A reversed-phase high-performance liquid chromatography (RP-HPLC) with ultraviolet detection was established for the determination of phenol, catechol, hydroquinone, and p-benzoquinone in the reaction solution of catalytic oxidation of phenol using hydrogen peroxide as the oxidant and copper-doped FeSBA-15 zeolite as the catalyst. Separation was accomplished on a reversed-phase C 18 column, and the elution condition was optimized by changing the composition of the mobile phase. A good resolution of all of the relative components in the reaction solution was achieved when the mobile phase was methanol-water-1% acetic acid aqueous solution = 10:50:40 (v/v/v). The concentrations of phenol, catechol, hydroquinone, and p-benzoquinone were determined in 11 different reaction solutions by the external standard method. The proposed HPLC method was simple, accurate, reliable, and suitable for tracing the amount of target products during the catalytic oxidation reaction of phenol. The results can provide data support for evaluating the