A new and rapid off-line LC-LC method was proposed for isolation and purification of PAHs from oil and lipidic extracts. The whole procedure requires less than 2 h with a minimum contribution of work by the operator and can be easily automated. Besides, the advantages of the method includes a large reduction of solvent volumes and sample manipulation. Recoveries are better than those obtained by using traditional sample preparation procedure including a liquid liquid partition step followed by SPE. Recovery and repeatability test confirmed that a precise and reproducible quantification of PAHs in oil samples can be easily achieved by this method.