LC-MS-MS测定河口及近岸海水中的氟喹诺酮类药物-《集美大学学报（自然科学版）》

文章信息/Info

Title:: Measurement of Fluoroquinolone Antibiotics in Estuarine and Coastal Seawater by Liquid Chromatography-Tandem Mass Spectrometry

作者:: 杨琳1; 黄东仁1; 温裕云2; (1.福建省海洋环境与渔业资源监测中心,福建福州 350003;2.厦门大学海洋与环境学院,福建厦门 361005)

Author(s):: YANG Lin1; HUANG Dong-ren1WEN Yu-yun2; (1.Monitoring Center of Marine Environment and Fishery Resources,Fuzhou 350003, China;2.College of Oceanography & Environmental Science,Xiamen University,Xiamen 361005,China)

Keywords:: fluoroquinolone antibiotics; estuarine and coastal seawater; solid phase extraction; liquid chromatography; tandem mass spectrometry

摘要:: 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0.002~0.010 μg/L，定量限（10σ）为0.010~0.050 μg/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 %（2.5 μg/L，n=6）

Abstract:: 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