The synthesis of uniform and monodispersed magnetic and optical nanocrystals has received much attention in recent years due to the size-dependent physicochemical properties. In this study, we have demonstrated a general approach for the synthesis of size-tunable ferrite and gold nanocrystals and their nanocomposite. The monodispersed magnetite nanocrystals were obtained by thermal decomposition of iron-oleate complex in a high boiling point solvent in presence of oleylamine and oleic acid. The size of magnetite nanocrystal can be tuned from 7 – 11nm by changing the amount of iron-oleate complex. The other key parameters such as temperature, amount of capping agents, types of solvent were also discussed. This synthetic procedure could also apply to synthesis other type of ferrite nanocrystals. When Mn-acetate was partially substituted for iron-oleate in a 1:2 ratio in the same reaction conditions as in the synthesis of Fe3O4, monodispersed MnFe2O4 nanocrytals with 14nm could be obtained. Except those magnetic nanocrystals, we also synthesized various sizes of monodispersed gold nanocrystals by reducing HAuCl4 in presence of t-butylamine-borane and oleylamine. By varying the reaction temperature, the particle size could be well-tuned from 2nm to 8nm with the characteristic surface plasmon absorption between 510 and 520 nm. For Fe3O4/Au composite, it was prepared via the decomposition of iron-oleate over the surface of the Au nanoparticles. The mean size of the Fe3O4/Au nanocomposite was ∼17 nm which shows a saturation magnetization of 46.92 emu/g and absorption peak at 512nm. These composites with both magnetic and optical properties would make them very promising in the fields of biomedine and environment.