Method development for the simultaneous determination of polybrominated, polychlorinated, mixed polybrominated/chlorinated dibenzo-p-dioxins and dibenzofurans, polychlorinated biphenyls and polybrominated diphenyl ethers in fish

Abstract

An analytical methodology was developed for simultaneous determination of five groups of persistent organic pollutants (POPs) including polybrominated, polychlorinated and mixed brominated–chlorinated dibenzo-p-dioxins and dibenzofurans (PBDD/DFs, PCDD/DFs and PXDD/DFs, respectively), polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) in fish samples. The presented analytical approach was based on well established and robust method for determination of PCDD/DFs and PCBs, which was augmented with gas chromatography coupled to high resolution mass spectrometry (GC–HRMS) to include PBDEs, as well as poorly investigated PBDD/DFs and PXDD/DFs at toxicologically significant levels. Intensive clean-up and fractionation procedures in combination with optimized instrumental parameters provided reliable detection and quantification of these compounds. The application of 13C12-labeled surrogates of analyzed compounds allowed the internal standardization and accurate measurement of selected contaminants. The developed procedure was validated while taking into account the Commission Regulation (EU) 252/2012 requirements for PCDD/DFs and PCBs, and was used to measure the occurrence of priority POPs in Baltic wild salmon.