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Bismuth vanadate (BiVO₄) has been investigated as a photocatalyst of great interest due to its ability to harvest photons efficiently in the visible spectral region. In addition, powdered BiVO₄ shows high photochemical stability, good dispersibility, and resistance to corrosion in oxidative conditions. Herein, we report the synthesis of monoclinic or tetragonal BiVO₄ particles using different methods, as well as the synthesis of hybrids materials through the combination of cobalt ferrite (CoFe₂O₄) and BiVO₄, and their application in the photodegradation of aqueous solutions of sulfamethoxazole (SMX) under simulated solar radiation. We demonstrate that high-crystallinity single-phase monoclinic BiVO₄ was synthesized fast and efficiently using a solid-state method and, in combination with magnetic CoFe₂O₄ particles, gives rise to a hybrid material that can be easily separated from the reaction medium, by applying an external magnetic field, without the need for further downstream treatments.