Magnetic microparticles have many applications in various areas today. The aim of this study was to develop hydrophobic magnetic microparticles as an alternative to traditional methods for high capacity and low cost removal of Victoria Blue R (VBR), which is valuable for industry and commercial, from wastewater and to determine the VBR adsorption ability of this adsorbent. Fe(II)–Co(II) double salt incorporated magnetic poly(2-hydroxyethyl methacrylate-N-methacryloyl-l-tryptophan) [m-poly(HEMA-MATrp)] microparticles were synthesized and used as adsorbent. These microparticles were synthesized in aqueous dispersion medium via microemulsion polymerization using MATrp and HEMA monomers. Magnetic hydrophobic microparticles were characterized via Fourier transform infrared spectroscopy, scanning electron microscopy, and vibrating sample magnetometer. Adsorption experiments were conducted for different conditions (pH, interaction time, amount of microparticles, temperature, and ionic strength) in batch system. VBR adsorption capacity of magnetic hydrophobic microparticles was estimated as 89.46 μmol/g. Adsorption–desorption cycles were repeated 4 times, and there was no significant decrease for the adsorption capacity observed.