Determination of polybrominated diphenyl ethers and polychlorinated biphenyls in fishery and aquaculture products using sequential solid phase extraction and large volume injection gas chromatography/tandem mass spectrometry

•Lab made SPE cartridges in tandem mode eliminated large lipids in extracts.•LVI-GC–MS/MS was optimized with high sensitivity and selectivity.•New MRM transitions were proposed for the measurement of PBDEs and PCBs.•The method was successfully applied in CRM sample and in real samples.

A new method was developed to determine polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) in fishery and aquaculture products. Samples were extracted by an accelerated solvent extraction system and cleaned up by sequential solid phase extraction (SPE) including dispersive SPE (D-SPE) and tandem SPE. PBDEs and PCBs were analyzed by a large-volume injection gas chromatography triple quadrupole mass spectrometry (LVI-GC–QqQ-MS/MS). Good linearity (R2 ≥ 0.9958) was achieved. Method detection limits (MDLs) were 0.16–3.3 pg g−1 (wet weight, ww) for PBDEs and 0.13–0.97 pg g−1ww for PCBs. Mean recoveries were 60–140% with relative standard deviations (RSDs) of less than 20% in weever fish, scallop and shrimp samples spiked at a lower level of 13–31 pg g−1 ww and a higher level of 50–125 pg g−1 ww. Certified reference materials were analyzed with acceptable results. The method reduced solvent consumption, analytical time and labor, and is suitable for the routine analysis of PBDEs and PCBs in fishery and aquaculture products.