We describe a facile method for the preparation of magnetic microparticles consisting of a metal-organic framew o r k ( M O F ) o f C u ( I I ) -B T C ( B T C = 1 , 3 , 5 -benzenetricarboxylate) for rapid magnetic solid-phase extraction (MSPE) of the dye Congo Red (CR) from aqueous solution. Magnetization of the MOF and solid-phase extraction of CR was simultaneously accomplished by mixing, under ultrasonication, the MOF and silica-coated magnetite microparticles in the solution to be extracted. Under optimized conditions, the magnetic MOF hybrid exhibits a fast adsorption rate and a high removal efficiency (>97 %) toward CR even over 15-fold reuse, which also features high adsorption capacity of 97.7 and 92.5 % for cationinc Methylene Blue (MB) and Crystal Violet (CV), respectively. The desorption of CR from the magnetic MOF was realized by washing it with ethanol and water. The material is considered to be a promising new adsorbent for use in wastewater treatment and in analytical preconcentration.