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采用超高效液相色谱-串联质谱法快速检测城市污水和污泥中的多种类药物。

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

机构信息

Key Laboratory of Aquatic Science and Technology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China.

Key Laboratory of Aquatic Science and Technology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China.

出版信息

J Environ Sci (China). 2014 Sep 1;26(9):1949-59. doi: 10.1016/j.jes.2014.06.022. Epub 2014 Jul 5.

Abstract

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 24min. 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 0.73ng/L and from 0.02 to 1.00μg/kg, respectively. Subsequently, this method was validated and applied for residual pharmaceutical analysis in a wastewater treatment plant located in Beijing, China. All the target pharmaceuticals were detected in the influent samples with concentrations varying from 0.09ng/L (tiamulin) to 15.24μg/L (caffeine); meanwhile, up to 23 pharmaceuticals were detected in sludge samples with concentrations varying from 60ng/kg (sulfamethizole) to 8.55mg/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.

摘要

本工作描述了一种基于超声溶剂萃取、固相萃取和超高效液相色谱-串联质谱定量分析的快速检测城市污水和污泥样品中多类药物的分析方法的开发、优化和验证。结果表明,所开发的方法能够在单一过程中有效提取所有目标药物(25 种),并在 24min 内对其进行分析。在不同加标浓度水平下,目标药物在废水和污泥中的回收率范围分别为 69%-131%和 54%-130%。该方法在废水中和污泥中的定量限范围分别为 0.02-0.73ng/L 和 0.02-1.00μg/kg。随后,该方法在中国北京的一个污水处理厂进行了验证和应用,用于残留药物分析。在进水样品中检测到所有目标药物,浓度范围从 0.09ng/L(替米考星)到 15.24μg/L(咖啡因);同时,在污泥样品中检测到多达 23 种药物,浓度范围从 60ng/kg(磺胺甲恶唑)到 8.55mg/kg(氧氟沙星)。所开发的方法证明了其在检测城市污水和污泥等复杂基质中的多类药物时的选择性、灵敏度和可靠性。

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