高效液相色谱法测定人体5-氟尿嘧啶血药浓度

350ChinaPharmacy2002Vol.13No.620021363(xs,n=12)Ka(1/h)352275509342K10(1/h)025004023003T1/2(h)10542621028159T1/2(h)141025153030CL(L/h)3036029140V/F(L)12332131254123Tmax(h)146026138031Cmax(g/ml))191031188022AUC0~(g/(mlh))1047174107114522(g/ml)()xsRSD(%)xsRSD(%)05058041680140282010175041231490442915178023131860341820150018121600311925120014121250252030100013131020201940076011140740131760050008160490091880036006160350082212002100417020004221600140021501400320240009002230090022223324AUCTmaxCmax,(P005)3,[1],80%~125%,t95%,(P005),(9759971)%3,Ka(352/h509/h),(P005)3AUCTmaxCmax(P005),P005,Tmax,,,130~240g/ml4h,10g/ml,:[1],,,[J],1998,3(3):203(:2002-02-01)高效液相色谱法测定人体5-氟尿嘧啶血药浓度邓斌1,任斌1,黎曙霞1,唐蕾1,彭惠霞2,洪晓丹1(1中山医科大学附属第一医院药学部,广州市510080;2深圳市宝安区妇幼保健院,深圳市518000):R97:A:1001-0408(2002)06-0350-02:目的:以高效液相色谱法测定人血浆中5-氟尿嘧啶的浓度方法:用硫酸铵作为蛋白沉淀剂,血浆样品用乙酸乙酯-异丙醇(85!15,V/V)提取,氮气吹干,残留物用流动相溶解后进样色谱柱为DiamonsilC18柱(46mm∀150mm,5m),流动相为001mol/LKH2PO4(pH55),流速15ml/min,紫外检测波长267nm,5-溴尿嘧啶为内标结果:本法最低检测浓度为0025g/ml,线性范围为03~10g/ml,日内RSD#50%(n=5),日间RSD#115%(n=5)结论:本法简便灵敏经济,可作为5-氟尿嘧啶药代动力学研究时血药浓度的测定方法:高效液相色谱法;5-氟尿嘧啶;血药浓度DeterminationoftheConcentrationof5-FluorouracilinHumanPlasmaWithHPLCDENGBin,RENBin,LIShuxia,TANGLei,HONGXiaodan(DeptofPharmacy,TheFirstAffiliatedHospital,SunYat-SenUniversityofMedicalSciences,Guangzhou510080)PENGHuixia(BaoanMaternalandChildCareCentre,Shenzhen518000)ABSTRACT:OBJECTIVE:ToestablishaHPLCmethodforthedeterminationof5-fluorouracilinhumanplasmaMETHODS:Theplasmasampleswereextractedwithethylacetate-isopropanol(85!15,V/V)followingprecipitationofplasmaproteinswithammoniumsulfateThesolventwasevaporatedtodrynessunderastreamofnitrogenThedryextractwasdissolvedinmobilephaseandtheninjectedintotheDiamonsilC18column(150mm∀46mm,5m)and001mol/LKH2PO4(pH55)wastakenasmobilephaseTheflowratewas15ml/min,UVdetectionwavelengthwas267nmTheinternalstandardwas5-bromouracilRESULTS:Theminimaldetectabledrugconcentrationinplasmawas0025g/mlThecalibrationcurvewaslinearoverarangefrom03g/mlto10g/mlTheintra-dayRSD#50%(n=5)andtheinter-dayRSD#115%(n=5)CONCLUSION:Themethodcanbeusedforstudyingthepharmacokineticsandbioavailabilityof5-fluorouracilKEYWORDS:HPLC;fluorouracil;plasmaconcentrationofdrug5-(5-fluorouracil,5-Fu)1957Heidelberger,5-Fu,,5-Fu,,1[1,2]11(600717486Millennium32,Waters);XW-80A();(TDx);710ApH(ORION)122002136ChinaPharmacy2002Vol.13No.63515-Fu(99%,:S85894012)5-(5-bromouracil,5-Bu,98%,:S23617743);;13:DiamonsilC18(46mm∀150mm,5m);:001mol/LKH2PO4(pH55);:15ml/min;:25∃;:267nm;:10l14:5-Fu50mg,1mg/ml:5-Bu100mg,(DMSO),40g/ml152ml,2500r/min10min,025ml15ml,25l(40g/ml),30s150mg,1min,10800r/min5min900l-(85!15,V/V),3min,10800r/min15min,,,100l,1min,10800r/min10min10l2215-Fu,5-Fu,37min103min,15min,1225-Fu(1mg/ml),10ml,,751252550125250g/ml025ml10l5-Fu,30s,5-Fu030512510g/ml,5-Fu(As)(Ai)(R,R=As/Ai),(C),C=31569R%00444,r=09999(n=6),5-Fu03~10g/ml0025g/ml(S/N=3!1)23025ml10l5-Fu,30s,5-Fu05210g/ml,,(5d),11(n=6)(g/ml)(%)RSD(%)0510222111529525058109302533331pH-KH2PO4(2!988!925!9530!70,V/V),001005mol/LKH2PO4,,,,001mol/LKH2PO4pH30405570001mol/LKH2PO4,,pH5532SpherisorbODS&DiamonsilC18Nacleosil100-SG18HypersilBDSC18HypersilODS&,DiamonsilC185-Fu,5-Fu,33,,,5-Fu5-Fu(2∃~8∃),3mo,5-Fu,5-Fu:[1]EGamelin,MBoisdronCelleRapidandsensitivehigh-performanceliquidchromatographicanalysisofhaloge_nopyrimidinesinplasma[J]JournalofChromatographyB,1997,695:409[2]MJoulia,FPinguet,PYGrosse,etalDeterminationof5-fluorouracilanditsmainmetaboblitesinplasmabyhigh-performanceliquidchromatography:Applicationtoapharamacokineticstudy[J]JournalofChromatog_raphyB,1997,692:427(:2001-10-29:2001-12-18)15-FuHPLC