Abstract: Fluorospectrophotometry and chemical method were applied to the determination of sodium lauryl benzenesulfate (SDBS) and alkanolamide (AKNM) in the complex systems. An amount of β-cyclodextrin with its molar concentration approximately equivalent to that of the SDBS in the sample solution molar of SDBS was added to enhance the fluorescence intensity of SDBS and to reduce significantly the interference of alkanolamide to SDBS. SDBS in the complex solution was determined by fluorospectrophotometry, giving values of recovery foun by standard addition method in the range of 101%-102%. After the sample solution was hydrolyzed for 10 h with sulfuric acid added as catalyst, content of AKNM was determined by chemical method, giving values of recovery found by standard addition method in the range of 98.2%-98.9%.