title: Development of a multi-residue analysis of diclofenac and some transformation products in bivalves using QuEChERS extraction and liquid chromatography-tandem mass spectrometry. Application to samples from mesocosm studies.
abstract: Pharmaceuticals are ubiquitously present in the aquatic environment, mainly due to insufficient removal in wastewater treatment plants. Although these compounds are often found at trace levels in waters, long-term exposure can have negative impacts on biotic communities due to their inherent biological activity. The non-steroidal anti-inflammatory drug diclofenac (DCF) is one of the most frequently detected human pharmaceuticals in water and has recently been included in the "watch" list of the European Union. However little data are available on the detection of this substance and its transformation products in aquatic organisms. In this context, an analytical methodology has been developed to quantify traces of DCF along with its biotic and abiotic transformation products in a wild species of bivalve, the zebra mussel Dreissena polymorpha. A modified QuEChERS extraction was implemented on a small quantity of soft bivalve tissue (100mg). This was followed by liquid chromatography coupled to tandem-mass spectrometry (LC-MS/MS) with electrospray ionization in positive mode (ESI+). Whole analytical method was validated on spiked real samples, with regard to linearity (from 1 to 50 or 100ng/g depending on the target compounds, R(2)>0.99), intra-day precision (relative standard deviation (RSD)<18%), inter-day precision (RSD <25%), (recoveries 78-117%), and limits of detection and of quantification (both inferior or equal to 1ng/g). The optimized method was successfully applied to organisms collected from mesocosm experiments. Bioconcentration factors comprised between 4 and 13 were observed for DCF in the zebra mussels. To the best of our knowledge, the product 2-indolone was for the first time detected in bivalves, with levels up to 6ng/g.
authors.affiliation: Université de Lyon, Institut des Sciences Analytiques, UMR5280, CNRS, Université Claude Bernard Lyon1, ENS-Lyon, 5 rue de la Doua, 69100 Villeurbanne, France. Electronic address: gaelle.daniele@isa-lyon.fr.
authors.forename: Gaëlle
authors.initials: G
authors.lastname: Daniele
authors.affiliation: Université de Lyon, Institut des Sciences Analytiques, UMR5280, CNRS, Université Claude Bernard Lyon1, ENS-Lyon, 5 rue de la Doua, 69100 Villeurbanne, France.
authors.forename: Maëva
authors.initials: M
authors.lastname: Fieu
authors.affiliation: INERIS, Laboratoire d'écotoxicologie in vitro et in vivo, Parc Technologique Alata, BP n°2, 60550 Verneuil-en-Halatte, France.
authors.forename: Sandrine
authors.initials: S
authors.lastname: Joachim
authors.affiliation: INERIS, Laboratoire d'écotoxicologie in vitro et in vivo, Parc Technologique Alata, BP n°2, 60550 Verneuil-en-Halatte, France.
authors.forename: Alice
authors.initials: A
authors.lastname: James-Casas
authors.affiliation: INERIS, Laboratoire d'écotoxicologie in vitro et in vivo, Parc Technologique Alata, BP n°2, 60550 Verneuil-en-Halatte, France.
authors.forename: Sandrine
authors.initials: S
authors.lastname: Andres
authors.affiliation: INERIS, Laboratoire d'écotoxicologie in vitro et in vivo, Parc Technologique Alata, BP n°2, 60550 Verneuil-en-Halatte, France.
authors.forename: Patrick
authors.initials: P
authors.lastname: Baudoin
authors.affiliation: UMR-I 02 INERIS-URCA-ULH SEBIO, Campus du Moulin de la Housse, BP 1039, 51687 Reims cedex 2, France.
authors.forename: Marc
authors.initials: M
authors.lastname: Bonnard
authors.affiliation: UMR-I 02 INERIS-URCA-ULH SEBIO, Campus du Moulin de la Housse, BP 1039, 51687 Reims cedex 2, France.
authors.forename: Isabelle
authors.initials: I
authors.lastname: Bonnard
authors.affiliation: UMR-I 02 INERIS-URCA-ULH SEBIO, Campus du Moulin de la Housse, BP 1039, 51687 Reims cedex 2, France.
authors.forename: Alain
authors.initials: A
authors.lastname: Geffard
authors.affiliation: Université de Lyon, Institut des Sciences Analytiques, UMR5280, CNRS, Université Claude Bernard Lyon1, ENS-Lyon, 5 rue de la Doua, 69100 Villeurbanne, France.
authors.forename: Emmanuelle
authors.initials: E
authors.lastname: Vulliet
mesh_terms: D000818:Animals; D049872:Bivalvia / Q000737:chemistry / Q000378:metabolism*; D005591:Chemical Fractionation / Q000379:methods*; D002853:Chromatography, Liquid; D003365:Costs and Cost Analysis; D004008:Diclofenac / Q000737:chemistry / Q000302:isolation & purification* / Q000378:metabolism*; D004780:Environment, Controlled; D004784:Environmental Monitoring; D015203:Reproducibility of Results; D012449:Safety; D012997:Solvents / Q000737:chemistry; D053719:Tandem Mass Spectrometry
chemical_list: D012997:Solvents; D004008:Diclofenac
keywords: LC-MS/MS; Mesocosm; Metabolite; Pharmaceuticals; Photoproduct; QuEChERS