title: Analytical methodologies based on LC-MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge.
abstract: In this work, two analytical methodologies based on liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) were developed for quantification of emerging pollutants identified in sewage sludge after a previous wide-scope screening. The target list included 13 emerging contaminants (EC): thiabendazole, acesulfame, fenofibric acid, valsartan, irbesartan, salicylic acid, diclofenac, carbamazepine, 4-aminoantipyrine (4-AA), 4-acetyl aminoantipyrine (4-AAA), 4-formyl aminoantipyrine (4-FAA), venlafaxine and benzoylecgonine. The aqueous and solid phases of the sewage sludge were analyzed making use of Solid-Phase Extraction (SPE) and UltraSonic Extraction (USE) for sample treatment, respectively. The methods were validated at three concentration levels: 0.2, 2 and 20 μg L(-1) for the aqueous phase, and 50, 500 and 2000 μg kg(-1) for the solid phase of the sludge. In general, the method was satisfactorily validated, showing good recoveries (70-120%) and precision (RSD < 20%). Regarding the limit of quantification (LOQ), it was below 0.1 μg L(-1) in the aqueous phase and below 50 μg kg(-1) in the solid phase for the majority of the analytes. The method applicability was tested by analysis of samples from a wider study on degradation of emerging pollutants in sewage sludge under anaerobic digestion. The key benefits of these methodologies are: • SPE and USE are appropriate sample procedures to extract selected emerging contaminants from the aqueous phase of the sewage sludge and the solid residue. • LC-MS/MS is highly suitable for determining emerging contaminants in both sludge phases. • Up to our knowledge, the main metabolites of dipyrone had not been studied before in sewage sludge.
authors.affiliation: Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellón, Spain.
authors.forename: C
authors.initials: C
authors.lastname: Boix
authors.affiliation: Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellón, Spain.
authors.forename: M
authors.initials: M
authors.lastname: Ibáñez
authors.affiliation: Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellón, Spain.
authors.forename: D
authors.initials: D
authors.lastname: Fabregat-Safont
authors.affiliation: Depuración de Aguas del Mediterráneo, Avda. Benjamin Franklin 21 Parque Tecnológico, Paterna, Spain.
authors.forename: E
authors.initials: E
authors.lastname: Morales
authors.affiliation: Depuración de Aguas del Mediterráneo, Avda. Benjamin Franklin 21 Parque Tecnológico, Paterna, Spain.
authors.forename: L
authors.initials: L
authors.lastname: Pastor
authors.affiliation: Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellón, Spain.
authors.forename: J V
authors.initials: JV
authors.lastname: Sancho
authors.affiliation: Depuración de Aguas del Mediterráneo, Avda. Benjamin Franklin 21 Parque Tecnológico, Paterna, Spain.
authors.forename: J E
authors.initials: JE
authors.lastname: Sánchez-Ramírez
authors.affiliation: Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellón, Spain.
authors.forename: F
authors.initials: F
authors.lastname: Hernández
keywords: Emerging contaminants; Quantification of selected emerging compounds in liquid and solid phases of the sewage sludge by LC–MS/MS; liquid chromatography; sewage sludge; solid-phase extraction; tandem mass spectrometry; ultrasonic-assisted extraction