Nickel zinc ferrite (Ni0.5Zn0.5Fe2O4) nanoparticles decorated poly (vinyl alcohol) was constructed by the electrospinning method and used for determining the sunitinib amount in real sample. In this study, resonance light scattering (RLS) technique was used for studying the interaction of nanofibers with sunitinib. Similar Ni0.5Zn0.5Fe2O4 nanoparticles-decorated nanofibers with average diameter of 200 nm and length up to several millimeters were prepared. The morphology and microstructure of the as prepared Ni0.5Zn0.5Fe2O4 nano particles-decorated nanofibers were studied in details. The nanofibers were characterized by energy dispersive X-ray spectroscopy, scanning electron microscopy, and transmission electron microscopy techniques. The nanofibers are formed through assembling magnetic nanoparticles with poly (vinyl alcohol) as the structure -directing template. Under the optimal conditions, the linear dynamic range and RSD were 5.0 x 10(-3)-10.0 mg L-1 and 1.62% (n = 3), respectively. A limit of detection of 1.0 x 10(-3) mg L-1 sunitinib was obtained from this method. The obtained results showed successful application of the method for the analysis of sunitinib in real samples.