A selective pressurized liquid extraction procedure (SPLE) was developed for a fast determination of polychlorinated biphenyls in sediment. The final method was performed at 100 degrees C with heptane/dichloromethane (90:10, v/v) as extraction solvent for 2x5 min. Sulfuric acid impregnated silica was placed downstream of the sample in the extraction cell to remove interfering components. This simultaneous extraction/clean-up was performed in 20 min, with an average congener recovery of 92% compared to a classical 24 h Soxhlet methodology and 2 h of external manual clean-up.