A catalyst preparation method using dielectric barrier discharge (DBD) plasma was investigated in this paper. The results indicated that DBD plasma is good method to prepare Mo/Co/K/ZSM-5 catalysts in a rapid and efficient way. The DBD plasma method has similar performance with the traditional roasting method using X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscope (SEM), however, the former could obtained smaller size of particles and low agglomeration degrees. The activity tests also showed that the catalysts prepared by DBD plasma have higher activities towards synthesis of hydrocarbon (C5+) directly from synthesis gas than those obtained by the traditional roasting method.