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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 pharmaceutical analysis in a wastewater treatment plant located in Beijing,China.All the target pharmaceuticals were detected in the influent samples with concentrations varying from0.09 ng/L(tiamulin)to 15.24μg/L(caffeine);meanwhile,up to 23 pharmaceuticals were detected in sludge samples with concentrations varying from 60 ng/kg(sulfamethizole)to8.55 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.
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. 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 1.00 μg / kg, respectively. Substituted, 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 sample s 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.