An analytical method using GC/MS was developed for the determination of 11 alkylphenols and 2,4-dichlorophenol (2,4-DCP) residues in various foods. The phenolic compounds were extracted with 50% diethyl ether-hexane after the alkaline decomposition of food samples. The extracts were cleaned up on an acidic alumina column and a SAX cartridge. The phenolic compounds were derivatized with heptafluorobutyric anhydride and the derivatives or parent compounds were determined by GC/MS (SIM or SCAN). The method was applied to determine alkylphenols and 2,4-DCP residues in 190 food samples purchased from markets. 4-Nonylphenol was found in some fish, meat and vegetables at the levels of 10-723 ng/g, 9-180 ng/g and 7-131 ng/g, respectively. In addition, 2,4-DCP was detected in some vegetables (2-17 ng/g)