Abstract: Based on the derivatization of benzoyl peroxide by p-hydroxyphenylacetic acid to give a fluorescent dimer in a basic medium of pH 10.2 with hemin as simulated enzymic catalytic agent and on the fluorescence property of the derivate as shown by its fluorescence spectrum at the wavelengths of 310 nm (λex) and 400 nm (λem), a fluorophotometric method for determination of benzoyl peroxide in wheat flour was proposed. Linear relationship was found between values of fluorescence intensity and mass concentration of benzoyl peroxide in the range of 0.05-50 mg·L-1, with detection limit (3s/k) of 1 mg·kg-1. The proposed method was used in the determination of benzoyl peroxide in wheat flour, giving values of recovery ranged from 98.0% to 102%, and RSD′s (n=6) ranged from 1.6% to 2.2%.