title: MicroQuEChERS-nanoliquid chromatography-nanospray-tandem mass spectrometry for the detection and quantification of trace pharmaceuticals in benthic invertebrates.
abstract: Due to industrialization and the use of chemical products in everyday life, various types of drugs and pesticides are present in our environment, which threaten and cause negative impacts on aquatic ecosystems. The consequences of these pollutants are gradually becoming visible. Recent evidence confirms that long term exposure to environmental pharmaceutical concentrations can induce adverse effects in aquatic vertebrates and invertebrates such as reproductive impairments and collapse wild populations. Consequently, one of the challenges of environmental science is to evaluate the associated risks. In this context, a new methodology has been developed using nano-LC-nano-ESI MS/MS to quantify traces of two pharmaceuticals (a neuropharmaceutical drug, fluoxetine, and an anticonvulsant drug, carbamazepine) in two molluscs, Potamopyrgus antipodarum and Valvata piscinalis, which are both prosobranch gastropods. A simple and quick extraction method was developed based on a modified and miniaturized version of the QuEChERS method. The procedure involves the extraction of approximately 10 mg of wet mollusc tissue by 500 µL of a mixture of acetonitrile/water/hexane (50/20/30) and 100 mg of buffer salt. Thus, the extraction step was carried out on an individual scale. The sensitivity of this method allowed for the detection of levels as low as 18 ng/g and 128 ng/g for carbamazepine and fluoxetine, respectively, with recoveries of greater than 85% for the two targeted compounds. This method was then applied to both gastropod species exposed to fluoxetine under laboratory conditions. The results provide evidence of bioaccumulation in both P. antipodarum and V. piscinalis and reveal the inter-species differences.
authors.affiliation: Université de Lyon-Institut des Sciences Analytiques, UMR 5280 CNRS-Equipe TRACES, Université Lyon1, ENS-Lyon-5 rue de la Doua, 69100 Villeurbanne, France.
authors.forename: Alexandra
authors.initials: A
authors.lastname: Berlioz-Barbier
authors.affiliation: Université de Lyon-Institut des Sciences Analytiques, UMR 5280 CNRS-Equipe TRACES, Université Lyon1, ENS-Lyon-5 rue de la Doua, 69100 Villeurbanne, France.
authors.forename: Robert
authors.initials: R
authors.lastname: Baudot
authors.affiliation: Université de Lyon-Institut des Sciences Analytiques, UMR 5280 CNRS-Equipe TRACES, Université Lyon1, ENS-Lyon-5 rue de la Doua, 69100 Villeurbanne, France.
authors.forename: Laure
authors.initials: L
authors.lastname: Wiest
authors.affiliation: IRSTEA, UR MAEP, Laboratoire d'écotoxicologie, 5 rue de la Doua, 69009 Lyon, France.
authors.forename: Marion
authors.initials: M
authors.lastname: Gust
authors.affiliation: IRSTEA, UR MAEP, Laboratoire d'écotoxicologie, 5 rue de la Doua, 69009 Lyon, France.
authors.forename: Jeanne
authors.initials: J
authors.lastname: Garric
authors.affiliation: Université de Lyon-Institut des Sciences Analytiques, UMR 5280 CNRS-Equipe TRACES, Université Lyon1, ENS-Lyon-5 rue de la Doua, 69100 Villeurbanne, France.
authors.forename: Cécile
authors.initials: C
authors.lastname: Cren-Olivé
authors.affiliation: Université de Lyon-Institut des Sciences Analytiques, UMR 5280 CNRS-Equipe TRACES, Université Lyon1, ENS-Lyon-5 rue de la Doua, 69100 Villeurbanne, France. Electronic address: audrey.bulete@isa-lyon.fr.
authors.forename: Audrey
authors.initials: A
authors.lastname: Buleté
mesh_terms: D000818:Animals; D000927:Anticonvulsants / Q000302:isolation & purification*; D018687:Antidepressive Agents, Second-Generation / Q000302:isolation & purification*; D002220:Carbamazepine / Q000302:isolation & purification*; D002853:Chromatography, Liquid / Q000379:methods; D005473:Fluoxetine / Q000302:isolation & purification*; D049851:Gastropoda / Q000737:chemistry* / Q000378:metabolism; D059625:Liquid-Liquid Extraction / Q000379:methods; D013045:Species Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods; D014874:Water Pollutants, Chemical / Q000302:isolation & purification*
chemical_list: D000927:Anticonvulsants; D018687:Antidepressive Agents, Second-Generation; D014874:Water Pollutants, Chemical; D005473:Fluoxetine; D002220:Carbamazepine
keywords: Endocrine disruptors; Extraction; Gastropods; MicroQuEChERS; Nano-liquid chromatography; Tandem mass spectrometry; Validation