title: Multi-residue method for the determination of over 400 priority and emerging pollutants in water and wastewater by solid-phase extraction and liquid chromatography-time-of-flight mass spectrometry.
abstract: This article describes the development and validation of a liquid chromatography high-resolution mass spectrometry method for the simultaneous determination of over 400 multi-class priority and emerging pollutants with different physicochemical properties in environmental waters (surface water and wastewater). The proposed approach is based on the use of a database consisting of retention time/exact mass (of selected ions) pairs implemented with specific software for data analysis. The targeted list comprises 430 contaminants belonging to different compound categories, including 105 multiclass pharmaceuticals (analgesics/anti-inflammatories, antibiotics, lipid regulators, β-blockers, antiepileptic/psychiatrics ulcer healings, diuretics, hormones and bronchodilatadors), life-style products (caffeine, nicotine), 21 drugs of abuse and their metabolites, 279 pesticides and some of their more relevant metabolites, nitrosamines, flame retardants, plasticizers and perfluorinated compounds. The proposed approach included a simple offline solid phase extraction (SPE) step using polymeric cartridges (Oasis HLB) with 200mL of water sample loaded, followed by analysis by rapid resolution liquid chromatography electrospray time-of-flight mass spectrometry (LC-TOFMS) in both positive and negative modes. The identification of the positive findings is accomplished with the data from accurate masses of the target ions along with retention time data and characteristic in-source fragment ions. The overall method performance was satisfactory with limits of quantification lower than 10ngL(-1) for the 44% of studied compounds. Recoveries between 50% and 130% were obtained for the 65% of the analytes (281 compounds). Matrix effects occurring with wastewater matrices were also assessed. The developed method was applied to the determination of target analytes in real surface water and wastewater samples.
authors.affiliation: Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, Jaén 23071 Spain.
authors.forename: José
authors.initials: J
authors.lastname: Robles-Molina
authors.affiliation: Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, Jaén 23071 Spain.
authors.forename: Felipe J
authors.initials: FJ
authors.lastname: Lara-Ortega
authors.affiliation: Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, Jaén 23071 Spain.
authors.forename: Bienvenida
authors.initials: B
authors.lastname: Gilbert-López
authors.affiliation: Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, Jaén 23071 Spain.
authors.forename: Juan F
authors.initials: JF
authors.lastname: García-Reyes
authors.affiliation: Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, Jaén 23071 Spain. Electronic address: amolina@ujaen.es.
authors.forename: Antonio
authors.initials: A
authors.lastname: Molina-Díaz
mesh_terms: D002853:Chromatography, Liquid; D004784:Environmental Monitoring / Q000379:methods*; D013058:Mass Spectrometry; D008970:Molecular Weight; D010575:Pesticides / Q000032:analysis; D015203:Reproducibility of Results; D052616:Solid Phase Extraction; D062065:Wastewater / Q000737:chemistry*; D014867:Water / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000737:chemistry
chemical_list: D010575:Pesticides; D062065:Wastewater; D014867:Water; D014874:Water Pollutants, Chemical
keywords: Environmental; Liquid chromatography; Mass spectrometry; Priority contaminants, Emerging contaminants, High resolution, Pesticides, Pharmaceuticals, Personal care products