资源描述:
《二至丸的定性定量测定.doc》由会员上传分享,免费在线阅读,更多相关内容在教育资源-天天文库。
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