Suitability of selective pressurized liquid extraction combined with gas chromatography–ion-trap tandem mass spectrometry for the analysis of polybrominated diphenyl ethers

A one-step extraction and clean-up method using pressurized liquid extraction (PLE) (selective PLE) combined with gas chromatography–ion-trap tandem mass spectrometry (GC–ITMS–MS) was evaluated for the analysis of polybrominated diphenyl ethers (from tri- to hepta-PBDEs) at low concentrations in fish and shellfish samples. To this end, the performance of an on-line PLE extraction/clean-up method and of a classical Soxhlet extraction and clean-up method using a multi-layer modified silica column were compared. The two sample treatment methods provided similar results, although an important reduction in the sample treatment time (40 min per sample) was achieved using the selective PLE method. In addition, the suitability of the PLE combined with GC–ITMS–MS method was evaluated by comparing the results obtained in the analysis of fish samples with those obtained by gas chromatography–high resolution mass spectrometry (GC–HRMS). Good agreement between both techniques was obtained with differences between the mean values of less than 16%. The selective PLE method coupled to GC–ITMS–MS produced accurate results for PBDE determination with low limits of detection (1.0–16.8 pg g−1 wet weight) and quantification (3.1–51 pg g−1 wet weight) as well as good precision (RSD < 16%). This method has been applied to the analysis of PBDEs in fish and shellfish samples collected at fish markets in Catalonia (NE Spain).