Gas chromatography–mass spectrometric determination of polybrominated diphenyl ethers in complex fatty matrices from aquaculture activities

• Published in: Analytica chimica acta Vol. 664; no. 2; pp. 190 - 198
• Main Authors: Nácher-Mestre, Jaime, Serrano, Roque, Hernández, Félix, Benedito-Palos, Laura, Pérez-Sánchez, Jaume
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 07.04.2010; Elsevier
• Subjects: Analytical chemistry; Animals; Aquaculture; Aquaculture matrices; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, High Pressure Liquid; Clean-up; Ethers; Exact sciences and technology; Fatty samples; Fish; Fish Oils - chemistry; Fish Products - analysis; Fishes - metabolism; Gas chromatographic methods; Gas chromatography; Gas Chromatography-Mass Spectrometry - methods; Halogenated Diphenyl Ethers - analysis; Halogenated Diphenyl Ethers - chemistry; Halogenated Diphenyl Ethers - isolation & purification; Ionization; Linseed Oil - chemistry; Mass spectrometry; Mathematical analysis; Matrices; Matrix methods; Other chromatographic methods; Polybrominated diphenyl ethers; Solid Phase Extraction; Spectrometric and optical methods; Gas chromatography; Polybrominated diphenyl ethers; Aquaculture matrices; Mass spectrometry; Clean-up; Fatty samples; Capillary column; Solid phase extraction; Vegetables; HPLC chromatography; Lipids; Identification; Oils and fats; Silica; Sulfuric acid; Thin film; Chemical enrichment; Sample preparation; Efficiency; Pisces; Quantitative analysis; Ether; Sample; Use; Elimination; Interference; Chemical ionization; Thickness; Vertebrata; Animal; Acid digestion; Negative ion; Application
• ISSN: 0003-2670; 1873-4324
• DOI: 10.1016/j.aca.2010.02.015

Gas chromatography coupled to mass spectrometry in negative chemical ionization mode (GC–(NCI)MS) has been applied to the quantification and reliable identification of polybrominated diphenyl ethers (PBDEs) in animal and vegetable samples from aquaculture activities. Matrices analyzed included fish fillet, fish feed, fish oil and linseed oil, their fat content ranged from 5% to 100%. Solid-phase extraction (SPE) (using Florisil and silica cartridges) and normal-phase high performance liquid chromatography were tested for an efficient clean-up in order to obtain sample extracts free of interfering compounds. Combining sulphuric acid digestion and SPE with Florisil led to the highest efficiency in the elimination of interferences from the extracts. The sample procedure developed, together with the application of GC–(NCI)MS for measurement, led to the satisfactory determination of PBDEs at μg kg −1 levels in complex aquaculture matrices with high lipid content. The use of a short and thin film-thickness fused-silica capillary column allowed to determine the problematic BDE 209 with satisfactory results. Three m/ z ions were acquired for each analyte, which ensured a reliable identification of compounds detected in samples.