title: Rapid analysis of diclofenac and some of its transformation products in the three-spined stickleback, Gasterosteus aculeatus, by liquid chromatography-tandem mass spectrometry.
abstract: Pharmaceuticals are emerging organic contaminants ubiquitously present in the environment due to incessant input into the aquatic compartment mainly resulting from incomplete removal in wastewater treatment plants. One of the major preoccupations concerning pharmaceuticals released into surface waters is their potential for bioaccumulation in biota, possibly leading to deleterious effects on ecosystems especially as they could affect a broad variety of organisms living in or depending on the aquatic environment. Thus, the development of accurate and sensitive methods is necessary to detect these compounds in aquatic ecosystems. Considering this need, this study deals with the analytical development of a methodology to quantify traces of diclofenac together with some of its biotic and abiotic transformation products in whole-body tissue of three-spined stickleback. A simple and reliable extraction method based on a modified QuEChERS extraction is implemented on 200 mg of fish. The detection and quantification of the ten target compounds are performed using liquid chromatography-tandem mass spectrometry. The whole process was successfully validated regarding linearity, recovery, repeatability, and reproducibility. The method limits of detection and quantification do not exceed 1 ng/g. To reproduce environmental conditions, we measured the concentration of DCF and its transformation products in three-spined sticklebacks after a 6-month exposure in mesocosms at several levels of DCF ranging from 0.05 to 4.1 μg/L. The phase I metabolite 4'-hydroxydiclofenac was detected in fish samples exposed at the highest DCF concentration. Graphical abstract Analysis of diclofenac and some of its transformation products in the three-spined stickleback, Gasterosteus aculeatus, by QuEChERS extraction followed by LC-MS/MS.
authors.affiliation: Université de Lyon, Institut des Sciences Analytiques, UMR 5280, CNRS, Université Lyon 1, ENS Lyon - 5, rue de la Doua, 69100, Villeurbanne, France. gaelle.daniele@isa-lyon.fr.
authors.forename: Gaëlle
authors.initials: G
authors.lastname: Daniele
authors.affiliation: Université de Lyon, Institut des Sciences Analytiques, UMR 5280, CNRS, Université Lyon 1, ENS Lyon - 5, rue de la Doua, 69100, Villeurbanne, France.
authors.forename: Maëva
authors.initials: M
authors.lastname: Fieu
authors.affiliation: Unité d'écotoxicologie in vitro et in vivo, INERIS UMR-I 02 SEBIO (INERIS, URCA, ULH), Parc Technologique Alata, BP n°2, 60550, Verneuil-en-Halatte, France.
authors.forename: Sandrine
authors.initials: S
authors.lastname: Joachim
authors.affiliation: Unité d'écotoxicologie in vitro et in vivo, INERIS UMR-I 02 SEBIO (INERIS, URCA, ULH), Parc Technologique Alata, BP n°2, 60550, Verneuil-en-Halatte, France.
authors.forename: Anne
authors.initials: A
authors.lastname: Bado-Nilles
authors.affiliation: Unité d'écotoxicologie in vitro et in vivo, INERIS UMR-I 02 SEBIO (INERIS, URCA, ULH), Parc Technologique Alata, BP n°2, 60550, Verneuil-en-Halatte, France.
authors.forename: Patrick
authors.initials: P
authors.lastname: Baudoin
authors.affiliation: Unité d'écotoxicologie in vitro et in vivo, INERIS UMR-I 02 SEBIO (INERIS, URCA, ULH), Parc Technologique Alata, BP n°2, 60550, Verneuil-en-Halatte, France.
authors.forename: Cyril
authors.initials: C
authors.lastname: Turies
authors.affiliation: Unité d'écotoxicologie in vitro et in vivo, INERIS UMR-I 02 SEBIO (INERIS, URCA, ULH), Parc Technologique Alata, BP n°2, 60550, Verneuil-en-Halatte, France.
authors.forename: Jean-Marc
authors.initials: JM
authors.lastname: Porcher
authors.affiliation: Unité d'écotoxicologie in vitro et in vivo, INERIS UMR-I 02 SEBIO (INERIS, URCA, ULH), Parc Technologique Alata, BP n°2, 60550, Verneuil-en-Halatte, France.
authors.forename: Sandrine
authors.initials: S
authors.lastname: Andres
authors.affiliation: Université de Lyon, Institut des Sciences Analytiques, UMR 5280, CNRS, Université Lyon 1, ENS Lyon - 5, rue de la Doua, 69100, Villeurbanne, France.
authors.forename: Emmanuelle
authors.initials: E
authors.lastname: Vulliet
mesh_terms: D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods*; D004008:Diclofenac / Q000737:chemistry* / Q000302:isolation & purification / Q000378:metabolism; D015394:Molecular Structure; D010473:Perciformes / Q000378:metabolism*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000737:chemistry* / Q000302:isolation & purification / Q000378:metabolism
chemical_list: D014874:Water Pollutants, Chemical; D004008:Diclofenac
keywords: Diclofenac; LC-MS/MS; Metabolite; Pharmaceuticals; Photoproduct; QuEChERS