Development and validation of a specific and sensitive gas chromatography tandem mass spectrometry method for the determination of bisphenol A residues in a large set of food items.

BPA-containing products are widely used in foodstuffs packaging as authorized within the European Union (UE no. 10/2011). Therefore, foods and beverages are in contact with BPA which can migrate from food contact material to foodstuffs. An accurate assessment of the exposure of the consumers to BPA is crucial for a non-ambiguous risk characterization. In this context, an efficient analytical method using gas chromatography coupled to tandem mass spectrometry (GC-MS/MS), in the selected reaction monitoring (SRM) mode, was developed for the quantification of BPA in foodstuffs at very low levels (<0.5µgkg(-1)). A standard operating procedure, based on the combination of two successive solid phase extractions (SPE), was developed for various liquid and solid foodstuffs. The use of (13)C12-BPA as internal standard allowed accurate quantification of BPA by isotopic dilution. Control charts based on both blank and certified materials have been implemented to ensure analytical data quality. The developed analytical method has been validated according to in-house validation requirements. R(2) was better than 0.9990 within the range [0-100µgkg(-1)], the trueness was 4.2%. Repeatability and within-laboratory reproducibility ranged from 7.5% to 19.0% and 2.5% to 12.2%, respectively, at 0.5 and 5.0µgkg(-1) depending on the matrices tested for. The detection and quantification limits were 0.03 and 0.10µgkg(-1), respectively. The reporting limit was 0.35µgkg(-1), taking into account the mean of the laboratory background contamination. The global uncertainty was 22.2% at 95% confidence interval.

Levels and trends of the emerging contaminants HBCDs (hexabromocyclododecanes) and PFCs (perfluorinated compounds) in marine shellfish along French coasts.

The levels and congener patterns of HBCDs (hexabromocyclododecanes) and PFCs (perfluorinated compounds) were determined in filter-feeding molluscs collected in 2008 and 2010 along the coasts of mainland France. α-HBCD and PFOS (perfluorooctane sulfonate) were detected in all samples, revealing widespread contamination of the coastal environment by these emerging contaminants. The spatial distribution of Σ-HBCD concentrations showed higher median levels in samples from the Mediterranean Sea and English Channel respectively, i.e. 0.19 ng g(-1) wet weight (ww) and 0.08 ng g(-1) ww, related to high anthropogenic pressure from urban and industrial activities, while the median concentration was 0.05 ng g(-1) ww in samples from the Atlantic coast. Among PFCs, PFOS was the only compound detected in all samples and PFDA (perfluorodecanoic acid) was the second most frequently-detected compound. PFOS median concentrations were 0.18 ng g(-1) ww, 0.09 ng g(-1) ww and 0.04 ng g(-1) ww in samples from the English Channel, the Atlantic coast and the Mediterranean coast respectively. The highest PFOS concentration was found in the Loire estuary, possibly related to local industrial activities. The Mediterranean samples showed a different pattern, with predominant long-chain PFCAs (perfluorocarboxylic acids), suggesting the presence of alternative sources on the Mediterranean coast. The temporal trends studied in archived samples from the Seine estuary site showed a significant exponential increase in HBCD concentrations between 1981 and 2011, with a doubling time of 7 years, while PFOS levels underwent a significant linear decrease over time. These trends are coherent with current regulations on the use of these compounds. The results presented in this paper provide the first data on the contamination of the French coastal marine environment by the selected emerging compounds, and constitute a reference for the future monitoring of French coastal contamination by emerging contaminants.