A new method is described for analyzing a binary mixture of analgin and adamon using extractive and derivative spectrophotometry. In the method, analgin and adamon both were extracted into chloroform as an ion-pair with thymol blue from their aqueous solution buffered to pH 3.6. Determination of these drugs was performed by reading the dA/dλ values at 600.0 nm and 310.5 nm in the first derivative spectra of the chloroform layer. Relative standard deviations of the method are 0.10% for analgin and 0.81% for adamon. The method was successfully applied to an injection solution containing these two active ingredients.