2023學(xué)年完整公開課版Introductiontopharmaceuticaliden

PharmaceuticalanalysisIntroductiontopharmaceuticalidentificationtechnologyIntroductiontopharmaceuticalidentificationtechnologyKeyanddifficultpointsMasterUnderstandItemsrequiringpharmaceuticalidentificationandcommonmethodsusedinpharmaceuticalidentification;Selectionprincipleofpharmaceuticalidentificationmethods;1.Overview(1)PharmaceuticalidentificationItistoprovetheauthenticityofknowndrugsbychemical,physicochemicalorbiologicalmethodsaccordingtothecomposition,structureandphysicalandchemicalpropertiesofdrugs.Itisnottocarryoutqualitativeanalysisonunknowndrugs.Itistheprimarytaskofdruginspectionandthepremiseofimpurityinspectionandcontentdetermination.2.Identifieditems(1)Property(2)Generalidentificationtest(3)Specificidentificationtest2.Identifieditems(1)PropertyAppearance:Sensoryevaluation,belongingtogeneraldescription.Solubility:Reflectthesolubilityinsomesolvent.Physicalconstant:Importantindicatorsevaluatingthedrugquality,reflectingthedegreeofdrugpurity.Meltingpoint,specificrotation,absorptioncoefficient,relativedensity,distillationrange,freezingpoint,refractiveindex,viscosity,acidvalue,saponificationvalue,iodinevalue,etc.2.Identifieditems(1)PropertyAppearance:Refertothephysicalsenseandcolorofdrugs,includingstateofaggregation,crystalstructure,color,odorandtasteE.g.VitaminB1"Itiswhitecrystalorcrystallinepowder;

withfaintodorandbittertaste;

DriedvitaminB1canimmediatelyabsorbabout4%ofthemoistureintheair"(Color)(Stateofaggregation)(Odor)(Taste)2.Identifieditems(1)PropertySolubility:Physicalpropertyofdrugs,reflectingthedrugpuritytoacertainextentVerysoluble:Refertothat1g(ml)ofsolutecandissolveinlessthan1mlofsolvent;Freelysoluble:Refertothat1g(ml)ofsolutecandissolvein1~10mlofsolvent;Soluble:Refertothat1g(ml)ofsolutecandissolvein10~30mlofsolvent;Sparinglysoluble:Refertothat1g(ml)ofsolutecandissolvein30~100mlofsolvent;Slightlysoluble:Refertothat1g(ml)ofsolutecandissolvein100~1,000mlofsolvent;Veryslightlysoluble:Refertothat1g(ml)ofsolutecandissolvein1000~10,000mlofsolvent;Practicallyinsolubleorinsoluble:Refertothat1g(ml)ofsolutecannotdissolvein10,000mlofsolvent;2.Identifieditems(1)PropertySolubilitytestmethod①Accuratelyweighandgrindthetestedproductintofinepowder②Addsolventat25℃±2℃③Shakeitfor30severy5min

Whentherearenovisiblesoluteparticlesordropletswithin30min,itisconsideredtobecompletelydissolved

2.Identifieditems(1)PropertyMeltingpoint1)Definition:AccordingtoCh.P,themeltingpointreferstothetemperatureatwhichasubstancemeltsfromsolidphasetoliquidphase,thetemperatureatwhichitdecomposesatthesametimeofmelting,orthetemperaturefromincipientmeltingtodeadmeltingduringmelting.E.g.Estradiol:175~180℃Dexamethasoneacetate:223~233℃

TheSample

CoarseningContractingDroplet(Incipientmelting)Clarified(Deadmelting)2.Identifieditems2)DeterminationmethodMethod1:DeterminesoliddrugsthatcanbeeasilycrushedMethod2:Determinesoliddrugsthatcannotbeeasilycrushed(suchasfat,fattyacid,paraffin,lanolin,etc)Method3:Determinevaselineorothersimilarsubstances2.Identifieditems(1)Property-physicalconstantSpecificrotation:Whenpolarizedlightpassesthroughthesolutionwithalengthof1dmandcontaining1gofopticallyactivesubstanceper1ml,itsopticalrotationmeasuredatcertainwavelengthandtemperatureiscalledspecificrotation. Ifthepolarizedlightrotatestotheright(clockwise),itiscalledright-handedrotation,whichisrepresentedby"+"; Ifthepolarizedlightrotatestotheleft(anticlockwise),itiscalledleft-handedrotation,whichisrepresentedby"-";[α]isspecificrotation;DislineDinsodiumspectrum(589.3nm),tisthetemperaturefordetermination,whichisspecifiedas20℃;αisthespecificrotationmeasuredinthetest;Cisthepercentageconcentrationoftestedproduct(g/100ml);listhelengthofdeterminationtube(dm);2.IdentifieditemsFactorsaffectingthedeterminationofopticalrotation:(1)Chemicalstructureofdrugs(2)Concentrationofsolution(3)Solvent(4)Thicknessofliquidlayerwherelightpassesthrough(5)Wavelengthoflight(6)Temperature2.IdentifieditemsItistoidentifytheauthenticityofmedicinesthroughchemicalreactionaccordingtothecommonchemicalstructureorthesamephysicalandchemicalpropertiesofacertaincategoryofmedicines.Organicdrugs-functionalgroupInorganicdrugs-anionandcationGeneralidentificationtestcanbeonlyusedtoconfirmwhichcategorythedrugbelongsto.Tofurtherconfirmwhichkindthedrugis,itisnecessarytocarryoutspecificidentificationtest.(2)Generalidentificationtest2.IdentifieditemsOrganicfluorine,organicacidsalt(salicylate),aromaticprimaryamine,tropanealkaloidandmalonylureaOrganicmetals(Na+,K+,Ca2+,Ba2+,Li+,Fe3+,Al3+,Zn2+,Cu2+,Ag+,Hg2+,etc.)Inorganicacidsalts(Cl-、SO42-、NO3-)(2)Generalidentificationtest2.Identifieditems(2)Generalidentificationtest-organicfluorideOrganicfluorineOxygenflaskcombustionInorganicfluorideionpH4.3AlizarinfluorineblueCeriumnitrateBluishvioletcomplex+F-+Ce3+

pH4.3Alkaliabsorptionmethod2.Identifieditems(2)Generalidentificationtest-salicylateSalicylicacid+FeCl3NeutralconditionFaintlyacidconditionRedcoordinationcompoundVioletcoordinationcompound6

+4FeCl3

+12HCl2.Identifieditems(2)Generalidentificationtest-aromaticprimaryamineTestproduct+Dilutehydrochloricacid0.1mol/LsodiumnitriteBasicβ-naphtholreagentOrangeto

scarletprecipitateN2+Cl-.

+NaNO2+2HCl+NaCl+2H2ON2+Cl-.

++NaOH+NaCl+2H2O2.Identifieditems(2)Generalidentificationtest-tropanealkaloidHydrolysis3HNO3

Trinitro-derivativeKOH(C2H5OH)KOHPrettyPurpleScopolicacid2.Identifieditems(2)Generalidentificationtest-inorganicmetalsalt(Na,K,Ca,NH4+)Testproduct+NaOHNH3Wetredlitmuspaperturnsblue

Filterpapermoistenedbymercurousnitratetestsolutionturnsblack

Ammoniumsalt:Flametest:Naturnsbrightyellow;Kturnsviolet;Caturnsbrickred

2.Identifieditems(2)Generalidentificationtest-inorganicacidradicalChloride:Cl-+Ag

+

AgClwhiteemulsionCl-+MnO2

Mn2++Cl2

Sulfate:SO42-+Ba2+BaSO4

white

SO42-+Pb2+PbSO4

white

Afteradditionofhydrochloricacid,thereisnowhiteprecipitateH2SO4

WetKI_starchtestpaperturnsblueHNO3

2.Identifieditems(3)SpecificidentificationtestItisthebasisforconfirmingacertainkindofdrug.Itcanidentifytheauthenticityofdrugsbyselectingsomeuniquesensitivequalitativereactionaccordingtothedifferentphysicalandchemicalpropertiesofeachdruginthesamecategory.Generalidentificationtestcandistinguishdrugsofdifferentcategoriesaccordingtothecommoncharacteristicsofcertaincategoryofdrugs.Specificidentificationtestcanidentifyeachdrugmonomeraccordingtothedifferenceinthechemicalstructuresofvariousdrugsonthebasisofgeneralidentificationtest.2.Identifieditems

Commonmalonylurea-CONHCONHCO-canreactwithsomemetalions(Ag+,Cu2+,Hg2+,etc.)toturncolororgenerateprecipitateBarbituratesR+2AgNO3

+2HNO3

Generalidentificationtest2.IdentifieditemsReactwithPb2+togenerateblackPbSReactwithformalin-sulfuricacidtopresentrosycolorReactwithiodinetomakethecolorofiodinefadeSodiumthiopentalSecobarbitalPhenobarbital2.Identifieditems1)Physicalandchemicalidentificationmethod2)Spectroscopicidentificationmethod3)Chromatographyidentificationmethod2.Identifieditems1)PhysicalandchemicalidentificationmethodAmethodtoidentifytheauthenticityofdrugsbyaddingappropriatereagentstothetestedproductsandcreatingachemicalreactionundercertainconditions.CharacteristicsofphysicalandchemicalidentificationEasyoperation,quickreaction,lowtestcostandwideapplication.However,itsspecificityispoorerthanthatofinstrumentalmethodClassificationColorreactionidentificationPrecipitategenerationreactionidentification(glucoseidentification)Fluorescencereactionidentification(vitaminB1identification)Gasgenerationreactionidentification(thioguanineidentification)Reagentfadingidentification(reactionbetweenvitaminCanddiohloroindophenol)2.Identifieditems1)PhysicalandchemicalidentificationmethodBasictartratecoppertestsolution(Fehlingtestsolution)Glucose+Cuprousoxide+gluconicacidVB1

Thiochrome(bluefluorescence)AlkalinityK3Fe(CN)6

Thioguanine●7H2OStrongacidity?H2S(Rotteneggstink)Leadacetatepaperturnsblack2.IdentifieditemsPhysicalandchemicalidentificationmethodshouldconsiderthetestconditions.Factorsinfluencingtheidentificationreactionmainlyin