RESUMO
An analytical method was developed and validated for the analysis of 32 halogenated flame retardants (HFRs), including 13 polybrominated diphenyl ethers (PBDEs), 9 dechlorane-related compounds (DRCs) and 10 of the so-called alternative BFRs in food samples of animal origin. Gas chromatography (GC) coupled with magnetic sector high resolution mass spectrometry (HRMS) was used for the instrumental analysis. Intralaboratory validation of the developed method was performed in terms of recovery, repeatability, linear calibration ranges, instrumental and method limits of quantitation (i-LOQ and m-LOQ). Where possible, trueness was verified by the analysis of reference materials (RMs). For analytes with available isotopically labeled surrogates, recoveries in the range of 70-120% and repeatability rates below 20% were observed, while for compounds quantitated using absolute calibration the values of recovery ranged from 59 to 153% and the repeatability in terms of RSDs was in the range of 1-26%. The values measured for the four analyzed RMs agreed with the provided consensus values, revealing that the recovery of reference concentrations for compounds with assigned consensus values was in 72-119% range. The elaborated method met the sensitivity criteria according to the Commission Recommendation, 2014/118/EU on the monitoring of BFRs in food products. The developed method was successfully applied for the analysis of numerous food samples. The analyses revealed ubiquitous presence of PBDEs and the majority of DRCs in the analyzed samples, while alternative BFRs were detected only occasionally.
