title: Simultaneous analysis of 45 pharmaceuticals and personal care products in sludge by matrix solid-phase dispersion and liquid chromatography tandem mass spectrometry.
abstract: Pharmaceuticals and personal care products (PPCPs) are a class of emerging contaminants widely distributed in the wastewater treatment system. The simultaneous analysis of multiple PPCPs in the sludge, which is a complex matrix, is still not fully studied. In this study, a procedure based on matrix solid-phase dispersion (MSPD) for the extraction of PPCPs from the sludge with determination by liquid chromatography tandem mass spectrometry (LC-MS/MS) was investigated. Forty-five PPCPs, including antibiotics, nonsteroidal anti-inflammatory drugs, β-blockers, antidepressants, antimicrobial agents, preservatives, UV filters, and so on, were studied. MSPD parameters, including the sorbent materials, the ratio of sample to sorbent, the eluent composition, and the elution volumes, were sequentially optimized. Best results were achieved by 0.1 g of sludge homogenized with 0.4 g of C18-bonded silica sorbent and elution by 6 mL methanol and 10 mL acetonitrile/5 % oxalic acid (8/2, v/v). The method quantification limits for the 45 PPCPs ranged 0.117-5.55 μg/kg. The PPCP recoveries ranged from 50.3 to 107 % with relative standard deviation lower than 15 %. The proposed method was applied to analyze PPCPs in the sludge collected from a domestic wastewater treatment plant over 1 year. Thirteen PPCPs were detected, with the concentrations of ofloxacin and triclocarban more than 1000 μg/kg. Temporal variations of the PPCP levels were observed. Thus, MSPD-LC-MS/MS method could achieve good sensitivity and recovery for the target PPCP analysis in the sludge samples, while MSPD provided one-step sample preparation which was easier and faster to perform compared to the commonly used methods. Graphical abstract Workflow of MSPD and LC-MS/MS chromatograms for PPCP analysis.
authors.affiliation: Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, 1799 Jimei Road, Xiamen, Fujian, 361021, China.|University of Chinese Academy of Sciences, Beijing, 100043, China.
authors.forename: Mingyue
authors.initials: M
authors.lastname: Li
authors.affiliation: Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, 1799 Jimei Road, Xiamen, Fujian, 361021, China. qsun@iue.ac.cn.
authors.forename: Qian
authors.initials: Q
authors.lastname: Sun
authors.affiliation: Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, 1799 Jimei Road, Xiamen, Fujian, 361021, China.|University of Chinese Academy of Sciences, Beijing, 100043, China.
authors.forename: Yan
authors.initials: Y
authors.lastname: Li
authors.affiliation: Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, 1799 Jimei Road, Xiamen, Fujian, 361021, China.|University of Chinese Academy of Sciences, Beijing, 100043, China.
authors.forename: Min
authors.initials: M
authors.lastname: Lv
authors.affiliation: Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, 1799 Jimei Road, Xiamen, Fujian, 361021, China.
authors.forename: Lifeng
authors.initials: L
authors.lastname: Lin
authors.affiliation: Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, 1799 Jimei Road, Xiamen, Fujian, 361021, China.|Department of Biology and Environmental Engineering, Hefei University, Hefei, Anhui, 230601, China.
authors.forename: Yang
authors.initials: Y
authors.lastname: Wu
authors.affiliation: Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, 1799 Jimei Road, Xiamen, Fujian, 361021, China.|Department of Chemistry, University of Gujrat, Gujrat, 50700, Pakistan.
authors.forename: Muhammad
authors.initials: M
authors.lastname: Ashfaq
authors.affiliation: Key Laboratory of Urban Pollutant Conversion, Institute of Urban Environment, Chinese Academy of Sciences, 1799 Jimei Road, Xiamen, Fujian, 361021, China.|Graduate Institute of Environmental Engineering, National Taiwan University, Taipei, 106, Taiwan.
authors.forename: Chang-Ping
authors.initials: CP
authors.lastname: Yu
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D045424:Complex Mixtures / Q000032:analysis / Q000737:chemistry; D003358:Cosmetics / Q000032:analysis* / Q000737:chemistry; D004364:Pharmaceutical Preparations / Q000032:analysis* / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012722:Sewage / Q000032:analysis / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D062065:Wastewater / Q000737:chemistry; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000737:chemistry
chemical_list: D045424:Complex Mixtures; D003358:Cosmetics; D004364:Pharmaceutical Preparations; D012722:Sewage; D062065:Wastewater; D014874:Water Pollutants, Chemical
keywords: Determination; LC-MS/MS; MSPD; PPCPs; Sludge