Graphene oxide (GO) modified expanded perlite (EP) was prepared as a new sorbent for solid phase extraction of Cu(II) and Pb(II) prior to determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS-FAAS). Characterization of the synthesized sorbent was proved by Fourier transform infrared spectroscopy (FT-IR); X-ray diffraction (XRD); Brunaer, Emmet, and Teller (BET); specific surface area; and scanning electron microscopy (SEM) techniques. Several parameters such as pH, eluent type and concentration, flow rate, sample volume, interfering ions, adsorption capacity of sorbent were investigated and optimized. The proposed method was successfully applied for spiked analysis of Cu(II) and Pb(II) ions in tap water and fruity sodas sample, and fine recoveries (relative error <10%) were obtained.