液相色谱-串联质谱法测定水体中8种典型喹诺酮类抗生素

Determination of 8 kinds of typical quinolones antibiotics by liquid chromatography-tandem mass spectrometry in water

中文关键词:  抗生素  喹诺酮类  液相色谱-串联质谱法

英文关键词:antibiotics  quinolones  liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)测定水体中8种喹诺酮类抗生素的分析方法并评价其在水体环境中的应用。方法 样品采用ACQUITY UPLC BEH C18色谱柱(10 mm×2.1 mm, 1.7 μm)分离, 以甲醇-0.1%甲酸水溶液为流动相, 设定柱温为35 ℃、流速为0.35 mL/min; 质谱条件采用电喷雾离子源正离子模式(electron spray ionization, ESI+)及多反应监测(multiple reaction monitoring, MRM)模式采集。结果 在0.1~100.0 μg/L浓度范围内, 马波沙星、氧氟沙星、洛美沙星、达氟沙星、恩诺沙星、沙拉沙星6种抗生素的质量浓度与峰面积线性关系良好(r2>0.99), 检出限为0.1 μg/L; 在5.0~500.0 μg/L浓度范围内, 培氟沙星、诺氟沙星的质量浓度与峰面积线性关系良好(r2>0.99), 检出限为5.0 μg/L。8种喹诺酮在环境水样品中的平均回收率为98.30%~111.77%, 相对标准偏差(relative standard deviations, RSDs)为0.71%~12.80%。结论 该方法简单、灵敏、准确, 可以满足水体环境中喹诺酮类抗生素检测要求。

英文摘要:

      Objective To establish a method for the determination of 8 kinds of quinolones antibiotics in water by liquid chromatography-tandem mass spectrometry (LC-MS/MS), and evaluate the application to environmental water. Methods The sample was separated on ACQUITY UPLC BEH C18 (10 mm×2.1 mm, 1.7 μm) column with methanol and water (0.1% formic acid) as the mobile phase (column temperature 35 ℃, flow rate 0.35 mL/min); and carried out by electron spray ionization (ESI+) and multiple reaction monitoring (MRM) mode. Results The quinolones showed good linearity between the peak areas and the mass concentrations in the ranges of 0.1 to 100.0 μg/L (r2>0.99) for marbofloxacin, ofloxacin, lomefloxacin, danofloxacin, enrofloxacin and sarafloxacin with the limits of detection of 0.1 μg/L; within the concentration range of 5.0?500.0 μg/L, the linear relationship between the mass concentration of pefloxacin and norfloxacin and the peak area was good (r2>0.99), and the limits of detection were 5.0 μg/L. The validation results showed that the average recoveries of 8 kinds of quinolones were ranged from 98.30%?111.77% in the environmental water samples, with relative standard deviations (RSDs) of 0.71%?12.80%. Conclusion This method is simple, sensitive and accurate, which can meet the detection requirements of quinolone antibiotics in water environment.