Simplified and rapid determination of polychlorinated biphenyls, polybrominated diphenyl ethers, and polycyclic aromatic hydrocarbons in fish and shrimps integrated into a single method

In this study, a new rapid and flexible method for the simultaneous determination of 18 key representatives of polychlorinated biphenyls (PCBs), 7 polybrominated diphenyl ethers (PBDEs), and 32 polycyclic aromatic hydrocarbons (PAHs) in fish and shrimps by gas chromatography coupled to mass spectrometry (GC–MS) was developed and validated. A substantial simplification of sample processing prior to quantification step was achieved: after addition of water to homogenized sample, transfer of hydrophobic analytes into ethyl acetate was supported by added inorganic salts. Bulk fat, contained in crude organic extract obtained by partition, was subsequently removed on a silica minicolumn. This approach enabled to process six samples in less than 1 h; moreover, the volume of an extraction solvent and consumption of other chemicals can be significantly reduced compared to, e.g., traditional Soxhlet extraction followed by gel permeation chromatography. The recoveries of target analytes were in the range of 73–120% even at the lowest spiking level (1 μg kg−1), repeatabilities (relative standard deviations, RSDs) ranged from 1 to 20%. Under optimized GC–MS conditions (time-of-flight mass analyzer, TOF), the limits of quantification (LOQs) were as follows: PCBs 0.1–0.5 μg kg−1, PBDEs 0.5 μg kg−1, and PAHs 0.05–0.25 μg kg−1. Ambient mass spectrometry employing a direct analysis in real time (DART) ion source was shown as an effective tool for fat control in extract, which is needed during the method development and examination of unknown samples prior to the analysis. Further extension of a method scope by other similar analytes is easily possible.

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► We developed a new sample preparation method for PCBs, PBDEs and PAHs analysis in fish and shrimps.
► Ethyl acetate-based extraction followed by silica minicolumn clean-up was used.
► DART–TOFMS was shown to be an effective tool for the fat control.
► GC–TOFMS enables simultaneous determination of all target analytes and potential non-target screening.