污泥中典型抗生素的检测

Determination of antibiotics in sludge

为了探寻一种操作简单、灵敏度高、回收率好的污泥中抗生素的分析方法,实验研究了超声萃取(ultrasound assisted extraction,USE)、加速溶剂萃取(accelerated solvent extraction,ASE)和基质固相分散(matrix solid-phase dispersion,MSPD)等5种方法,提取污泥中10种抗生素(磺胺嘧啶、磺胺甲嘧啶、磺胺甲基嘧啶、磺胺对甲氧嘧啶、磺胺甲恶唑、磺胺二甲氧哒嗪、恩诺沙星、沙拉沙星、达氟沙星和氧四环素)。结果显示,MSPD对目标抗生素的回收率最好,且具有成本低、操作便捷等优势。采用MSPD和高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)分析污泥中典型抗生素,对10种抗生素的加标回收率为40.15%~114.73%,检测限为0.02~0.28μg/kg。应用此方法分析厦门某污水处理厂夏季和冬季的污泥样品,10种抗生素浓度为nd^1 013μg/kg,冬夏平均检出浓度最高的物质为氧四环素和恩诺沙星,分别为789.67μg/kg和32.65μg/kg。

Ultrasonic assisted extraction（ USE）,accelerated solvent extraction（ ASE） and matrix solidphase dispersion（ MSPD） were applied to extract 10 antibiotics（ sulfadiazine,sulfamethazine,sulfamerazine,sulfameter,sulfamethoxazole,sulfadimethoxine,enrofloxacin,sarafloxacin,danofloxacin,oxytetracycline） in the sludge. The antibiotic recoveries by MSPD were better compared to USE and ASE. In addition,MSPD was easy to operate,cost effective,and environmentally friendly. Thus,MSPD coupled with high performance liquid chromatography-tandem mass spectrometry（ HPLC-MS / MS） was used to analyze the antibiotics in the sludge samples. Results show that the recoveries of the 10 antibiotics are in the range of 40. 15% —114. 73%,and the method detection limits are 0. 02—0. 28 μg / kg. Summer and winter sludge samples from a wastewater treatment plant of Xiamen were analyzed. The concentrations of 10 target antibiotics are nd—1 013 μg / kg. Oxytetracycline and enrofloxacin are the predominant antibiotics in summer and winter samples,with the mean concentrations of789. 67 μg / kg and 32. 65 μg / kg,respectively.