A new method for the simultaneous determination of PAHs and NDL-PCBs in fish and fish products was developed and validated using a GC-SQ-MS system. The efficacy of different solvents for a quantitative extraction was studied, as was the efficacy of different sorbents for sample clean up. The developed method, which includes extraction by DCM and sample clean up by SPE using Isolute® SI cartridges, was statistically validated at two concentration levels by assessing: accuracy, precision, limit of quantification, limit of detection and matrix effect. The method was used for analysing fresh, frozen and smoked fish products from the Greek retail market. None of the samples examined showed results above the maximum limits set by EU regulations.