Simultaneous analysis of historical, emerging and novel brominated flame retardants in food and feed using a common extraction and purification method.

Brominated Flame Retardants (BFRs) are still widely used for industrial purposes. These contaminants may enter the food chain where they mainly occur in food of animal origin. The aim of our work was to provide a unique method able to quantify the widest range of BFRs in feed and food items. After freeze-drying and grinding, a pressurized liquid extraction was carried out. The extract was purified on acidified silica, Florisil® and carbon columns, the four separated fractions were analyzed by gas and liquid chromatography coupled to high resolution and tandem mass spectrometry. Isotopic dilution was preferentially used when commercial labelled compounds were available. Analytical sensitivity was in accordance with the expectations of Recommendation 2014/118/EU for PBDEs, HBCDDs, TBBPA, TBBPA-bME, EHTBB, BEHTEBP and TBBPA-bME. Additional BFRs were included in this analytical method with the same level of performances (LOQs below 0.01 ng g-1 ww). These are PBBs, pTBX, TBCT, PBBz, PBT, PBEB, HBBz, BTBPE, OBIND and T23BPIC. However, some of the BFRs listed in Recommendation 2014/118/EU are not yet covered by our analytical method, i.e. TBBPA-bOHEE, TBBPA-bAE, TBBPA-bGE, TBBPA-bDiBPrE, TBBPS, TBBPS-bME, TDBPP, EBTEBPI, HBCYD and DBNPG. The uncertainty measurement was fully calculated for 21 of the 31 analytes monitored in the method. Reproducibility uncertainty was below 23% in isotopic dilution. Certified reference materials are now required to better characterize the trueness of this method, which was applied in the French National Control Plans.

Field investigation to determine the environmental source of PCBs in a pig farm.

During a national monitoring plan, a pork fat sample was declared non-compliant for the sum of dioxins and PCB-DL (EU regulation). The National Reference Laboratory together with competent authorities conducted extended investigations to determine rapidly the contamination source at the farm level. A range of samples (n = 129), representative of potential contamination sources, was selected for further characterization (fat, feed, materials, dust, soil) and was analyzed for PCDD/Fs and DL-PCBs by GC-HRMS. A hot spot was localized in the farm, which corresponded to a pre-feed storage tank, the paints of which presented huge DL-PCB concentrations (>1 × 106 pg g-1), responsible for the contamination. The present case report describes a new source of PCB contamination, previously undescribed.