The interest in the physiological roles and bioactivities of plant phenols has increased over the past decades. In seaweeds, many investigations have dealt with phenolic compounds of Phaeophyceae (phlorotannins), even though little is known so far about the ecophysiological variations of their pool or their biosynthetic pathways. We describe here a simple procedure based on the use of water-organic solvent mixtures for the extraction of phlorotannins. Crude extracts are semi-purified and fractionated by separating methods based on both the polarity and the molecular size of compounds. Phenols are then quantified by the Folin-Ciocalteu method and their radical-scavenging activity is characterized using the DPPH test. All along the purification process of phenolic compounds, the efficiency of separation is assessed by 1H-NMR.