A procedure for the determination of quinaldine residue in various fish tissues is described. Homogenized tissues are extracted with hexane-ethyl ether, the extracts are concentrated by partitioning through 0.1N sulfuric acid, and the residues are measured by alkali flame ionization gas chromatography. Muscle tissues containing from 0.01 to 10.0 ppm quinaldine were successfully analyzed with recoveries from 75 to 100%.