EP7.0--盐酸莫西沙星

EUROPEANPHARMACOPOEIA7.0Moxifloxacin

hydrochloride

K.R=H,R′=CO-C6H4-pNO2:5-O

-(4-nitrobenzoyl)moxidectin,

E.(4S

)-2-dehydro-4-hydromoxidectin,

L.(23Z)-moxidectin.

01/2008:2254corrected6.2

MOXIFLOXACINHYDROCHLORIDE

Moxifloxacini

hydrochloridum

G.(23E,25S)-5O-desmethyl-28-deoxy-25-[(1E)-1,3-dimethylbut-1-enyl]-23-(methoxyimino)milbemycin

B,

C21H25ClFN3O4

Mr437.9

DEFINITION

1-Cyclopropyl-6-fluoro-8-methoxy-7-[(4a6H-pyrrolo[3,4-b]pyridin-6-yl]-4-oxo-1,4-dihydroquinoline-3-S,7aS)-octahydro-carboxylicacidhydrochloride.

Content:98.0percentto102.0percent(anhydroussubstance).PRODUCTION

TheH.

2,5-didehydro-5-deoxymoxidectin,

satisfactoryproductionenantiomericmethodispurityvalidatedofthetofinaldemonstrateproduct.

theCHARACTERS

Appearancehygroscopic.

:lightyelloworyellowpowderorcrystals,slightlySolubility(96percent),:sparinglypracticallysolubleinsolubleinwater,inacetone.

slightlysolubleinethanolIDENTIFICATION

A.Specificopticalrotation(seeTests).

B.Infraredabsorptionspectrophotometry(2.2.24).Comparison:moxifloxacinhydrochlorideCRS.

C.Dissolve50mgin5mLofwaterR,add1mLofdilutenitricacidR,mix,allowtostandforI.(23S)-23-des(methoxyimino)-23-[(methylsulfanyl)me-

givesreaction(a)ofchlorides(52.3.1min).andfilter.Thefiltratethoxy]moxidectin,

TESTS

Appearancethanofsolution.ThesolutioniscolouredreferencethanreferencesuspensionsolutionII(2.2.1GY)andnotnotmoremoreopalescentintenselyintendedforuseinthemanufacture2of(2.2.2,parenteralMethodpreparations,II).Ifthethansolutionreferenceisclearsolution(2.2.1GY)andnotmoreintenselyII).

coloured2(2.2.2,MethodDissolve1.0gin20mLofdilutesodiumhydroxidesolutionR.pH(2.2.3):3.9to4.6.

Dissolve0.10gin50mLofcarbondioxide-freewaterR.Specificsubstance).

opticalrotation(2.2.7): 125to 138(anhydrousJ.Rmoxidectin,=CH2-S-CH3,R′=H:7-O-[(methylsulfanyl)methyl]-Dissolve0.200gin20.0mLofamixtureofequalvolumesofacetonitrileRandwaterR.

GeneralNotices(1)applytoallmonographsandothertexts

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MoxonidineEUROPEANPHARMACOPOEIA

7.0

Relatedoutthetestsubstancesprotected.Liquidfromlight.

chromatography(2.2.29).CarrySulfated1.0ginaashplatinum(2.4.14crucible.

):maximum0.1percent,determinedonSolutionA.Dissolve0.50goftetrabutylammoniumhydrogensulfateASSAY

aboutLiquidand0.050500RandgmL1.0ofofanhydrouswatergofpotassiumR.Addsodium2dihydrogenmLsulfiteofphosphoricphosphateR,thendiluteacidRtoRinrelatedchromatographysubstanceswith(the2.2.29following)asdescribedmodification.inthetestfor1000.0mLwithwaterR.

Injection:testsolution(b)andreferencesolution(a).

TestCalculatethepercentagecontentofCexaminedsolutioninsolution(a).DissolveAand50.0dilutemgtoof50.0themLsubstancewiththetosamebedeclaredcontentofmoxifloxacinhydrochloride21H25ClFN3OCRS4from.thesolution.

TestSTORAGE

withsolutionsolution(b)A.

.Dilute2.0mLoftestsolution(a)to20.0mLInanairtightcontainer,protectedfromlight.

ReferenceLABELLING

hydrochloridesolution(a).Dissolve50.0mgtheCRSinsolutionAanddiluteofmoxifloxacinto50.0mLwithThewithsamesolutionsolution.A.

Dilute2.0mLofthissolutionto20.0mLforuselabelinstates,themanufacturewhereapplicable,ofparenteralthatthepreparations.substanceissuitableReferencesolution(b).Dissolve5mgofmoxifloxacinforpeakIMPURITIES

identificationSpecifiedimpurities:A,B,C,D,

E.

solutionAandCRSdilute(containingto5.0mLimpuritieswiththesameA,B,solution.C,DandE)inReference100.0mLwithsolutionsolution(c).DiluteA.Dilute1.01.0mLmLoftestofthissolutionsolution(a)toto10.0mLwithsolutionA.Column:

—size:l=0.25m,Ø=4.6mm;

—stationaryphase:end-cappedphenylsilylsilicagelforchromatographyR(5μm);A.R—temperature:45°C.

6H=-pyrrolo[3,4-R′=F:1-cyclopropyl-6,8-difluoro-7-[(4ab]pyridin-6-yl]-4-oxo-1,4-dihydroquinoline-3-S,7aS)-octahydro-Mobilecarboxylicacid,ofasolutionphasecontaining:mix28volumes0.5g/LofofmethanoltetrabutylammoniumRand72volumesB.RhydrogensulfateR,1.0g/Lofpotassiumdihydrogen7a=S)-octahydro-6R′=OCH3:1-cyclopropyl-6,8-dimethoxy-7-[(4aH-pyrrolo[3,4-b]pyridin-6-yl]-4-oxo-1,4-S,phosphateRand3.4g/LofphosphoricacidR.dihydroquinoline-3-carboxylicacid,Flowrate:1.3mL/min.

C.RDetection:spectrophotometerat293nm.

7a=S)-octahydro-6F,R′=OC2HH5:-pyrrolo[3,4-1-cyclopropyl-8-ethoxy-6-fluoro-7-[(4ab]pyridin-6-yl]-4-oxo-1,4-S,Injectiondihydroquinoline-3-carboxylicacid,and(c).

:10μLoftestsolution(a)andreferencesolutions(b)D.R=OCH3,R′=F:1-cyclopropyl-8-fluoro-6-methoxy-7-[(4aS,Runtime:2.5timestheretentiontimeofmoxifloxacin.

7aIdentificationdihydroquinoline-3-carboxylicS)-octahydro-6H-pyrrolo[3,4-acid,b]pyridin-6-yl]-4-oxo-1,4-withofimpurities:useE.R=F,R′=OH:1-cyclopropyl-6-fluoro-8-hydroxy-7-[(4aS,chromatogrammoxifloxacin7athepeaksduetoobtainedforpeakidentificationthechromatogramCRSandsuppliedthe

impuritieswithA,referenceB,C,DandsolutionE.(b)toidentifydihydroquinoline-3-carboxylicS)-octahydro-6H-pyrrolo[3,4-acid.

b]pyridin-6-yl]-4-oxo-1,4-Relative(retentionretention01/2008:1758impurityBtime=about=aboutwithreferencetomoxifloxacin

1.3;14impuritymin):impurityC=aboutA=1.4;about1.1;corrected6.0

impurityD=about1.6;impurityE=about1.7.Systemsuitability:referencesolution(b):

MOXONIDINE

—resolutionmoxifloxacin:minimumandimpurity1.5betweenA;

thepeaksduetoMoxonidinum

—thesuppliedchromatogramwithmoxifloxacinobtainedforissimilarpeakidentificationtothechromatogramCRS.Limits:

—correctionpeakcorrectionareasfactorsfactor:ofthefollowing:forthecalculationofcontent,multiplytheimpurityBimpurities=1.4;impuritybytheEcorresponding=3.5;

C9H12ClN5OM—impuritiesA,B,C,D,E:foreachimpurity,notmorethan[75438-57-2]

r241.7

theDEFINITION

withareareferenceofthesolutionprincipal(c)peak(0.1inperthecent);

chromatogramobtained4-Chloro-—unspecifiedimpurities:foreachimpurity,notmorethanthemethylpyrimidin-5-amine.

N-(imidazolidin-2-ylidene)-6-methoxy-2-areaContent:97.5percentto102.0percent(driedsubstance).withofreferencetheprincipalsolutionpeak(c)in(0.10theperchromatogramcent);

obtained—totalCHARACTERS

inthe:notchromatogrammorethan3obtainedtimesthewithareareferenceoftheprincipalsolutionpeak(c)Appearance:whiteoralmostwhitepowder.

(0.3percent);

Solubility—disregardmethanol,:slightlyveryslightlysolublesolubleinmethyleneinwater,chloride,sparinglyverysolubleslightlyininlimit:0.5timestheareaofsolubleinacetonitrile.

(0.05theperchromatogramcent).

obtainedwithreferencetheprincipalsolutionpeak(c)IDENTIFICATION

Water(2.5.12):maximum4.5percent,determinedon0.200g.Infraredabsorptionspectrophotometry(2.2.24).

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Seetheinformationsectionongeneralmonographs(coverpages)

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