Rapid detection of multiple class pharmaceuticals in both municipal wastewater and sludge with ultra high performance liquid chromatography tandem mass spectrometry

• Published in: Journal of environmental sciences (China) 2014-09, Vol.26 (9), p.1949-1959
• Main Authors: Yuan, Xiangjuan, Qiang, Zhimin, Ben, Weiwei, Zhu, Bing, Liu, Junxin
• Format: Article
• Language: English
• Subjects: China; Chromatography, High Pressure Liquid; Liquids; Mass spectrometry; Mathematical analysis; Municipal wastewater; Optimization; Pharmaceutical Preparations - analysis; Pharmaceuticals; Sewage - analysis; Sludge; Solid phase extraction; Solvent extraction; Tandem Mass Spectrometry; Ultrasonic solvent extraction; UPLC–MS/MS; Waste water; Water Pollutants, Chemical - analysis; 串联质谱法; 城市污水; 快速检测; 污水处理厂; 污泥; 溶剂萃取; 药品; 超高效液相色谱
• ISSN: 1001-0742; 1878-7320
• DOI: 10.1016/j.jes.2014.06.022

This work described the development, optimization and validation of an analytical method for rapid detection of multiple-class pharmaceuticals in both municipal wastewater and sludge samples based on ultrasonic solvent extraction, solid-phase extraction, and ultra high performance liquid chromatography-tandem mass spectrometry quantification. The results indicated that the developed method could effectively extract all the target pharmaceuticals （25） in a single process and analyze them within 24 min. The recoveries of the target pharmaceuticals were in the range of 69%-131% for wastewater and 54%-130% for sludge at different spiked concentration levels. The method quantification limits in wastewater and sludge ranged from 0.02 to 0.73 ng/L and from 0.02 to 1.00μg/kg, respectively. Subsequently, this method was validated and applied for residual pharma- ceutical analysis in a wastewater treatment plant located in Beijing, China. All the target pharmaceuticals were detected in the influent samples with concentrations varying from 0.09 ng/L （tiamulin） to 15.24 μg/L （caffeine）; meanwhile, up to 23 pharmaceuticals were detected in sludge samples with concentrations varying from 60 ng/kg （sulfamethizole） to 8.55 mg/kg （ofloxacin）. The developed method demonstrated its selectivity, sensitivity, and reliability for detecting multiple-class pharmaceuticals in complex matrices such as municipal wastewater and sludge.