Monodisperse magnetic C(18) microspheres were prepared based on the three-step reactions of solvothermal reduction, silanization and alkylation. The microspheres are of uniform sizes in the range of 200-260 nm. The structure of synthesized magnetic C(18) microspheres was studied by transmission electron microscopy, scanning electron microscopy, X-ray diffraction patterns, element analysis and vibrating sample magnetometry. This material has a high magnetic saturation value of 59 emicrog(-1) and is easy to manipulate under a magnet. The prepared material was used for the preconcentration of the polycyclic aromatic hydrocarbon in water. The effects of desorption solvent and the amount of adsorbent on the preconcentration were also investigated. The results showed that the developed method was beneficial for the preconcentration of PAHs of middle molecular weight.