二至丸的定性定量测定

ThequalitativeanalysisandquantitativeanalysisofErzhipillPurpose1.TomasterthequalitativeanalysisofcomposingdrugsofChinesetraditionalpatentmedicinebythinlayerchromatogram.2.TograsptheapplicationofhighperformanceliquidchromatograminquantitativeanalysisoftraditionalChinesepatentmedicine.Part1.QualitativeAnalysisCondition1.Apparatus:Ultrasoniccleaner,ultraviolateanalyzer2.Reagents:Erzhipill,diethylether,ethyl,OleanolicacidCRS,ethanol,chloroform,methanol,phosphomolybdicacid,andetc.Procedure1.PreparationofthetestsolutionandthereferencesolutionTo0.5gofthepowderadd30mlofdiethylether,heatunderrefluxfor40mins,andfilter.Evaporatethefiltratetodryness,anddissolvetheresiduein1mlofethylasthetestsolution.DissolveOleanolicacidCRSinethylalcoholtoprepareasolutioncontaining1mgpermlasthereferencesolution.2.TLCprocedureCarryoutthemethodforthinlayerchromatography,usingsilicagelGasthecoatingsubstanceandchloroformandmethanol(40:1)asthemobilephase.Applyseparately5μlofeachofthetwosolutionstotheplate.Afterdevelopingandremovaloftheplate,dryinair,spraywithphosphomolybdicacidandheattothespotsclear.①Part2.QuantitativeAnalysisCondition1.Apparatus:Ultrasoniccleaner2.Reagents:Erzhipill,methanol,specnuezhenideCRS,wedelolactoneCRS,acetonitrileand0.1%phosphoricacidsolutionandetc.Procedure1.PreparationofthereferencesolutionThereferencesolutionispreparedbydissolvingaquantityofspecnuezhenideCRSandwedelolactoneCRSinmethanoltoproduceasolution.ThecontentofspecnuezhenideCRSis0.8mg/ml.ThecontentofwedelolactoneCRSis0.1mg/mg.2.Preparationofthetestsolution1.0gofthesampleisweighedandcontainedina25mlvolumetricflask.Addaccurately20mlofmethanoltotheflask,extractfor45minsinanultrasoniccleaner.Afterthat,takeitoutandallowittocool.Addmethanoltothemaskofthevolumetricflask.Shakeitwellandfilter.Afterfiltration,thesuccessivefiltratewasfurtherfilteredwithMilliporemembrane(particlesize1.45μm).thus,thesuccessivefiltrateisusedasthetestsolution.3.QuantitativeanalysisconditionsColumn:DIKMAC18(4.6mm×200mm，5μm)Mobilephase:acetonitrileand0.1%phosphoricacidsolutionFlowrate:0.1ml/minWavelengthofdetector:215nm②4.20μloftestsolutionisinjectedaccuratelyintothecolumn,andthecontentofthesampleisdeterminedaccordingtoonepointexternalstandardmethod.①ChinesePharmacopoeia2010②HEMu,YAOWeifeng,ZHANGLi,DINGAnwei,SimultaneousdeterminationoffourcompoundsinErzhiwanbyHPLC,ChinajournalofChineseMateriaMedica,Vol.37，Issue5March，2012