应用离子对hplcelsd法测定磷霉素钠中磷霉素及有关物质的含量

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1、应用离子对HPLCELSD法测定磷霉素钠中磷霉素及有关物质的含量【摘要】建立了HPLCELSD法测定磷霉素钠中磷霉素及有关物质的含量。采用ODS柱，柱温35℃，以0.015mol/L正辛胺溶液(用冰乙酸调节pH至5.2)∶乙腈(90∶10)为流动相，蒸发光散射检测器温度为45℃，雾化气体压力为0.35MPa。磷霉素及其二醇物分别在26.0～207.7和7.6～60.6μg/ml范围内呈良好的线性关系，两者的定量限分别为8.7和7.7μg/ml。【关键词】离子对HPLCELSD含量测定磷霉素钠有关物质Fosfomycinisasynthetic,broadspect

2、rumbactericidalantibioticfororaladministration.IthasinvitroactivityagainstawiderangeofGrampositiveandGramnegativeaerobicmicroorganisms,whichareassociatedwithuncomplicatedurinarytractinfection［1］.ThefactthatfosfomycinhasnoUVVisabsorptionhasledtothedevelopmentoffewanalyticalmethodsforits

3、determination.Asfarasweknow,onlytheHPLCwithrefractiveindex(RI)detectionmethod,i.e.theBritishPharmacopoeia(BP)methodusedforanalysisoffosfomycintrometamol［2a］canprovideseparationforfosfomycinandrelatedsubstances.DuetothepoorsensitivityofRIdetector,11verylargeamountofsampleisinjectedwhichcau

4、sesthefosfomycinpeaktobebroadened,andtheresolutionbetweenfosfomycinandrelatedsubstancesmightbereduced.Furthermore,duetothepoorbuffercapacityofthemobilephaseandleaststabilityoftheNH2column,theBPmethodisnotrobustenough.AccordingtoBP［2b］,fosfomycinsodiumanddisodium1,2(dihydroxypropyl)phosph

5、onate(diolsubstance)aredeterminedbytitrimetricmethodwhichlacksofaccuracy.UtilizingtheChinesePharmacopoeia(ChP)method［3a］,fosfomycininfosfomycinsodiumisdeterminedbymicrobiologicalanalysis,whilefosfomycinsodiumdiolsubstancesaredeterminedbytitrimetricmethod.ThisarticleprovidedanionpairHPLC

6、ELSDmethodforthedeterminationoffosfomycinandrelatedsubstancesinfosfomycinsodium.　　1Experiment1.1MaterialsFosfomycinsodiumandfosfomycincalciumwereprovidedbyShanghaiAsiaPioneerPharmaceuticalsCo.,Ltd.FosfomycinChineseNationalChemicalReferenceStandard(CRS)ofactivity11651μg/mg,fosfomycintrome

7、tamolEuropeanPharmacopoeiaCRSofactivity53.1%,andfosfomycintrometamolimpurityA(diolsubstance)EuropeanPharmacopoeiaCRSwereused.OctylaminewaspurchasedfromAldrich.AcetontrilewasHPLCgradeandobtainedfromE.Merck.Allotherchemicalswereanalyticalgradereagents.Allsolutionswe