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Capillary

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CapillaryCapill

    Capillary

analysisofquinolonedrugsandpharmacokineticsstudy

    ;YanMingLiu,JunTaoCao,HuiWang

    ;CollegeofChemistryandChemicalEngineering,XinyangNormalUniversity,Xinyang464000,China

    ;Received28January2008

    ;Abstract

    ;Anovelmethodforthedeterminationoftwoquinolonedrugsnorfloxacin(NOR)andlevofloxacin(LVX)wasdescribedby

    ;capillaryelectrophoresiswelectrochemiluminescencedetection.Thegoodrelationship(r>0.9991)betweenpeakareaand

    ;concentrationofanalyteswasestablishedovertwoordersofmagnitude.Thelimitsofdetection(LOD,S/N=3)instandardsolution

    ;are4.8×10mol/LforNORand6.4×10

    mol/LforLVX,respectively.Thelimitsofquantitation(LOo,S/N=10)inreal ;humanurinesamplesare1.2×l0

    .mo1/LforNORand1.4×10.mol/LforLvx.respectively.Thepresentmethodwas ;successfullyappliedtothedeterminationofN0RandLvxinhumanurilleandthestudyofpharmacokineticsofNOR.

    ;(e)2008YanMingLiu.PublishedbyElsevierB.VonbehalfofChineseChemicalSociety.AUrightsreserved.

    ;Keywords:Capillaryelectrophoresis;Electrochemiluminescencedetection;Quinolonedrugs;Urineanalysis;Pharmacokinetics

    ;Fluorinatedquinolonedrugs.suchasNORandLVX.couldimprovethetreatmentofinfectiousdiseasesduetotheir

    ;fewertoxicsideeffectsandalsoenhancedpharmacokineticspropertiesandextensiveandpotentactivityagainst

    ;Gram.positiveand.negativebacteria,includingresistantstrains.Recently,capillaryelectrophoresis(CE)hasattracted

    ;considerableattentioninthebiologicalsampleanalysis[1_4.InCE,severaldetectionmo

    des,suchasUV[5hasbeen

    ;usedfortheanalysisofLVX,anddiodearraydetection[6,UVphoto.diodearraydetectio

    n[7andLIF[8,havebeen

    ;usedfortheanalysisofN0R.Electrochemiluminescence(ECL)basedonRu(bpy).hasreceivedconsiderable

    ;attentionduetoitsexcellentpropertiesandcompatibilitywithawiderangeofanalytes.ThemarriageofCEtoECL

    ;(CE_ECL)hasprovedtobeapromisinganalytica1technique[912.

    ;Inthisstudy,thesimultaneousdeterminationofNORandLVXwascarriedoutbVCEEC

    Lforthefirsttime.The

    ;applicabilityoftheproposedmethodwasillustratedinthedeterminationoftwodrugsinhumanurinesamplesandthe

    ;pharrnacokineticsstudyforN0R.

    ;1.Experimental

    ;NORandLVXwerepurchasedfromNationalInstitutefortheControlofPharmaceuticalandBiologicalProducts

    ;(Beijing,China).NORcapsuleswereacquiredfromShanghaiYan’anpharmaceuticalCo.,Ltd.(Shanghai,China).

    ;Correspondingauthor.

    ;E?mailaddress.”liuym9518@sina.corn(Y.M.”u)

    ;1001?8417/$seefrontmatter

    2008YanMingLiu.PublishedbyElsevierB.VonbehalfofChineseChernica/Society.Allrightsreserved.

    ;doi:10.1016/j.cclet.2008.05.027

    ;

    ;

    ;YM.Liuela1./ChineseChemicalLetters19f2008)962-964

    ;Tris(2,2.bipyridy1)ruthenium(H)chloridehexahydratewaspurchasedfromAlfaAesar(AJohnsonMatthey

    ;Company,Hi11,MA,USA).AHotherChemicalswereofanalytica1.reagentgradeandusedwithoutfurther

    ;purification.10mmol/LstocksolutionsofN0RandLVXwerepreparedbydissolvingthestandardsamplesin

    ;O.1mol/LHClandstoredinthedarkplace.Aseriesofworkingstandardsolutionswerepreparedbydilutingthestock

    ;solutionwithacetonitrile(MeCN)-watermixtureswitll7O%(v/v)MeCN.Thefreshurinesamplesofhealthy

    ;volunteerswereprovidedbyXinyangCentralHospita1.leurinesampleswerecollectedatthefollowingtimepoints:

    ;beforeoraladministration,andat1,2,3,4,6,8,12,24hafteroraladministrationof200mgNOR.Eachoftheurine

    ;sampleorthespikedstandardswasdilutedwithMeCN.leratioofurinetoMeCNis3:7(v/v).lemixturewas

    ;centrifugedandthesupernantwastakenoutforanalysis.0thersolutionswerepreparedwithultrapurewater

    ;(18.2MQcm)andfilteredthrough0.22mmembranepriortouse.

    ;leexperimentswereperformedonamodelMPI.ACE-ECLsystem(Xi’anRemaxElectroni

    csCo.Ltd,Xi’an,

    ;China).A55cmlongcapillary(50mi.d.,YongnianReafineChromatographyLtd.,Hebei,China)wasusedfor

    ;separation.lenewcapillarywasrinsedsuccessivelywitll2.0mol/LCH0H-NaOH(2gNaOHdissolvedin25mL

    ;(4:1)methanol/watersolution),1.0mol/LNaOH,1.0mol/LHC1,andH20for15min,andfinallywithelectrophoretic

    ;bufferfor30min.Priortouse,thecapillarywassequentiallyflushedwitllO.1mo1/LNaOH,0.1mol/LHCl,water,and

    ;electrophoreticbufferfor5min.respectively.Electromigrationinjectionwasusedat10kVfor10s.,I1lleapplied

    ;separationvoltagewas18kV.Thepeakareawasusedfortheanalysis.

    ;2.Resultsanddiscussion

    ;Parametersaffectingtheseparationefficiencyanddetectionsensitivity,suchasseparationvoltage,concentration

    ;andpHofelectrophoreticbuffer,pHofthebufferindetectioncell,etc.,wereinvestigatedindetail.20mmol/L

    ;phosphatebufferatpH8.0wasusedintheseparationprocess.lebuffersolutioninthedetectioncellwas5mmol/L

    ;Ru(bpy)3’witll5Ommol/LphosphatebufferatpH8.2.leworkingelectrodewasbiasedat1.15VInaddition.

    ;severalsamplesolventsincludingelectrophoreticbuffer,0.1mol/LHC1.waterandMe(

    -watermixtureweretested

    ;forpreparingthestandardandsampleworkingsolutions.respectively.leresultsshowedthatthesensitivitycanbe

    ;improvedmarkedlybyuseofMeCN-watermixturewitll7O%(v/v)MeCN.

    ;Undertheoptimizedconditions,theresponselinearity,thedetectionlimits,andrepeatabilityoftwoanalytewere

    ;examined.lecalibrationcurveswerelinearbetween1.0and300i~mol/LforNORandbetween2.0and200i~mol/L

    ;forLVX.rnlecalibrationequationsandregressioncoemcientswere:Y=406.

    +5212.6andr=0.9993forNOR.

    ;Y=650.6x+9417.9andr=0.9991forLVXintermsofpeakarearesponseasafunctionofanalyteconcentration.

    ;01o02o030o4o05o0600700

    ;Migrationtime(s)

    ;Fig.1.Electropherogramsoftheblankhumanurinesample(A)andtheurinesamplespikedwith5x10_’mol/LNORand4.4x10mol/LLVX

    ;03).Peak1,NOR;peak2,LVX;X,unknowncompounds.

    ;

    ;Y.M.Liueta1./ChineseChemicalLetters19f200S)962964

    ;Detectionlimitsof4.8×10mol/LforNORand6.4×10

    mol/LforL:VXwereobtained(S/N=3).Theprecision

    ;oftheproposedmethodwasstudiedbyassayingthreeconcentrationlevels:5.50.150Ixmol,LofNORandLVX

    ;withinaday(intraday)andin3days(interday).TheRSDoftheNORrangedfrom1.8to3.4%withinaday=5)and

    ;from4.1to7.1%in3days=12),respectively.TheRSDofLVXrangedfrom2.1t04.2%withinadayandfrom5.4

    ;to8.1%in3days.respectively.

    ;ThepresentmethodwassuccessfullyappliedinthedeterminationofNORandLVXinhuma

nurinesamples.The

    ;typicalelectropherogramsofblankurinesampleandurinesamplespikedwith5×10

    mol,LNORand4.4×

    ;10

    mol/LLVXwereshowninFig.1.Fromtheurineanalysis.theLOQ(definedasthelowestanalyteconcentration

    ;yieldingasigna1tentimesgreaterthanthenoise)were1.2×10

    .mo1/LforLVX. .mol/LforNORand1.4×10

    ;respectively.Therecoveriesofthetwoanalytesatthreespikedconcentrationlevelswerecarriedoutandvariedfrom

    ;84.3t092.3%forLVXinurinesamples.respectively.TheR.S.D.ofthetwoanalytesatthreespikedconcentration

    ;levelsvariedfrom5.7to7.2%forNORand5.4to7.7%forLVX.respectively. ;TheproposedmethodwasalsousedinthemonitotingofpharmacokineticsforNOR.Twohealthymalevolunteers

    ;receivedanoraladn3inistrationof200mgofNOR,respectively.ThemeasuredresultsshowedthatcontentofNORin

    ;thetwovolunteersachievedamaximumvalueat6hafteroraladministrationandthendecreased.ThecomentofNOR

    ;involunteer1ishigherthanthatinvolunteer2atanytimeafteroraladministration.Thismightcorrelatewiththe

    ;differentabsorptioncapacityofgastrointestinaltractfrompersontoperson. ;3.Conclusion

    ;Inthisstudy,anovelCE-ECLmethodwasdevelopedforthesimultaneousdetectionofNORandLVXinreal

    ;samples.ThepharmacokineticsofNORinhumanbodywasalsostudied.ThisworkexploitsanewscopeforCE

    ;applicationsanddemonstratesthatCE-ECLcoulddevelopintoasimple,novelandpracticalmethodinclinicaland

    ;biochemicalanalysis.

    ;Acknowledgments

    ;ThisworkwassupportedbytheNationalNaturalScienceFoundationofChina(No.20575056)andHenan

    ;InnovationProjectforUniversityResearchTalents(No.2005126). ;References

    ;[1C.Q.Wang,H.Wang,Y.M.Liu,Chin.Cheil1.Lett.18(2007)452.

    ;[2X.H.Qi,J.Q.Mi,X.x.Zhang,eta1.Ana1.Chim.Acta551(2005)115.

    ;[3X.Ji,Z.He,X.Ai,etaI.Talanta70(2006)353.

    ;[41S.Chen,YXu,B.FLiu,eta1.J.Chromatogr.A1162(2007)149.

    ;f51A.FFaria,M.V.N.deSouza,M.VdeAlmeida,eta1.Ana1.Chim.Acta579(2006)185 ;[6A.Alnaiiat,A.M.Idris,H.H.AbuSeada,Microchem.J.87(2007)35. ;7A.Alnajjat,H.H.AbuSeada,A.M.Idris,Talanta72(2007)842.

    ;f81C.L.Chen2,C.FFu,C.H.Chou,J.Chromatogr.B856(2007)381.

    ;[9YM.Liu,J.Cao,Y.L.Zheng,Chem.J.Chin.UIli29(2008)81.

;f10YDu,E.K.WmJ.Sep.Sci.30(20o7)875.

    ;[11H.Y.Chiu,Z.Y.Lin,C.WWhang,eta1.J.Chromatogr.A1177(2008)195. ;f121YHuang,WPan,S.Z.Yao,eta1.J.Chromatogr.A1154(2007)373. ;

    ;

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