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目的建立城市污水处理厂污泥中20种磺胺类抗生素的液相色谱-串联质谱分析方法。方法比较超声萃取(USE)和加速溶剂萃取(ASE)对污泥中目标药物的提取效率,优化了富集净化过程。样品经USE提取,MAX固相萃取柱净化,用液相色谱-电喷雾串联质谱法(LC-ESI-MS/MS)检测。C18柱分离,正离子多反应监测模式检测,内标法定量。结果方法定量限为0.25～10.0μg/kg;三个加标水平的回收率为50.1%～120.0%,相对标准偏差小于30%。应用此方法在北京某污水处理厂活性污泥和剩余污泥中检出磺胺嘧啶、磺胺吡啶和磺胺甲恶唑,含量为2.1～153.1μg/kg。结论该方法适用于污泥中20种磺胺类抗生素的同时检测。
Objective To establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the analysis of 20 sulfonamides in sewage sludge from municipal wastewater treatment plants. Methods The extraction efficiency of target drugs in sludge by ultrasonic extraction (USE) and accelerated solvent extraction (ASE) was compared, and the enrichment and purification process was optimized. The samples were extracted by USE and purified by MAX solid-phase extraction. The samples were detected by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS / MS). C18 column separation, positive ion multi-reaction monitoring mode detection, internal standard method. Results The limit of quantification was 0.25-10.0 μg / kg. The recoveries of three spiked levels were 50.1% -120.0% with relative standard deviations less than 30%. This method was used to detect sulfadiazine, sulfapyridine and sulfamethoxazole in activated sludge and residual sludge of a sewage treatment plant in Beijing with the content of 2.1 ~ 153.1μg / kg. Conclusion This method is suitable for the simultaneous detection of 20 sulfonamides in sludge.