A direct derivative, D1 i.e. dA/dλ, spectrophotometric procedure for simultaneous determination of diethylamine salicylate and methyl nicotinate in their binary mixtures and in ointments has been investigated. Good percent mean recoveries, 99.68 ± 0.58 & 99.71 ± 0.27 and 100.85 ± 0.21, could be obtained for diethylamine salicylate at 303 nm & 236 nm and methyl nicotinate at 224 nm, in order, added to ointment. The band overlapping in the first order due to the coexisting parabens, main additive, and the water-washable ointment base occurs sufficient away from those wavelengths chosen for the direct D1-measurement of both drug substances.