A GC-EI-MS/MS Method for the Determination of 15 Polybrominated Diphenyl Ethers (PBDEs) in Fish and Shellfish Tissues

Abstract

This paper describes the development and validation of an analytical method to determine 15 polybrominated diphenyl ethers (PBDEs) in fish and shellfish tissues with gas chromatography coupled to triple quadrupole mass spectrometry using electron impact source (GC-EI-MS/MS). A QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe)-like procedure was applied; the extract was cleaned up on an acidic Extrelut-NT3 column connected on top of a silica cartridge and further purified with gel permeation chromatography (GPC). The SIM acquisition proved to yield better results than traditional MRM approach for octa-, nona-, and deca-brominated congeners. The validation study was carried out in inter-laboratory conditions. The average recoveries were in the range 66–118%, with relative standard deviations generally lower than or equal to 22%. Quality assurance and quality control practices were thoroughly described and highlighted. These long and tedious practices are fundamental to obtain reliable quantitative data during food monitoring programs and, therefore, to support daily intake assessments. Finally, the procedure was applied to the analysis of marine fish samples collected in local markets. Mackerel and mullet were the most contaminated species.