在线固相萃取/高效液相色谱/串联四极杆质谱仪(SPE/UPLC/MS/MS)同时检测水中17种抗生素
Simultaneous Determination of 17 Antibiotics in Water by Online Solid-Phase Extraction,High-Performance Liquid Chromatography and Tandem Quadrupole Mass Spectrometry(SPE/UPLC/MS/MS)
周日安 1杨义右 1张苏燕 1黄杨瓯 1吴素慧 1陈约约 1郑仕1
作者信息
- 1. 国家城市供水水质监测网温州监测站,浙江温州 325000;温州市自来水有限公司,浙江温州 325000
- 折叠
摘要
研究建立了在线富集高效液相色谱-串联质谱法同时检测水中大环内酯类、磺胺类、四环素类、喹诺酮类四大类共17种抗生素含量的分析方法.水样通过Waters SPE模式在线富集经Waters Oasis® HLB固相富集小柱(30 mm×2.1 mm,20 μm)富集净化后,以ACQUITY UPLC® BEH C18色谱柱(100 mm×2.1 mm,1.7 μm)分离,0.1％甲酸水溶液-乙腈为流动相,在电喷雾离子源正离子模式下采用质谱多反应监测模式(MRM)检测.结果表明,各目标化合物质量浓度在5～100 ng/L,线性关系良好(R＞0.990),检出限为2.04～3.30 ng/L;17种抗生素的加标回收率为49.1％～133.8％,相对标准偏差(RSD,n=6)为3.8％～11.3％.应用该方法测定温州市饮用水水源地的水样,除某水库下游红霉素、克拉霉素、阿奇霉素、磺胺甲恶唑、罗红霉素被检出外,其余12种抗生素均未有检出.
Abstract
In this study,it was established an online enrichment high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for simultaneous detection of 17 antibiotics in water,including macrolides,sulfonamides,tetracyclines,and quinolones.The water samples were enriched online through the Waters SPE mode using the Waters Oasis® HLB solid-phase extraction cartridge(30 mm×2.1 mm,20 μm)and then separated on the ACQUITY UPLC® BEH C18 column(100 mm×2.1 mm,1.7 μm)with 0.1％formic acid aqueous solution-acetonitrile as the mobile phase.Detection in positive ion mode using multiple reaction monitoring(MRM)in an electrospray ionization source.The results indicated a good linear relationship between the target compound and mass concentration(R＞0.990)in the range of 5～100 ng/L,and the detection limit was 2.04～3.30 ng/L.The recovery rates of the 17 kinds of antibiotics were 49.1％～133.8％,and the relative standard deviation(RSD,n=6)was 3.8％～11.3％.The method was applied to detect the water samples from the drinking water sources in Wenzhou City,and except for certain reservoir downstream of erythromycin,clarithromycin,azithromycin,sulfamethoxazole,roxithromvcin,no other 12 kinds of antibiotics were detected.
关键词
液相色谱/串联质谱/检测/在线富集/抗生素/水体Key words
liquid chromatography-tandem mass spectrometry/detection/in-situ enrichment/antibiotics/water bodies引用本文复制引用
基金项目
温州市自来水有限公司专业技术课题(2024)(WSSYF-202402003)
出版年
2024
国家科技期刊平台
NSTL
万方数据