Two new spectrophotometric methods for the simultaneous determination of analgin and hyoscine N-butyl bromide in their binary mixture are described. In the first method, derivative spectrophotometry, the determination of these drugs were performed by measuring the dA/dλ values at 291.8 nm and 219.8 nm in the first derivative spectra of the mixture for analgin and hyoscine N-butyl bromide respectively. The relative standard deviation of the method was found to be 0.08% for analgin and 0.77% for hyoscine N-butyl bromide. In the second method, the determination of these compounds in mixture was realized by precipitating hyoscine N-butyl bromide with ammonium reineckate at pH 6.0 selectively and reading the absorbance of the solution of the precipitate in acetone at 532.2 nm for hyoscine N-butyl bromide and, by measuring the dA/dλ values at 306.2 nm in the first derivative spectra of the remaining solution for analgin. The relative standard deviation of the method was found to be 0.75% for hyoscine N-butyl bromide and 0.10% analgin. These two methods have been succesfully applied to a sugar-coated tablets containing hyoscine N-butyl bromide and analgin.