A reliable and sensitive procedure is presented for the analysis of erythromycin (ERY) and oleandomycin (OLE) in food of animal origin, such as meat, liver, kidney, raw milk and egg. The method is based on a solid-phase extraction clean-up with a cation exchange cartridge, a 9-fluoromethylchloroformate (FMOC) precolumn derivatization and a separation by HPLC with fluorometric detection.