A simple, rapid and inexpensive fluorimetric method for simultaneously determining ASA and SA in a single scan of the co-existing specimen had been established. When the wavelength interval (delta lambda) is 80 nm for scaning, the amounts of ASA and AS could be quantitatively determined respectively. The fluorescence intensity was linearly related to the aspirin concentration in the range of 4.0 x 10(-6)-1.0 x 10(-4) mol x L(-1) with correlation coefficient 0.9949; the fluorescence intensity was linearly related to the salicyclic acid concentration in the range of 8.0 x 10(-7)-1.0 x 10(-4) mol x L(-1) with correlation coefficient 0.9975, the determination limit was 4.0 x 10(-7) mol x L(-1). The method is simple, rapid and inexpensive, it can be used for medicament analysis.