城市污水处理厂污泥中磺胺类抗生素的液相色谱-串联质谱法测定

Analysis of 20 sulfonamides in sewage sludge by high performance liquid chromatography tandem mass spectrometry

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 develop a comprehensive method for simultaneous analysis of 20 sulfonamides in sewage sludge by liquid chromatography tandem mass spectrometry（LC-MS/MS）.Methods Ultrasonic extraction and accelerated solvent extraction was compared with respect to the recovery of target drugs from sludge.Cleanup procedure was optimized during the test.The sludge samples were ultrasonicly extracted and purified by a mix mode anion-ion exchange solid-phase extraction,following determination using LC-MS/MS.20 sulfonamides were separated by a C18 column and analyzed under positive ion mode with multi-reaction monitoring.Isotopic internal standards calibration was used for quantification.Results The method quantification limits for 20 analytes were 0.25-10.0 μg/kg with overall recoveries of 50.1%-120.0%,and the relative standard deviations less than 30%.The method was finally used to analyze sulfonamides in sludge from sewage treatment plants in Beijing,and 3 target compounds（sulfadiazine,sulfapyridine and sulfamethoxazole） were detected at a concentration range of 2.1-153.1μg/kg.Conclusion This method could be applied in simultaneous analysis of 20 sulfonamides in municipal sludge samples.