Here, the development of a highly sensitive and selective surface plasmon-enhanced light scattering technique for ultra-trace cyanide sensing using silver magnetic nanoparticles is reported. The assay relies upon the nanoparticles plasmonic enhanced effects and rapid interaction of cyanide with Ag nanoparticles in the Ag/Fe3O4 nanostructures. A decrease in Rayleigh intensity in the presence of cyanide was observed and the decrease in Rayleigh scattering intensity (ΔIR) is directly proportional to the concentration of CN− in a certain range.