（精选课件）中国药典四部色谱法概况

中国药典2015年版四部色谱法概述,1,BEAConfidential.|2,主要内容,2015年版药典四部色谱法目录及修订情况色谱法的基本概念色谱法在中国药典中的沿革中国药典2015年版色谱法内容概况,2015版四部色谱法目录,3,BEAConfidential.|4,色谱法的基本概念,色谱法是利用混合物中各组分的理化性质的差异(吸附力、溶解度、分子形状和大小、分子极性、分子亲和力等)，使各组分以不同程度分布在两个相中，其中一个相叫固定相，另一相流过此固定相叫作流动相。由于各组分受流动相作用产生的推力和受固定相作用产生的阻力的不同，使各组分产生不同的移动速度，使得结构上只有微小差异的各组分得到分离。再配合相应的光学、电学、电化学和或其他相关检测手段，对各组分进行定性和定量分析的方法。,5,色谱法的分类,6,色谱法的基本概念,分离原理吸附色谱法分配色谱法离子交换色谱法排阻色谱法,分离方法纸色谱法薄层色谱法柱色谱法高效液相色谱法气相色谱法,7,色谱法在中国药典中的沿革,纸色谱法(1985)薄层色谱法(1985)柱色谱法(1985)高效液相色谱法(1985)气相色谱法(1985)电泳法(1990)毛细管电泳法(2000)分子排阻色谱法(2000)离子色谱法(2010)超临界流体色谱法（2015）临界点色谱法（2015）,8,0501纸色谱法,系以纸为载体，纸上所含水分或其他物质为固定相，用展开剂进行展开的分配色谱,鉴别纯度检查含量测定,9,0501纸色谱法,二部P1000页,10,0502薄层色谱法,薄层色谱法系将供试品溶液点于薄层板上，在展开容器内用展开剂展开，使供试品所含成分分离，所得色谱图与适宜的标准物质按同法所得的色谱图对比，亦可用薄层色谱扫描仪进行扫描，用于鉴别、检査或含量测定,将旧版药典“对照物”修订为“对照标准物质”,11,0502薄层色谱法,新版药典规范了市售薄层板的要求：市售薄层板按固定相种类分为硅胶薄层板、聚酰胺薄层板、氧化铝薄层板等；按固定相粒径大小分为普通薄层板（1040um）和高效薄层板（510um）；按硅胶板是否含有荧光剂分为硅胶G板和硅胶GF254板。操作方法:点样点直径限值由3mm修改为4mm。其他变化：基本整合旧版药典一部和二部。,12,0502薄层色谱法,仪器与材料薄层板点样器展开容器显色剂显色装置检视装置薄层扫描仪,13,0502薄层色谱法,操作方法薄层板制备点样展开显色与检视记录,14,0502薄层色谱法,操作方法薄层板制备（1）市售薄层板除聚酰胺薄膜外，110活化30分钟；如被空气杂质污染，可以用溶剂预洗（2）自制薄层板,15,0502薄层色谱法,操作方法点样在洁净干燥的环境中用专用毛细管或配合相应的半自动、自动点样器械点样于薄层板上一般为圆点状或窄细的条带状点样基线距底边1015mm，高效板一般基线离底边810mm。圆点状直径一般不大于4mm，高效板一般不大于2mm；条带状宽度一般为510mm，高效板条带宽度一般为48mm。点间距离可视斑点扩散情况以相邻斑点互不干扰为宜，一般不少于8mm，高效板供试品间隔不少于5mm,16,0502薄层色谱法,展开,示意图,高效板上行一般为58cm,17,0502薄层色谱法,操作方法显示与检视有颜色的物质直接可见光下检视无色物质可用喷雾和浸渍以适宜的显色剂显色，或者加热显色紫外荧光下显色（254nm和365nm）在紫外光下有吸收的成分，可用GF254板（带荧光剂），观察淬灭形成的斑点,18,0502薄层色谱法,操作方法记录摄像设备拍摄，记录光学照片或电子图像薄层扫描仪扫描仪扫描或其他方式记录色谱图,19,0502薄层色谱法,系统适用试验要求（1）比移值,Rf=0.20.8,20,0502薄层色谱法,系统适用试验要求按各品种项下要求对实验条件进行系统适用性试验，即用供试品和标准物质对实验条件进行试验和调整，应符合规定的要求。,21,Rf=0.20.8,0502薄层色谱法,（1）比移值,22,0502薄层色谱法,（2）检出限,指限量检査或杂质检査时，供试品溶液中被测物质能被检出的最低浓度或量。一般采用已知浓度的供试品溶液或对照标准溶液，与稀释若干倍的自身对照标准溶液在规定的色谱条件下，在同一薄层板上点样、展开、检视，后者显清晰可辨斑点的浓度或量作为检出限。,23,0502薄层色谱法,（3）分离度（分离效能）,供试品与对照标准物质色谱中斑点均应清晰分离薄层扫描法用于限量检查和含量测定时，R1.0,24,0502薄层色谱法,（4）相对标准偏差,（薄层扫描要求）同板同供试液（不显色）：RSD5.0%同板同供试液（显色）：RSD10.0%不同板同供试液（显色和不显色）：RSD10.0%,25,0502薄层色谱法,测定法,鉴别：供试品与对照标准物质斑点颜色和比移值一限量检查与杂质检查：半定量颜色（峰面积）：供试品杂质斑点“SlideTransition”,BEAConfidential.|113,SlideAnimationGuidelines,Thepurposeofslideanimationandbuildsistoenhancethemessage,notdetractfromitBecauseofthis,itisimportanttouseslideanimationsparinglyandonlywhennecessaryToadjusttheslideanimations,select“CustomAnimation”undertheTaskPaneUse“Appear”optionfortheanimation,BEAConfidential.|114,SettingBlackandWhitePrintingPreferences,Tosettheblackandwhiteprintingpreferences:SelectgrayscaleorpureblackandwhiteviewViewColor/GrayscaleGrayscaleThiswilldisplaytheslideingrayscalemodeandwillallowyoutoseehowtheslidewillprintClickonaslideobjectandselectGrayscaleSettingfromthemenuYouwillseealistingofoptionstochoosefromAutomaticisthedefaultandisacceptableExperimentwithalternateGrayscalesettingstoensureoptimumprintingSelectViewColor/GrayscaleColortoreturntothecolorslidemode,Continuedonslide15,BEAConfidential.|115,SettingBlackandWhitePrintingPreferences(Cont.),Ifyouareusingtransparency(forhighlights,etc.),youwillneedtoturntheblackandwhiteprintingsettingsto“dontshow”Tosettheblackandwhiteprintingsettingsto“dontshow”SelectViewColor/GrayscaleGrayscaleRight-clickonthetransparentobjectSelectGrayscaleSettingDontShowThehighlightboxbelowisincludedasanexampleofanobjectwithproperlysetblackandwhiteprintingsettings,ThisprocessaccommodatesforaprintingbugwithinPowerPointapplication,BEAConfidential.|116,SavingThisTemplateasYourDefaultDesignTemplate,OpentheBEACorporateTemplateGototheFilemenuandselect“Saveas”AtthebottomoftheSaveAsdialogbox,click“Saveastype,”andchoose“DesignTemplate”Inthe“Filename”box,typetheword“Blank”Click“Save”Thefilewillbesavedas“Blank.pot,”whichPowerPointrecognizesasadefaulttemplatefile,BEAConfidential.|117,ApplyingtheCorporateTemplateSlideDesigntoanExistingPresentation,Openanexistingpresentation,selectallslidesfromtheslidesorterviewandselectEditCopyOpenacopyofthenewBEAtemplateand“paste”theslidesintotheslidesorterviewA“pasteoptions”clipboardiconwillappearRollyourmouseovertheiconandfollowthedownarrowSelect“Usedesigntemplateformatting”SelecteachslideandapplyadesigntemplateRight-clickonslidesintheslidesorterviewandselect“SlideDesign”IntheSlideDesignpane,rollyourmouseovertheBEAstyleyouwanttoapply,clickthearrowinsidethethumbnailandselect“applytoselectedslides”,Continuedonslide18,BEAConfidential.|118,ApplyingtheCorporateTemplateSlideDesigntoanExistingPresentation(Cont.),Next,eachslidewillneedtohavetheappropriateslidelayoutappliedRight-clickonslidesintheslidesorterviewandselect“SlideLayout”IntheSlideLayoutpane,mouseoverthedesiredlayoutthumbnailandselect“applytoselectedslides”GraphicelementsontheslidesmayneedtobeadjustedtoreflectthenewcolorpaletteSomeslideelementswillneedlayoutadjustmentstoconformtothenewtemplatedesign,BEAConfidential.|119,ImportingSlidesfromAnotherPresentation,OpenthepresentationyouareconvertingandacopyoftheBEAtemplateinSlideSorterViewSelecttheslide(s)youwouldliketoimport,andchooseEditCopySelecttheBEACorporatetemplateSelecttheslideyouwanttheimportedslide(s)tofollow,andchooseEditPasteTheimportedslidesshouldtakeontheBEAtemplateEnsureeachslidehastheappropriateslidelayoutappliedRight-clickonslidesintheslidesorterviewandselect“SlideLayout”IntheSlideLayoutpane,mouseoverthedesiredlayoutthumbnailandselect“applytoselectedslides”,BEAConfidential.|120,“Usethisformatforquotes.Textsizeshouldbeaminimumof22pt.andcanbeaslargeas32pt.Textshouldnotbecenteraligned.Pleasedonotresizethegrayboxaroundthequote.”-SourceName,QuoteSlide,ColorPaletteandSampleCharts,121,BEAConfidential.|122,ColorPalette,BEAConfidential.|123,FlowDiagramUsingCorporateColors,Step1,Step2,Step3,SupportingbulletcopyhereSupportingbulletcopyhere,SupportingbulletcopyhereSupportingbulletcopyhereSupportingbulletcopyhere,SupportingbulletcopyhereSupportingbulletcopyhere,BEAConfidential.|124,SampleBarChart,Instructions:Thecolorpalettehasbeensetinthischart.Tocreateanewchart,copythischartontoyourslide.Toupdatethedata,double-clickonthecharttobringupthePPTcharteditor.ForadditionalinformationonworkingwiththePPTchartingfeature,followthislink,BEAConfidential.|125,SamplePieChart,Instructions:Thecolorpalettehasbeensetinthischart.Tocreateanewchart,copythischartontoyourslideandupdatethedatatosuityourneeds,BEAConfidential.|126,Instructions:ThistablewascreatedusingPowerPointsbuilt-intableprogram.Thetablewilldynamicallyadjusttothecontent.Toenteroreditthedata,simplyclickonthetable.Keepformatcolorsasis.,SampleTableSlide,BEAConfidential.|127,SampleTableSlideWithHighlight,BEAConfidential.|128,SampleTableSlideWithBulletText,BEAConfidential.|129,AlternativeAgendaSlide,StandardBoxes,Arrows,andShapes,130,BEAConfidential.|131,StandardArrowStyles,BEAConfidential.|132,StandardBlueBoxStyles,Boxw/Shadow,BEAConfidential.|133,StandardGreenBoxStyles,Boxw/Shadow,BEAConfidential.|134,StandardPurpleBoxStyles,Boxw/Shadow,BEAConfidential.|135,StandardGrayBoxStyles,Boxw/Shadow,BEAConfidential.|136,ExampleofaDiagram,ServiceInfrastructure,ServicesManagement,ServiceBus,CommonServices,InformationAccessServices,PresentationServices,SharedBusinessServices,CompositeApplications,BEAConfidential.|137,Photography,UseofphotographyshouldbeminimalNevermix-and-matchblackandwhiteandcolorimagesonthesamepageNeveruseclipartAdefinedcollectionofstockphotographyisavailableatRightclickontheURL,selectOpenHyperlinktoopenthePhotoLibraryinthebrowserBecauseLiquidnaturallycallstomindstrongvisualimagery,theremightbeadesiretousedifferenttypesofwaterimagery(e.g.,waves,rivers,waterfalls,droplets,etc.).However,inordertomaintainaconsistentlook-and-feel,werecommendnotusingthistypeofimagery,BEAConfidential.|138,ExampleUseofPhotography,BEAConfidential.|139,ExampleUseofPhotography,SpecialNeeds,140,RemovetheLiquidBackgroundforSlidesWithLargeGraphics,Applications,ServicesCatalog,ServiceInfrastructure,Servic