In the present study, the PCL-Diol-b-PU/Au nanocompsite nanofibers were fabricated via electrospinning process during two different stages to load an anticancer temozolomide (TMZ) drug into the nanofibers. The first stage was the incorporation of Au nanoparticles into the nanofibers and the second stage was coating the gold nano particles on the surface of PCL-Diol-b-PU/Au composite nanofibers. The prepared nanofibrous formulations were characterized using FUR, SEM and TEM analysis. Box-Behnken-design was used to investigate the influence of electrospinning parameters including solution concentration, applied voltage to tip-collector distance ratio and collector speed on the morphology and fiber diameter of PCL-Diol-b-PU/Au nanofibers. Drug loading efficiency, in vitro release profiles of TMZ from PCL-Diol-b-PU/Au and gold-coated PCL-Diol-b-PU/Au composite nanofibers as well as in vitro antitumor efficacy against U-87 MG human glioblastoma cells were carried out. The TMZ release data were well described using Korsmayer-Peppas kinetic model in which results indicated Fickian diffusion of TMZ from nanofibers. The obtained results revealed the higher efficiency of PCL-Diol-b-PU/Au@TMZ nanofibrous implants for treatment of glioblastoma tumors. (C) 2017 Elsevier B.V. All rights reserved.