高效液相色谱-电喷雾串联质谱法同步检测污水处理厂活性污泥中12种抗生素

本文建立了活性污泥中三类12种抗生素的高效液相色谱电喷雾串联质谱（HPLC-ESI-MS／MS）检测方法。将活性污泥样品经乙腈与EDTA-Mcllvaine缓冲溶液超声萃取，采用串联固相萃取柱处理样品中的目标化合物，质谱检测采用正离子扫描，选择反应监测模式12种抗生素类药物的加标回收率为63．17％～102．83％，相对标准偏差（n=6）1．28％～9．30％，方法的检出限为0．11～1．15μg／kg。将建立的方法应用于石河子市某污水处理厂活性污泥中12种抗生素的残留分析，结果表明：除洛美沙星（LOM）外，其他抗生素均被检出；磺胺类、喹诺酮类及四环素类抗生素总浓度分别为：50．00μg／kg、148．94μg，／kg及247．08μg／kg。说明该方法的选择性强、灵敏度高、重现性较好，可满足活性污泥中抗生素类药物残留检测的要求。

Simultaneous Determination of 12 Antibiotics in the Activated Sludge of Municipal Sewage Treatment Plants by High Performance Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry

A method for the determination of 12 antibiotics in the activated sludge was developed by Oasis MAX followed by the Oasis HLB solid phase extraction （SPE） cartridges and high performance liquid chromatography-eleetrospray ionization tandem- mass spectrometry （HPLC ESI-MS-/MS）. Activated sludge samples were ultrasonically extracted （USE） by a mixture of ace- tonitrile and EDTA-Mcllvaine buffer. Target antibiotics were prepared by SPE cartridges. Target compounds were analyzed by HPLC-ESI-MS/MS under positive electro spray ionization and selected reaction monitoring mode （SRM）. Results showed that the average recoveries of antibiotics in the activated sludge were from 63. 17% to 102. 83% and the corresponding relative standard deviations（RSI）,n=6）were from 1.28% to 9.30% ,respectively. Detection limits of this method were from 0.11 to 1. 15 μg/kg. The developed method was applied to analyze the activated sludge of municipal sewage treatment plants in Shihezi. Results showed that all of the 12 antibiotics were detected in all samples except lomefloxacin （LOM）. Total concentrations of sulfanilamide,quinolone and tetracycline antibiotics were 50. 00 μg/kg, 148. 94 μg/kg and 247.08 μg/kg, respectively. These date indicates that this method is selective, sensitive and reproducible for analysis of antibiotics in the activated sludge.