A method has been developed for the determination of trimethylselenonium (TMSe) Ion and selenite (Se032™) Ion In urine by anion exchange chromatography, selectively eluting TMSe and Se032'. Since the recoveries are quantitative, a method of additive spikes Is employed to determine TMSe and Se032" Ion concentrations In urine specimens. The TMSe and Se032-chromatographic elutions were collected In vials, Irradiated with neutrons, and radloassayed for 77mSe activity. The limit of detection Is 10 ng of Se as TMSe or Se032"/mL of urine. Thirteen urine specimens from normal subjects were analyzed for TMSe, Se032™, and total selenium concentration.