A simple gas chromatographic assay of the psycho-stimulant pemoline in human urine, plasma and saliva has been developed. Instead of direct extraction of the drug from urine, plasma and saliva, it is hydrolyzed to 5-phenyl-2,4-oxazolidine-dione with 1 N hydrochloric acid. After extraction this compound is methylated with diazomethane and determined by gas-liquid chromatography using a capillary SCOT column with a mixed stationary phase, a solid injection system and a nitrogen-selective detector. 5-Phenyl-2,4-oxazolidinedione, which was also found to be a metabolite of pemoline, could be determined quantitatively in human urine.