A new spectrophotometric procedure is described for the determination of ppm concentrations of adrenaline. The procedure is based on formation of Tris(O-phenanthroline)iron(II) complex (ferroin) upon reaction of adrenaline with an iron(III)-O-phenanthroline mixture in slightly acidic medium. The ferroin complex is then spectrophotometrically measured at 510 nm. In addition to being facile and rapid, the procedure is sufficiently selective and accurate, being particularly suitable for the assay of adrenaline in pharmaceutical formulations; the standard deviation didnot exceed 0.64%.