Fast and environmental-friendly methods for the determination of polybrominated diphenyl ethers and their metabolites in fish tissues and feed

Abstract

Environmental-friendly, cost-effective and fast methods were developed and validated for the analysis of seven PolyBrominated Diphenyl Ethers (PBDEs) and eight methoxylated PBDEs (MeO-PBDEs) in three distinct seafood matrices (muscle, liver and plasma) and feed using a Quick, Easy, Cheap, Efficient, Rugged and Safe (QuEChERS) extraction approach for solid samples and a Dispersive Liquid-Liquid Microextraction method (DLLME) for plasma. Instrumental analyses were performed with gas chromatography coupled to triple quadrupole mass spectrometry using electron impact source (GC-EI-MS/MS) and negative ion chemical ionization (GC-NICI-MS) to assess BDE-209. Statistical validation showed recoveries for all target substances near 100% with average Relative Standard Deviation (RSD) lower than 9% and recovery standards higher than 65% (average RSD below 20%). Average calculated Method Detection Limits (MDLs) were lower than 65 pg·g−1 wet weight (WW) for muscle, 5.35 ng·g−1 WW for liver, 4.50 ng·g−1 WW for feed, and 0.60 ng·mL−1 for plasma samples. Quality assurance and quality control practices were comprehensively described. Methods scored high in an analytical Eco-scale, thus being classified as “an excellent green analysis”. Finally, real seafood samples collected in local markets and local fishermen were analyzed. Positive samples presented both PBDEs and MeO-PBDEs in safe amounts (0.28–125.80 ng·g−1 WW) for human consumption.