The fluorescence characteristics of acid degraded product of oxytetracycline with aluminium(Ⅲ) in micellar system has been studied.The experiment indicated that oxytetracycline reacts with hydrochloric acid and produces more strong fluorescent species.After CTMAB and aluminium(Ⅲ)are added in this species,its fluorescence intensity can be enhanced greatly in pH 7.20 Na2HPO4-KH2PO4 buffer solution.Based on this,a new fluorimetric method involving acidic degradation and enhancement by surfactant and aluminium(Ⅲ)is proposed for the determination of oxytetracyline.The maximum excitation and emission wavelengths are 392nm and 492nm,respectively.The fluorescence intensity is proportional to the concentration of oxytetracycline over the range of 2.01×10-8mol/L^2.10×10-6mol/L with the detection limit of 1.0×10-8 mol/L.The method has been used to the determination of oxytetracycline in tablets with satisfacoty results.