全自动在线SPE-UPLC-MS/MS测定中水中15种喹诺酮  

Fully Automated Online Solid Phase Extraction-Super High Performance Liquid Chromatography-Tandem Mass Spectrometry Determination of 15 Quinolones in Reclaimed Water

作　　者：冯月超[1] 丁奇 杨一帆 王建凤[1] 贾丽[1] 陈冬梅 邵鹏[1] FENG Yue-chao;DING Qi;YANG Yi-fan;WANG Jian-feng;JIA Li;CHEN Dong-mei;SHAO Peng(Beijing Engineering Research Center of Food Safety Analysis,Beijing Centre for Physical&Chemical Analysis,Beijing 100089,China)

机构地区：[1]北京市理化分析测试中心,北京市食品安全分析测试工程技术研究中心,北京100089

出　　处：《中国给水排水》2020年第12期143-149,共7页China Water & Wastewater

基　　金：北京市科学技术研究院创新工程项目(PXM2018_178305_000007)。

摘　　要：建立了中水中15种喹诺酮类物质的全自动在线固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)测定方法。在中水样品加入0.2%甲酸酸化后加入5%甲醇,进样量为5 m L,仪器自动完成6个步骤:加载样品、淋洗、洗脱、SPE柱的再生、被测物的分离和质谱分析测定。分析方法采用电喷雾正离子扫描(ESI+),多反应监测(MRM)模式检测,外标法定量。在加标浓度范围为0.05~5μg/L时,15种喹诺酮标准曲线线性良好,相关系数(R^2)均大于0.991,回收率范围为84.4%~116.2%(n=6),RSD≤19.92%,检出限(LOD)范围为0.7~8.7 ng/L。采用该方法检测了30个实际中水样品,其中13个中水样品检出了7种喹诺酮,浓度范围为0.004 2~0.47μg/L。A fully automated online solid phase extraction-super high performance liquid chromatography-tandem mass spectrometry( SPE-UPLC-MS/MS) method was developed for detecting15 quinolones in reclaimed water samples.The samples were acidized with 0.2% formic acid,then added 5% methanol.The injection volume was 5 m L,and the instrument automatically completed 6 steps:loading sample, cleanup, elution, online SPE column regeneration, separation of the object and determination by mass spectrometry.The analytical methods were electrospray positive ion scanning( ESI+),multi-reaction monitoring( MRM) mode detection,and external standard legal quantity.When the standard concentration range was 0.05-5 μg/L,the standard curve of 15 quinolones was linear and the correlation coefficient( R^2) was greater than 0.991.The recovery range was 84.4%-116.2%( n =6),the RSD was no more than 19.92%,and the limit of detection( LOD) range was 0.7-8.7 ng/L.30 reclaimed water samples were analyzed by this method.As a result,7 quinolones were detected in 13 reclaimed water samples.The concentration of the compounds ranged from 0.004 2 to 0.47 μg/L.

关 键 词：中水 喹诺酮类 在线SPE 超高效液相色谱-串联质谱 

分 类 号：TU992[建筑科学—市政工程]