This article deals with the design of an unsegmented-flow injection manifold for the simultaneous determination of adrenaline and noradrenaline two structurally related compounds with overlapping spectra. An FIA manifold is proposed for the simultaneous determination in which the sample solution is directly injected into a carrier-reagent stream of aqueous NaOH. The selected wavelengths (first derivative) were 394 and 342 nm, for noradrenaline and adrenaline, respectively with an integration time of 0.4 s. The calibration graphs are linear over the range 2.0–30 ppm for both drugs. The method is applied to different synthetic mixtures of both drugs.