药科大学教案(药物分析试验首页1)

10中国药科大学教案 (药物分析试验首页1)课程名称 药物分析 总学分(时) 102其中:

理论51 选修课试验51 必教材名称药物分析试验与指导 杭太俊主编2023年1版试验一葡萄糖的性状、鉴别和检查教学目的1234、把握药品中一般杂质检查的方法原理和限量计算方法。本章讲授提纲及学时安排

教学对象

和临床药学方向专业【性状】本品为无色结晶或白色结晶性或颗粒性粉末；无臭，味甜。溶解性―――――――构造式分析〔60min〕比旋度测定 依中国药典2023年版二部附录ⅥE测定，比旋度为＋52.5°至＋53.0°。―――――旋光仪使用〔120min〕【鉴别】(1)碱性酒石酸铜试液，生成氧化亚铜的红色沉淀。――――――化学反响式〔60min〕【检查】――――――各检查的留意事项〔120min〕酸度20ml溶解，加酚酞指示液与氢氧化钠滴定液，应显粉红色。氯化物2023年版二部附录ⅧA6.0ml制成的比照液比较，不得更浓(0.01％)。重金属依中国药典2023年版二部附录ⅧH第一法检查，含重金属不得过百万分之五。砷盐2023年版二部附录ⅧJ第一法检查，应符合规定(0.0001％)。教学参考书2023年版二部本章内容的重点旋光仪的使用比色管的使用及清洗一般杂质限量的计算本章内容的难点古蔡氏试砷法中所加各试剂的作用与操作留意点复习思考题1?2?34?5教具及教学设备要求100ml容量瓶，10ml离心管，旋光仪，纳氏比色管，试砷瓶。Experiment1 TheDescription，IdentificationandTestsofGlucosePurposeTounderstandtheaimsandpurposesofthedrugqualitycontrol.Tolearnaboutthemethodsforthedeterminationandthespecialwordsforthedescriptionofthecharacteristicsofdrugs.Toexperimentontheidentificationofglucose.Tostudyandexperimentonthemethodsofdrugtests2.ContentsandteachtimeassignmentDescriptionColourlesscrystalsorawhitecrystallineorgranularpowder；odourless；taste,sweet.Dissolubility (60min)Specificopticalrotation Polarimeter (120min)Identification announcements (60min)Dissolveabout0.2gin5mlofwater，adddropwisehotalkalinecuprictartrateTS；aredprecipitateofcuprousoxideisproduced.examination (120min)AcidityDissolve2.0gin20mlofwater,add3dropsofphenolphthaleinISand0.20mlofsodiumhydroxide(0.02mol/L)VS;apinkcolourisproduced.ChlorideCarryoutthelimittestforchlorides(AppendixVIIIA)，using0.60g.Anyopalescenceproducedisnotmorepronouncedthanthatofareferenceusing6.0mlofsodiumchloridestandardsolution(0.01%).HeavymetalsDissolve4.0gin23mlofwater，add2mlofsodiumacetateBS(pH3.5)，carryoutthelimittestforheavymetals(AppendixVIIIH，method1):notmorethan0.0005%.Arsenic(AppendixVIIIJ，method1)(0.0001%).ReferencestheVolumn2ofChinesePharmacopoeiaFocalpointTheuseofPolarimeterHowtouseandclearthecolorcomparisontubeHowtofigureoutthelimitofarsenicorheavymatalsDiscussionWhatarethepurposesofdrugidentificationandtest?Whataretheusualitemsofdrugtests?.Whatarethestandardoperationproceduresfortheclaritytest?Howmuchoftheleadstandardsolutionshouldbetakenforthelimittestforheavymetalsinthisexperiment?Whatprecautionsshouldbetakenforthelimittestforarsenic(AppendixVIIIJ，method? Andwhatisthefunctionforeachofthetestsolutionsadded?Figureouttheamountofthearsenicstandardsolutionthatshouldbetakenforthelimittestforarsenic(AppendixVIIIJ，method1)(0.0001%)inthisexperimentwiththespecifiedquantityof2.0gofsample.teachingdevice100mlvolumetricflask;10mlcentrifugetube;polarimeter;colorcomparisontube;arsenictestbottle试验二阿司匹林及阿司匹林肠溶片的质量分析教学目的把握质量检验的工程与方法；把握阿司匹林及阿司匹林肠溶片分析的操作条件及要点。本章讲授提纲及学时安排【性状】本品为白色结晶或结晶性粉末；无臭或微带醋酸臭，味微酸；遇湿气即缓缓水解。溶解性―――――――构造式分析〔30min〕【鉴别】(1)0.1g10ml1滴，即显紫堇色。0.5g10ml2分钟后，放冷，加过量的稀硫酸，即析出白色沉淀，并发生醋酸的臭气。――――――化学反响式〔1hour〕【检查】――――――各检查的留意事项〔1hour〕溶液的澄清度0.50g4510ml溶解后，溶液应澄清。游离水杨酸制的稀硫酸铁铵溶液、硫酸铁铵指示液显色，与比照液(周密称取水杨酸配制)比较，不得更深(0.1％)。【含量测定】―――――――〔5.5hour〕原料中性乙醇溶解后，加酚酞指示液3滴，用氢氧化钠滴定液直接滴定。片剂两步滴定法。本课程学科的进展与理论课相结合，再复习阿司匹林的各种含量测定法，相关文献介绍。教学参考书2023年版二部本章内容的重点原料与片剂为何要用不同的测定含量方法本章内容的难点中性乙醇的制备，两步滴定法的操作留意点本章内容及讲授的改进意见复习思考题阿司匹林原料药物与及阿司匹林肠溶片在质量检验方面有哪些不同之处？为何不同？阿司匹林肠溶片释放度检查中为什么要更换溶剂？教具及教学设备要求50ml烧杯，10ml离心管，电炉，水浴锅，滴管，滴定管。Experiment2 TheAnalysisofAspirinandAspirinEnteric-coatedTabletsI.PurposeTolearnabouttheproceduresandtheitemsfordruganalysis.ToexperimentontheanalysisofAspirinanditsEnteric-coatedTablets.2.ContentsandteachtimeassignmentDescriptionDissolubility (30min)Identification announcements (1hour)Toabout0.1gadd10mlofwater，boilandcool.Add1dropofferricchlorideTS；avioletcolourisproduced.Toabout0.5gadd10mlofsodiumcarbonateTS，boilfor2minutesandcool.Adddilutesulfuricacidinexcess；awhiteprecipitateisproducedandanodourofaceticacidisperceptible.Examination (1hour)ClarityofsolutionSalicylicacidAssay (5.5hour)Material directtitrationusingsodiumhydroxideTablet two-steptitration.ReferencestheVolumn2ofChinesePharmacopoeiaFocalpointThepreparationofneutro-alcoholHowtooperatetow-steptitrationDiscussionWhatisthedifferencebetweentheassayofaspirinanditsenteric-coatedtablets?Giveanexplanationofthepurposeofthesolventchangingduringthedrugreleasetestofaspirinenteric-coatedtablets.teachingdevice50mlbeaker;10mlcentrifugetube.electricfurnace,thermostat-controlledwaterbath,volumeburet试验三复方磺胺甲噁唑片的质量分析教学目的生疏复方制剂双波长计算分光光度方法含量测定原理；把握复方磺胺甲噁唑片试验的操作条件及要点。本章讲授提纲及学时安排【性状】本品为白色片。标示量等特性――――〔20min〕【鉴别】(1取本品的细粉适量〔约相当于磺胺甲噁唑50m反响〔中国药典2023年版二部附录Ⅲ。(2取本品的细粉适量〔约相当于甲氧苄啶50m10m0.5ml，即生成棕褐色沉淀。――――――化学反响式〔1.5hour〕【含量测定】―――――――――――〔6hour〕磺胺甲噁唑照分光光度法〔中国药典2023年版二部附录ⅣA，以257nm长λ2，在304nm为参比波长λΔAAλ2-λ10λ2与λ1波特长分别测定供试品溶液的稀释液与比照品溶液(1)的稀释液的吸取度，求出各自的吸取度差值ΔA，计算，即得。甲氧苄啶照分光光度法〔中国药典2023年版二部附录ⅣA，以239nm为测定波长λ2，在295nm波长为参比波长λ1ΔAλ2λ10λ2与λ1波特长分别测定供试品溶液的稀释液与比照品溶液(2)的稀释液的吸取度，求出各自的吸取度差值ΔA，计算，即得。本课程学科的进展另有方法测定为HPLC。教学参考书2023年版二部本章内容的重点双波长测定法的原理本章内容的难点双波长测定法的原理复习思考题分别说明本品中磺胺甲噁唑和甲氧苄啶双波长法含量测定时波长选择的依据；为何甲氧苄啶含量测定时供试液的稀释倍数与磺胺甲噁唑测定时的要不同？教具及教学设备要求50ml烧杯，10ml离心管，研钵，电子天平，100ml容量瓶，50ml容量瓶，紫外分光光度仪，比色皿。Experiment3 TheAnalysisofCompoundSulfamethoxazoleTabletsI.PurposeTostudythespectro-photometricmethodforthesimultaneousdeterminationofdrugcomponentsincompoundformulation.To experiment on the assay of Compound Sulfamethoxazole Tablets by thespectro-photometricmethod.2.ContentsandteachtimeassignmentDescriptionWhitetablets (20min)Identification announcements (1.5hour)Yieldsthereactionscharacteristicofprimaryaromaticamines(AppendixIII)，usingaquantityofthepowderedtabletsequivalenttoabout50mgofSulfamethoxazole.Toaquantityofthepowderedtabletsequivalenttoabout50mgoftrimethoprimadd10mlofdilutesulfuricacid，heatgentlytodissolve，coolandfilter.Tothefiltrateadd0.5mlofiodineTS，adarkbrownprecipitateisproduced.Assay (6hour)Sulfamethoxazole

=257nm,=304nm,sothat A A=0.Measuretheabsorbanceof2 1 2 1dilutedtestsolutionandthatofdilutedreferencesolution(1)atwavelengthsand，calculate2 1thedifferenceinabsorbance(A)foreachsolutionandthecontentofCHNOS.10 11 3 3Trimethoprim

=239nm,=295nm,sothat A A =0.Measuretheabsorbanceof2 1 2 1dilutedtestsolutionandthatofdilutedreferencesolution(2)atwavelengthsand，calculate2 1thedifferenceinabsorbance(A)foreachsolutionandthecontentofCH NO.14 18 4 3ReferencestheVolumn2ofChinesePharmacopoeiaFocalpointTheprincipalofdualwavelengthassay.DiscussionGiveanexplanationofthebasisofthewavelengthselectionforthedeterminationofsulfamethoxazoleandtrimethoprim，respectively.Whyisthemoredilutedsolutionusedfortheassayoftrimethoprimthanthatforsulfamethoxazole?teachingdevice50mlbeaker;10mlcentrifugetubemortarelectronicbalance100mlvolumetricflask50mlvolumetricflaskUVspectrometer1cmcell试验四血浆中阿司匹林的高效液相色谱法测定教学目的了解生物样品测定的过程；把握阿司匹林血浆样品测定的方法和步骤。本章讲授提纲及学时安排1. 标准溶液―――――――――――――溶液配置〔60min〕阿司匹林标准溶液(100g/ml)：OOHO CHOOH3O邻甲基苯甲酸(内标)标准溶液(50g/ml)：OOHOOH32. 血浆样品处理――――――――――――〔1hour〕阿司匹林血浆样品处理0.5ml置1.5ml的离心管中，周密参与邻甲基苯甲酸标准溶液10l0.5mol/L0.1ml0.5ml，1分钟，415分钟后，412023rpm100.5ml，加氯0.1g5秒，410分钟后，12023rpm10分钟，分取上清液作为供试液。3.标准曲线――――――――――〔1hour〕将阿司匹林与内标邻甲基苯甲酸的峰面积比即得。阿司匹林血药浓度测定回收率和周密度试验――――――――――〔1hour〕阿司匹林血药浓度测定项下的条件分别测中、高浓度的回收率和周密度，应符合规定。阿司匹林血药浓度测定――――――――――〔3hour〕照高效液相色谱法(2023年版二部附录ⅤD)测定。测定法20l，注入液相色谱仪，记录色谱图，按内标法，以标准曲线进展计算即得。本课程学科的进展HPLC-MS的应用。教学参考书Analysisandbioanalysis本章内容的重点生物样品的处理方法本章内容的难点生物样品的处理过程本章内容及讲授的改进意见复习思考题12、阿司匹林标准溶液在4℃贮存的目的是什么？为什么冰冻的阿司匹林血浆样品在冰水浴中解冻？30.5mol/L0.1ml的目的是什么？4、试验中添加内标物邻甲基苯甲酸的目的是什么？回收率试验的目的和意义是什么？教具及教学设备要求50ml烧杯，10ml离心管，电子天平，100ml容量瓶，移液器，离心机，水浴锅，高效液相色谱仪Experiment4 Determinationofaspirin(ASA)inhumanplasmabyHPLCPurposeTolearnabouttheprinciplesandproceduresforthedeterminationofdrugsinbiologicalsamples.Toexperimentonthedeterminationofaspirininhumanplasma.ContentsandteachtimeassignmentStandardsolutions (60min)O O OCH3 11O12O 2-methylbenzoicacid(internalstandard)(MBA，50μO CH3Samplepreparation (1hour)Aspirinplasmasamplepreparation Thawthefrozenplasmasampleinanice-waterbath.Transferaccurately0.5mlofittoa1.5mlmicrocentrifugetubeandaddaccurately10μlofMBAstandardsolution.Thenadd0.1mlof0.5mol/Lhydrochloricacidand0.5mlofacetonitrile.Vortexthemixturefor1minuteandkeepat4℃for15minutes.Thencentrifugeat12023rpmfor10minat4℃.To0.5mlofthesupernatantadd0.1gofsodiumchlorideandvortexfor5sandplacedat4℃for10minbeforecentrifugeat12，000rpmfor10minat4℃.Usethesupernatantforthedeterminationofaspirin.Calibrationcurve (1hour)Establishthecalibrationcurvebyplottingthepeak-arearatiosofASAtointernalstandardversusitsconcentrations.RecoveryandprecisionforASAdetermination (1hour)Thenmakethedeterminationaccordingtotheproceduresdescribedunderthe‘determinationofASAinhumanplasma’.Themeanrecoveryandprecisionofdifferentconcentrations，calculatedbycomparisonofthepeak-arearatiosofASAtoMBAinthetestsolutionswiththoseofstandardsatthesameconcentration，mustcomplywiththerequirements.DeterminationofAspirininhumanplasma 3(hour)DeterminationInject20μlofASAplasmasampleintothecolumn，andrecordthechromatogram.CalculatetheASAconcentrationintheplasmawithrespecttothepeakarearatiosobtainedinthechromatogrambytheinternalstandardmethodaccordingtothecalibrationcurve.ReferencesAnalysisandbioanalysisFocalpointThepretreatmethodofbiologicalspecimen.DiscussionWattemethodusedfortheeliminationoftheplasmaproteininterferencesinthisanalysis?Whatotherusualmethodsaretherefortheeliminationoftheplasmaproteininterferences? Whataretherespectivecharacteristicsofthem?WhatarethepurposestokeeptheASAstandardsolutionat4℃?Whyshouldthefrozenplasmasamplesbethawedintheice-waterbath?Whataretheaimsofadding0.1mlof0.5ml/Lhydrochloricacidduringthesamplepreparation?WhyshouldtheMBAbeaddedastheinternalstandardinthetest?Whataretheaimsandsignificancesoftherecoverytest?teachingdevice50mlbeaker;10mlcentrifugetubeelectronicbalance100mlvolumetricflasktransferpettorcentrifugalmachinethermostat-controlledwater-bathhighperformancechromatographofliquid试验五维生素E胶丸的含量测定教学目的把握气相色谱法测定的原理与方法；把握维生素E含量的操作条件及要点。本章讲授提纲及学时安排【性状】―――――――――――――〔30min〕本品为微黄色或黄色透亮的黏稠液体；几乎无臭；遇光色渐变深。本品在无水乙醇、丙酮、乙醚或石油醚中易溶，在水中不溶。【含量测定】―――――――――――――〔7.5hour〕取装量差异项下的内容物，混合均匀，周密称取适量〔E20m色具塞锥形瓶中，照维生素E项下的方法，周密参与内标溶液10ml，密塞，摇匀，取1～3μl注入气相色谱仪，并依法测定校正因子，计算，即得。照气相色谱法(2023年版二部附录ⅤE)测定。色谱条件与系统适用性试验(OV-17226理论板数按维生素E500，维生素E峰与内标物质峰的分别度应大于2。校正因子测定取正三十二烷适量，制备内标溶液。另取维生素E比照品制备比照品10ml1～3μl注入气相色谱仪，计算校正因子。本课程学科的进展GC的应用。教学参考书JournalofChromatographyA本章内容的重点气相色谱仪的使用本章内容的难点气相色谱仪的使用本章内容及讲授的改进意见复习思考题1E含量时为什么使用内标法？23、维生素E含量测定的其它方法有哪些？各有什么特点？教具及教学设备要求具塞锥形瓶，电子天平，10ml容量瓶，气相色谱仪Experiment5 TheAssayofVitaminEPurposeTostudytheprinciplesandproceduresofgaschromatographyfortheassayofvolatiledrugs.ToexperimentontheassayofVitaminE.ContentsandteachtimeassignmentDescription (30min)Aclearpaleyelloworyellowviscous，oilyliquid；almostodourless；thecolurdeepensonexposuretolight.Freelysolubleindehydratedethanol，acetone，etherorpetroleumether；insolubleinwater.Assay (7.5hour)MixwellthecontentsobtainedinthetestforWeightvariation.Toaquantity，accuratelyweighed，ofthemixedcontentsequivalentto20mgofvitaminEadd10ml，accuratelymeasured，ofinternalstandardsolutioninanambercolouredflaskstoppered，shakewell.CarryouttheAssaydescribedundervitaminE，injecting1~3lofthesolutionintothecolumnanddeterminethecorrectionfactoraccordingly.CalculatethecontentofCH O.31 52 3Carryoutthemethodforgaschromatography(AppendixVE，method3)，usingacolumnpackedwith2%silicone(OV-17)asthestationaryphaseandmaintainthecolumntemperatureat265℃.Thenumberoftheoreticalplatesofthecolumnisnotlessthan500，calculatedwithreferencetothepeakofvitaminE，andtheresolutionfactorbetweenthepeaksofvitaminEandinternalstandardisnotlessthan2.Dissolveaquantityofdotriacontaneinn-hexanetoproduceasolutionof1.0mgpermlastheinternalstandardsolution.To20mgofvitaminECRS，accuratelyweighed，inanambercolouredflaskwithstopper，add10mlofinternalstandardsolution，accuratelymeasured，stoppertheflask，shakewell.Inject1~3lintothecolumnandcalculatethecorrectionfactor.ReferencesJournalofChromatographyAFocalpointTheuseofgaschromatograph.DiscussionWhyistheinternalreferencestandardmethodemployedfortheassayofVitaminEbyGC?GiveanexplanationofthefeaturesandapplicationsofGCmethod?WhatothermethodsaretherefortheassayofVitaminE?teachingdeviceconicalflaskelectronicbalance10mlvolumetricflaskgaschromatograph试验六醋酸氢化可的松中其他甾体的检查双黄连口服液的质量检验教学目的了解甾体激素类药物中有关物质的来源和检查的意义。把握醋酸氢化可的松的有关物质检查方法。把握中成药特征成分的薄层比照品法及比照药材法的鉴别；本章讲授提纲及学时安排一、醋酸氢化可的松中其他甾体的检查本品为11，17α，21-三羟基孕甾-4-烯-3，20-三酮21-醋酸酯。按枯燥品计算，含C H O应为97.0%～102.0％。23 32 6【性状】本品为白色或几乎白色的结晶性粉末；无臭。本品在乙醇或氯仿中微溶，在水中不溶。【检查】―――――――――――――――〔2hour〕其他甾体自身比照法，照薄层色谱法(2023年版二部附录ⅤB)试验，喷以碱性四氮唑蓝试液，马上检视。二、双黄连口服液的质量检验【处方】金银花375g 黄芩375g 连翘750g【性状】本品为棕红色的澄清液体；味甜，微苦。【鉴别】薄层色谱法(1)金银花、黄芩比照品法―――――――――――――〔2hour〕(2)连翘比照药材法―――――――――――――〔2hour〕本课程学科的进展TLC的应用。教学参考书JournalofChromatographyA本章内容的重点TLC点样碱性四氮唑蓝显色本章内容的难点TLC点样碱性四氮唑蓝显色本章内容及讲授的改进意见复习思考题甾体激素中“其它甾体”检查的意义和常用方法是什么？哪类甾体激素可与四氮唑蓝产生反响，是构造中的何种基团参与了反响，反响式是什么？在中成药及中药材的薄层色谱鉴别中何时承受比照药材法？教具及教学设备要求薄层板，点样毛细管，10ml容量瓶，5ml容量瓶，喷瓶，紫外光灯，水浴锅，回流管，圆底烧瓶Experiment6TestsofHydrocortisoneAcetateorHydrocortisoneAcetateTheAnalysisofShuanghuanglianKoufuyeI.PurposeTostudytheoriginsoftherelatedcompoundsofsteroidaldrugsandthesignificanceofthelimittestsforthem.Toexperimentonthelimittestfortherelatedcompoundsofhydrocortisoneacetate.TostudythemethodfortheidentificationoftraditionalChinesemateriamedicawithreferencetoCRSorreferencedrug.2.Contentsandteachtimeassignment1、HydrocortisoneAcetateHydrocortisoneAcetateis11，17，21-trihydroxypregn-4-ene-3，20-dione-21-acetate.Itcontainsnotlessthan97.0%andnotmorethan102.0%ofCH O，calculatedonthedriedbasis.

23 32 6DescriptionAwhiteoralmostwhitecrystallinepowder；odourless.Slightlysolubleinethanolorchloroform；insolubleinwater.OthersteroidsCarryoutthemethodforthin-layerchromatography(AppendixVB) (2hour)2、ShuanghuanglianKoufuyeIngredientsFlosLonicerae375g；Radixscutellariae375g；FructusForsythiae750g.DescriptionAclear，brownish-redliquid；taste，sweetandslightlybitter.Identificationfloslonicerae,scutellaria (2hour)forsythiasuspensabyreferencedrug (2hour)ReferencesJournalofChromatographyAFocalpointThespottingofTLCTheuseoftetrazoliumDiscussionWhatarethecommonlyusedmethodforandthesignificanceofthelimittestforothersteroidsforthesteroidaldrugs?WhatkindofsteroidaldrugscanreactwiththealkalinetetrazoliumblueTS? Whatisthechemicalreactionequation?WhenshouldthereferencedrugbeusedfortheidentificationoftraditionalChinesemateriamedica?teachingdevicethinlayerplate,spottingcapillary,10mlvolum