SPE_HPLC法测定水中4种头孢类抗生素_陶辉_李文君_陈卫_陈连生_冯博_王

SPE－HPLC法测定水中4种头孢类抗生素陶辉，李文君，陈卫，陈连生，冯博，王伦，徐峰(河海大学环境学院浅水湖泊综合治理与资源开发教育部重点实验室，江苏南京210098)摘要:建立了SPE－HPLC法同时检测水中头孢氨苄、头孢拉定、头孢他定和头孢噻肟等4种常见头孢类抗生素的方法。结果表明:亲水亲脂平衡反相吸附剂(Poly－SeryHLB型)对水中4种头孢类抗生素的富集效果较好，在含量为0～50μg/L范围内，4种头孢类抗生素的回收率为82%～121%，远高于反相C18型吸附剂。以甲醇－水为流动相，采用梯度淋洗的方法，可在7min内完成水中4种抗生素完全分离。测定4种抗生素的线性范围均为0．1～5．0mg/L，线性良好，Ｒ2＞0．999，峰面积的相对标准偏差≤0．45%，时间的相对标准偏差≤2．37%，平均加标回收率为84．19%。水样经HLB预处理后，四种抗生素的方法检出限均为50ng/L，方法回收率在83．62%～122．12%之间。该方法的回收率高、重现性好、准确性和灵敏度较高、成本低、检测快速，适用于同时测定水中4种头孢类抗生素。关键词:头孢类抗生素;检测;固相萃取;高效液相色谱中图分类号:TU991文献标识码:C文章编号:1000－4602(2014)10－0096－04基金项目:国家自然科学基金资助项目(50908074)DeterminationofFourCephalosporinAntibioticsinWaterbySolidPhaseExtractionandHigh-performanceLiquidChromatographyTAOHui，LIWen-jun，CHENWei，CHENLian-sheng，FENGBo，WANGLun，XUFeng(KeyLaboratoryofIntegratedＲegulationandＲesourceDevelopmentonShallowLakes＜MinistryofEducation＞，CollegeofEnvironment，HohaiUniversity，Nanjing210098，China)Abstract:Thesimultaneousdeterminationoffourcephalosporinantibiotics(cephalexin，cefra-dine，ceftazidimeandcefotaxime)inwaterbysolidphaseextractionandhigh-performanceliquidchroma-tography(SPE-HPLC)wasestablished．Theresultsshowedthathydrophiliclipophilicbalancereversed-phasesorbents(Poly-SeryHLB)havebetterenrichmenteffectoffourcephalosporinantibiotics，there-coveryratesoffourcephalosporinantibioticswithcontentof0to50μg/Lwere82%to121%，farhigherthanreversed-phaseC18sorbent．Withmethanolandwaterasmobilephase，usinggradientelutionmeth-od，thefourcephalosporinantibioticscouldbefullyseparatedwithin7min．Thelinearrangeswere0．1to5mg/L，withagoodlinearity(Ｒ2＞0．999)．Therelativestandarddeviationsofthepeakareawere≤0．45%，therelativestandarddeviationsoftimewere≤2．37%，andtheaveragerecoverywas84．19%．AfterpretreatmentbyHLB，themethoddetectionlimitsoffourantibioticswere50ng/L，andthemethod·69·第30卷第10期2014年5月中国给水排水CHINAWATEＲ＆WASTEWATEＲVol．30No．10May2014recoverieswerebetween83．62%to122．12%．Thismethodhashighrecovery，goodreproducibility，highaccuracyandsensitivity，lowcostandrapiddetermination．Itcanbeappliedtosimultaneou