The work is devoted to the treatment of wastewater from pharmaceuticals by enhanced oxidation. Some studies have shown the high degree and speed of pharmaceutical degradation under the action of a hydroxyl radical formed by the combined action of UV and H2O2 (enhanced oxidation, which was fully confirmed by a decrease in absorption in the UV spectrum. This paper shows that, unlike spectrophotometry, the spectrofluorimetry method can be used in the analyzing the process of destruction of hard-to-degrade pharmaceuticals. The object of the study was synthetic alkaloid vinpocetine, which has an indole core. Vinpocetine solutions were irradiated in a laboratory setup which included a TUV 30w / GTV low-pressure argon-mercury lamp (Philips) for 5–15 min, and also irradiated for 1-10 minutes after adding hydrogen peroxide at a concentration of 100 mg / L). The spectrophotometry method showed an increase (instead of a decrease) in the absorption spectra with an increase in the duration of UV irradiation. Under the same conditions, the spectrofluorimetry method recorded a decrease in the signal intensity in the registration and excitation spectra, and under enhanced oxidation, the appearance of new bands characteristic of the phenolic group.