineundertheultravioletlightat365nm.Thespotinthechromatogramobtainedinthetestsolutioncorr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