Development and optimization of gas chromatography coupled to high resolution mass spectrometry based method for the sensitive determination of Dechlorane plus and related norbornene-based flame retardants in food of animal origin

An analytical method has been developed for the trace determination of 10 dechlorane-related compounds (DRCs) in food products by gas chromatography - high resolution mass spectrometry (GC-HRMS). The highest sensitivity of this instrumental analysis method was achieved by selection of the GC column type, optimization of the heated zones within the instrument, and adjusting the electron impact energy. The efficiency of solid phase extraction as clean-up procedure was also optimized. Two different types of cartridges - neutral silica gel and Florisil®, as well as seven organic solvents or their mixtures - n-hexane, cyclohexane, acetone, toluene, n-hexane/ethyl acetate, n-hexane/acetone, and n-hexane/dichloromethane - were evaluated. The analytical method was characterized as selective, precise, accurate, and linear over the concentration ranges from 1.00 to 100 pg μL−1 for DRCs. Ultra-trace level sensitivity was achieved with the instrumental limits of quantification (i-LOQs) varying from ∼0.01 pg to ∼ 1 pg and method limits of quantification (m-LOQs) by the analysis of 10 g of sample varying from ∼0.04 to ∼ 5 pg g−1. The developed method was successfully applied for the analysis of food samples and the analyses revealed the presence of majority of selected DRCs, with the Dechlorane Plus (DP) isomers occurring to a greater extent, pointing to the highest levels in cod liver and other fish products.