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This work presents a simple and sensitive flow injection fluorimetric method for the determination of carbamazepine (CBZ) in pharmaceutical samples. It is based on the fluorescence signal measurement of the product generated by photoinduced (λ ex = 251 nm; λ em = 434 nm) using a flow injection manifold containing an on-line homemade photoreactor. In order to optimize the experimental setup, the variable conditions were studied using a multivariate optimization method, thus finding the set of optimum parameters according to the evaluated responses (sensitivity and sampling frequency) and minimizing the number of experiments performed. Under optimal experimental conditions, linear relationship with good correlation coefficient (0.9956) was found between the fluorescence intensity and CBZ concentration in the range of 0.13-40 µg•mL −1. The limit of detection was 0.04 µg•mL −1. The precision of the method was satisfactory; the values of relative standard deviations were better than 4.36%. The proposed method was validated and successfully applied to the determination of CBZ in pharmaceuticals with good accuracy; being the recovery values from 89.45%-112.20%.