高效液相色谱-质谱联用法同时检测水体中 14种喹诺酮类药物残留

Simultaneous determination of 14 quinolone residues in water by high per-formance liquid chromatography-tandem mass spectrometry

中文关键词:  喹诺酮类药物残留  抗生素  水体  高效液相色谱-质谱法

英文关键词:quinolone residues  antibiotics  water  high performance liquid chromatography mass spectrometry mass spectrometry

中文摘要:

      目的 建立水体中14种喹诺酮类药物残留的高效液相色谱-质谱联用快速筛查检测方法。方法 水样经高速离心后过0.22 μm微孔滤膜直接进样, 以甲酸(0.05%)+甲醇-乙腈为流动相, 经Atlantis dC-C18柱分离, 采用电喷雾离子源(electro spray ion source, ESI)、正离子模式、多反应监测(multi-reaction monitoring, MRM)模式检测。结果 14种喹诺酮类化合物均在线性范围内线性关系良好, 其中氧氟沙星、恩诺沙星、洛美沙星、双氟沙星、沙拉沙星、氟甲喹、加替沙星的线性范围为5 ng/L~1000 ng/L, 环丙沙星、奥比沙星、麻保沙星、培氟沙星的线性范围为10 ng/L~1000 ng/L, 氟罗沙星、依诺沙星的线性范围为20 ng/L~1000 ng/L, 单诺沙星的线性范围为50 ng/L~1000 ng/L, 相关系数r除了环丙沙星外其他13种均大于 0.99, 回收率均在83.9%~110.0%范围内, 相对标准偏差均小于2.4%~15.4%, 检出限均在1.0 ng/L~20 ng/L范围内。结论 本方法快速、简便、灵敏、重现性好, 为开展水体中抗生素污染水平的调查与监测提供依据。

英文摘要:

      Objective To establish a rapid analytical method for the simultaneously screening and detection of 14 quinolone residues in water by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods After a high speed centrifugation, the samples were filtered 0.22 μm millipore filter and then were separated on an Atlantis dC-C18 column with the mobile phases of formic acid (0.05%) and methanol-acetonitrile. The electrospray ionization (ESI) source in positive ion mode was used for multiple reaction monitoring (MRM). Results The 14 quinolone chemical components showed a good linear relationship in their concentration ranges with the correlation coefficients more than 0.99 except ciprofloxacin. The linear relationship of ofloxacin, enrofloxacin, lomefloxacin, difloxacin, sarafloxacin, flumequine and gatifloxacin were 5 ng/L~1000 ng/L, ciprofloxacin, orbifloxacin, marbofloxacin and pefloxacin were 10 ng/L~1000 ng/L, fleroxacin and enoxacin were 20 ng/L~1000 ng/L, and danofloxacin was 50 ng/L~1000 ng/L. The recoveries were all of 83.9%~110.0% and the relative standard deviation (RSD) were all of 2.4%~15.4%. The limits of detection (LOD) were all of 1.0 ng/L~20 ng/L. Conclusion This method is rapid, simple, sensitive, and accurate, which provides a basis for the investigation and monitoring of the pollution level of antibiotics in water.