Abstract: Based on the catalytic action of Cu(Ⅱ) on the oxidation of indigo carmine in ammoniacal buffer medium, leading to enhancement of fluorescence of the reaction system, a fluorophotometric method for determination of Cu(Ⅱ) was proposed. Linear relationship was found between values of ΔF (F-F0) measured at wavelengths of 320 nm (λex) and 391 nm (λem) and concentration of Cu(Ⅱ) in the range of 0.2-100 μg·L-1. Limit of detection (3σ) of the method found was 0.05 μg·L-1. The proposed method was used in the determination of Cu(Ⅱ) in samples of rice, flour and tea, giving values of recovery ranged from 96.2% to 104.9%, and of RSD′s (n=5) ranged from 0.72% to 1.5%.