Although a wide variety of compounds are deposited during the smoking process, much more attention has been given to phenols and polycyclic aromatic hydrocarbons (PAHs). However, even though phenols have an important role to play as food antioxidants, some PAHs have cytotoxic and mutagenic effects. In the present work, two fish species differing in composition (dolphinfish ( Coryphaena hippurus) and sardine ( Sardina pilchardus)) were salted and cold-smoked. Two different smoking treatments were selected in order to compare phenol content and muscle antioxidant activity employing the ferric reducing power (FRAP) method. Both smoking treatments increased fish lipid oxidation stability compared with the salted muscle. The characterization of the volatile components of the headspace of the more intensely processed smoked products was carried out by SPME/GC/MS, which revealed the presence of typical phenol and carbonyl derivatives, as well as some oxidation products and PAHs of low molecular weight. PAH composition was further investigated by extracting and identifying the PAHs by GC/MS. Neither benzo(a)pyerene nor other high molecular weight PAHs were detected, naphthalene and its derivatives being the most abundant compounds in the smoked products.