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Poster De Conférence Année : 2012

Development and validation of a multiresidue method for the analysis of priority and emerging pollutants in biota

Développement et validation d'une méthode multirésidus pour l'analyse des polluants prioritaires et émergents dans le biote

Résumé

Monitoring of water quality has become a main challenge in Europe since the implementation of the Water Framework Directive (WFD, /2000/60/CE) which aim is to obtain a good ecological and chemical status for European waters. The European Commission (EC) Daughter Directive 2008/105/EC and the recent proposal for a Directive 2011/0429/EC recommend the use of biota or sediment, instead of water, as a preferential matrix for the monitoring of hydrophobic substances (i.e., with logKow >3). In this context, we developed a method to determine 25 emerging and priority pollutants in aquatic biota: hexachlorobenzene (HCB), hexachlorobutadiene (HCBD), alpha-hexabromocyclododecane (HBCD), 3 hormones (estrone (E1), beta-estradiol (E2), alpha-ethinylestradiol (EE2)), 4 perfluorinated compounds (PFCs: PFOA, PFDA, PFDoA, PFOS), and 6 polybromodiphenylethers (PBDE-28, -47, -99, -100, -153, -154) bisphenol A (BPA), tetrabisphenol A (TBBPA), and 7 indicator polychlorobiphenyl compounds (PCB-28, -52, -101, -118, -138, -153, -180). Among these compounds, 6 PBDEs, HCB and HCBD are priority substances listed in Annex II of the Daughter Directive 2008/105/EC; and PFOS and BPA are optional substances listed in Annex III of the same directive. HBCD (isomer alpha) was recently proposed as a priority substance in Annex I of the proposal Directive 2011/0429/EC. After collection, fish tissues were freeze-dried and finely ground. Then, 0.5g of dried fish was extracted by Pressurized Fluid Extraction (PFE) with a solvent mixture cyclohexane/acetone. The main difficulty was to overcome the matrix effects by removing lipids contained in the samples. Optimization of the method showed that the best solution was to carry out a centrifugation and eventually acidification, before cleaning up the extract by solid-phase extraction (SPE) performed on Florisil cartridge. Extracts were then analysed by gas chromatography with electron capture detector or by liquid chromatography coupled to tandem mass spectrometry, according to the physicochemical properties of molecules. Through illustrations (chromatograms, recoveries, …), we discuss the experimental solutions developed to minimize matrix effects. Then, this method was validated on 5 different matrices (i.e., mollusc, crustacean, 3 species of fishes) via the determination of linearity, repeatability and robustness. The limits of quantification (LOQ) were about 1 ng.g-1dry weight. The method was assessed by applying the analytical method to 50 aquatic biota samples from the Rhône and the Saône Rivers. PBDEs, PCBs and HCBD were the most frequently quantified substances, with concentrations ranging from 2 to 160 ng.g-1 dry weight.
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Dates et versions

hal-02597720 , version 1 (15-05-2020)

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Fabienne Serveto, E. Lionard, Marina Coquery, Cecile Miege. Development and validation of a multiresidue method for the analysis of priority and emerging pollutants in biota. NORMAN Workshop "Occurence, fate and effects of emerging pollutants in the environment - chemical analysis and toxicological assessment", Nov 2012, Amsterdam, Netherlands. pp.1, 2012. ⟨hal-02597720⟩

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