Surface coastal sediments (0-10 cm) collected from three natural environments on the Spanish Northern Atlantic Coast were analyzed so as to determine concentrations of 6 marker polychlorinated biphenyls (PCBs), 12 dioxin-like PCBs (dl-PCBs) and 17 polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans (PCDD/Fs). An analytical procedure based on Soxhlet extraction followed by an automated cleanup and final high-resolution gas chromatography coupled to high-resolution mass spectrometry was applied for the determination of the persistent organic pollutants. Marker PCB levels ranged from 385.5 to 4,060.9 pg/g dry weight (d.w.) showing a similar congener pattern in all sediments dominated by the less volatile congeners PCB 153 and PCB 138. Linear correlations were found between marker and dl-PCBs. Toxicity equivalent values were calculated for PCDD/Fs and dl-PCBs reaching its maximum at 0.52 pg WHO 1998 -TEQ/g d.w., with an average dl-PCBs contribution on the toxicity of the samples of 75%, and showing to be in good agreement with background levels in the North-East Atlantic Ocean Coasts of nearly 1 pg/g WHO 1998 -TEQ d.w. Dimensionless environmental quality criteria were much lower than 1 indicating the low probability to induce ecotoxicological impacts.