Novel photocatalysts Gd2FeSbO7, Gd2InSbO7 and Gd2YSbO7 were synthesized by the solid state reaction method for the first time. A comparative study about the structural and photocatalytic properties of Gd2MSbO7 (M = Fe, In, Y) was reported. The results showed that Gd2FeSbO7, Gd2InSbO7 and Gd2YSbO7 crystallized with the pyrochlore-type structure, cubic crystal system and space group Fd3m. The lattice parameter a for Gd2FeSbO7, Gd2InSbO7 or Gd2YSbO7 was 10.276026 Å, 10.449546 Å or 10.653651 Å. The band gap of Gd2FeSbO7, Gd2InSbO7 or Gd2YSbO7 was estimated to be 2.151 eV, 2.897 eV or 2.396 eV. For the photocatalytic water-splitting reaction, H2 or O2 evolution was observed from pure water with Gd2FeSbO7, Gd2InSbO7 or Gd2YSbO7 as catalyst under visible light irradiation (wavelength > 420 nm). Moreover, H2 or O2 also spilt by using Gd2FeSbO7, Gd2InSbO7 or Gd2YSbO7 as catalyst from CH3OH/H2O or AgNO3/H2O solutions under visible light irradiation (λ > 420 nm). Gd2FeSbO7 showed the highest activity compared with Gd2InSbO7 or Gd2YSbO7. At the same time, Gd2InSbO7 showed higher activity compared with Gd2YSbO7. The photocatalytic activities were further improved under visible light irradiation with Gd2FeSbO7, Gd2InSbO7 or Gd2YSbO7 being loaded by Pt, NiO or RuO2. The effect of Pt was better than that of NiO or RuO2 for improving the photocatalytic activity of Gd2FeSbO7, Gd2InSbO7 or Gd2YSbO7.