In this study, bench-scale experiments were conducted to examine the UV/H2O2 oxidation of 17α-ethynyestradiol (EE2) in water in a batch operation mode. The EE2 degradation exhibited pseudo-first-order kinetics, and the removal was ascribed to the production of hydroxyl radicals (•OH) by the UV/H2O2 system. Typically, the EE2 oxidation rate increased with increasing UV intensity and H2O2 dose, and with deceasing initial EE2 levels and solution pH. At EE20 = 650 µg/L, UV intensity = 154 µW/cm2, H2O2 = 5 mg/L, and neutral pH, the UV/H2O2 treatment was able to remove 90% of the EE2 content within 30 min. Four anions commonly present in water were found to inhibit EE2 degradation to varying degrees: > > Cl− > . Our results demonstrate that the described UV/H2O2 process is an effective method to control EE2 pollution in water.