Gold nanoparticles were prepared in an aqueous solution with polyacrylamide to reduce HAuCl4. The polyacrylamide played double roles in the preparation of Au nanoparticles. Firstly, it acted as reducing reagent; in addition, it also stabilized the Au nanoparticles to prevent agglomeration and provided environment for forming nanostructure around Au nanoparticles. UV-vis spectra of the Au nanocrystals colloids reveal the plasmon resonance peak position. TEM confirms the presence of gold nanoparticles in the fibers. This is a versatile and applicable approach to prepare many other combinations of functional fibers electrospun