分析方法的建立ppt课件

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1、AnalyticalMethodDevelopmentandValidation分析方法的建立和验证28March2008Outline总纲HPLCMethodDevelopment高效液相方法建立HPLCTrouble-shootingGuideHPLC问题解答MethodOptimization方法优化MethodValidation方法验证SystemSuitabilityRequirements系统适应性要求GMP“Mind-set”GMP理念MethodDevelopment–MethodClassifi

2、cation方法开发－分析方法分类AssayMethod含量方法ImpurityProfile杂质情况-RelatedSubstances有关物质ChiralPurity手性纯度ContentUniformity含量均一性DissolutionCleaningValidation清洁验证Identity–Fingerprint鉴别－指纹法MethodDevelopment方法开发–UsefulInformation有用的信息ChemicalstructureandMW化学结构和分子量Solventsolubility

3、溶剂中的溶解度pKaandpHsolubility酸性解离常数和PH溶解度UVspectrum紫外光谱Processimpurities工艺杂质Possibledegradationimpurities可能的降解杂质LiteratureReferences参考文献MSDS–Materialsafetydatasheets安全数据表MethodDevelopment方法开发–ResourcePlanning&Gathering资源计划收集Solventsandreagents溶剂和试剂Placebomaterials安

4、慰剂Individualformulationcomponents各个处方成分Relatedsubstancestandards有关物质标准品APIReferenceStandards活性成分标准品Acceleratedstresssample强降解样品MethodDevelopment方法开发–HPLCColumn色谱柱Reversedphase:C18(USPL1),C8(L7)反相：C18(USPL1),C8(L7)Normalphase:Silica,CN,andNH2Silica,CN,andNH2Ion-

5、Exchange:Dionexcolumn离子交换：DionexcolumnIonpairChromatography:C18/C8/CN离子对色谱法：C18/C8/CNSizeExclusionChromatography排阻色谱法Chiralseparation手性分离MethodDevelopment–HPLCColumn(cont.)色谱柱ColumnDimension:柱子的尺寸4.6mmx25cm4.6mmx15cm4.6mmx10cmParticleDiameter:粒径10µm,5µm,3.5µm,

6、1.8µmPoresize,Surfacearea,Endcapping孔径，表面积，封尾MethodDevelopment方法开发–HPLCColumn色谱柱：考考你???ParticleSize粒径Length长度ExpectedN要求3.5µm5cm42003.5µm10cm???5µm25cm1200010µm25cm???ParticleSize粒径Length长度Resolution分离度3.5µm5cm1.53.5µm10cm???MethodDevelopment方法开发–HPLCColumn(con

7、t.)色谱柱GuardColumn预柱ColumnWash柱子冲洗ColumnTemperature(35˚C-60˚C)柱温（35˚C-60˚C）ColumnStorage柱子的储存MethodDevelopment方法开发–HPLCcolumnselectionsummary色谱柱选择：总结C18Column:firstchoiceC18柱：首选Shortlength:10cmor15cm短柱：10cmor15cmSmalldiameter:3.5µmor5µm小的粒径：3.5µmor5µmEnd-capped封

8、尾MethodDevelopment方法开发–HPLCMobilePhase流动相Strongsolventcomponent:强溶剂组份Methanol甲醇Acetonitrile乙腈Tetrahydrofuran四氢呋喃Weaksolventcomponent:弱溶剂组份Water水Buffer缓冲液Dilutedacid(0.1%H3PO