Nickel zinc ferrite (Ni0_5Zn0_5Fe2O4) nanoparticles decorated poly (vinyl alcohol) was constructed by the elec- trospinning 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 NiO_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 Ni 0_5Zn 0_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 na- nofibers are formed through assembling magnetic nanoparticles with poly (vinyl alcohol) as the structure-di- recting template. Under the optimal conditions, the linear dynamic range and RSD were 5.0 >< 10-3- 10.0 mg LT1 and 1.62% (n = 3), respectively. A limit of detection of 1.0 >< 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