A fluorometric method of Tb-SSA-EDTA-surfactant complex for determining salicylic acid in serum and urine is proposed. This method is fast, simple, sensitive in determining sallicylate ion in aqueous medium. Protein removal from serum is not required. 1.0 × 10−-4M- 1.0 × 10−-2M of salicylic acid in samples can be determined by the proposed procedure. The percentage of recovery was satisfactory. This procedure can be used in emergency toxicology.