二至丸的定性定量测定.doc

二至丸的定性定量测定.doc

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1、ThequalitativeanalysisandquantitativeanalysisofErzhipillPurpose1.TomasterthequalitativeanalysisofcomposingdrugsofChinesetraditionalpatentmedicinebythinlayerchromatogram.2.TograsptheapplicationofhighperformanceliquidchromatograminquantitativeanalysisoftraditionalCh

2、inesepatentmedicine.Part1.QualitativeAnalysisCondition1.Apparatus:Ultrasoniccleaner,ultraviolateanalyzer2.Reagents:Erzhipill,diethylether,ethyl,OleanolicacidCRS,ethanol,chloroform,methanol,phosphomolybdicacid,andetc.Procedure1.Preparationofthetestsolutionandtheref

3、erencesolutionTo0.5gofthepowderadd30mlofdiethylether,heatunderrefluxfor40mins,andfilter.Evaporatethefiltratetodryness,anddissolvetheresiduein1mlofethylasthetestsolution.DissolveOleanolicacidCRSinethylalcoholtoprepareasolutioncontaining1mgpermlasthereferencesolutio

4、n.2.TLCprocedureCarryoutthemethodforthinlayerchromatography,usingsilicagelGasthecoatingsubstanceandchloroformandmethanol(40:1)asthemobilephase.Applyseparately5μlofeachofthetwosolutionstotheplate.Afterdevelopingandremovaloftheplate,dryinair,spraywithphosphomolybdic

5、acidandheattothespotsclear.ChinesePharmacopoeia2010Part2.QuantitativeAnalysisCondition1.Apparatus:Ultrasoniccleaner2.Reagents:Erzhipill,methanol,specnuezhenideCRS,wedelolactoneCRS,acetonitrileand0.1%phosphoricacidsolutionandetc.Procedure1.Preparationofthereference

6、solutionThereferencesolutionispreparedbydissolvingaquantityofspecnuezhenideCRSandwedelolactoneCRSinmethanoltoproduceasolution.ThecontentofspecnuezhenideCRSis0.8mg/ml.ThecontentofwedelolactoneCRSis0.1mg/mg.2.Preparationofthetestsolution1.0gofthesampleisweighedandco

7、ntainedina25mlvolumetricflask.Addaccurately20mlofmethanoltotheflask,extractfor45minsinanultrasoniccleaner.Afterthat,takeitoutandallowittocool.Addmethanoltothemaskofthevolumetricflask.Shakeitwellandfilter.Afterfiltration,thesuccessivefiltratewasfurtherfilteredwithM

8、illiporemembrane(particlesize1.45μm).thus,thesuccessivefiltrateisusedasthetestsolution.1.QuantitativeanalysisconditionsColumn:DIKMAC18(4.6mm×200mm,5μm)M

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