Photocatalytic degradation of carbamazepine (CBZ) was investigated by hydrothermally synthesized antimony trioxide (Sb2O3)/ead oxide (PbO) photocatalyst. The photocatalyst synthesized with different ratio of Sb2O3 and PbO viz. 1:1, 2:1, 3:1, 1:2, and 1:3. Photocatalyst with 3:1 ratio of Sb2O3 and PbO showed the best photocatalytic activity towards CBZ. Transmission electron microscopy (TEM) analysis suggested that the particle size increased by increasing PbO ratio in the catalyst. It was observed that Sb2O3 synthesis with PbO showed less band gap energy in comparison to Sb2O3. The Brunauer-Emmer-Teller (BET) surface area of the Sb2O3/PbO (3:1) was determined to be 4.78 m(2) g(-1). In absence of catalyst, very low degradation of CBZ was achieved, while significant enhancement in CBZ degradation was observed in presence of the synthesized catalyst. CBZ degradation followed the pseudo first-order kinetics with rate constant of 0.016 min(-1). Increased degradation rate was recorded when peroxymonosulfate (PMS) was used with UV/Sb2O3/PbO. Active species trapping experiment revealed that in CBZ degradation, O-center dot(2)- radical produced by synthesized catalysts played a major role. In presence of PMS, generation of SO4-center dot radical enhanced the catalytic activity of synthesized catalyst.