CAJ | 학술논문

建立了河口及近岸海水中氟喹诺酮类药物残留的固相萃取富集-高效液相色谱-串级质谱测定方法.以Waters HLB固相萃取（SPE）小柱富集水样中的氟喹诺酮类药物,用XDB-C18柱、乙腈、甲酸（体积分数为0.2%）水流动相进行分离,ESI正离子源、三重串级质谱及多反应监测模式（MRM）进行目标物的定性、定量测定.优化实验条件下,方法的检出限（3σ）为0.002～0.010μg/L,定量限（10σ）为0.010～0.050μg/L,样品加标回收率为73.3%（奥比沙星）～119.7%（氧氟沙星）,相对标准偏差（RSD）为1.3%～5.8%（2.5μg/L,n=6）.
건립료하구급근안해수중불규낙동류약물잔류적고상췌취부집-고효액상색보-천급질보측정방법.이Waters HLB고상췌취（SPE）소주부집수양중적불규낙동류약물,용XDB-C18주、을정、갑산（체적분수위0.2%）수류동상진행분리,ESI정리자원、삼중천급질보급다반응감측모식（MRM）진행목표물적정성、정량측정.우화실험조건하,방법적검출한（3σ）위0.002～0.010μg/L,정량한（10σ）위0.010～0.050μg/L,양품가표회수솔위73.3%（오비사성）～119.7%（양불사성）,상대표준편차（RSD）위1.3%～5.8%（2.5μg/L,n=6）.
An accurate method was developed for measurement of fluoroquinolone antibiotics in estuarine and coastal seawater by solid phase extraction（SPE） and liquid chromatography-tandem mass spectrometry.The fluoroquinolones were enriched by Waters HLB SPE column,eluted and concentrated before separating with XDB-C18 column with mobile phase of acetonitrile and water containing 0.2 % formic acid.The analytes were then detected with tandem mass spectrometer using positive ESI at MRM mode.Under the optimized operating conditions,relative standard deviation（RSD） for developed method were 1.3 %~5.8 %（2.5 μg/L,n=6）,standard added recoveries were 73.3 %（orbifloxacin） ~119.7 %（ofloxacin）,limits of detection（3σ） were 0.002~0.010 μg/L,limits of quantification（10σ）were 0.010~0.050 μg/L.