In the present study, we used E. profundum loaded onto Amberlite XAD-4 resin for solid-phase extraction (SPE) of Cu(II), Ni(II), and Pb(II). Some conditions of the SPE procedure, for instance, sample flow rate, pH, eluent type and concentration, the sample volume, amount of E. profundum XAD-4 resin, and the effects of foreign interferences ions are discussed in detail. Surface microstructures of the biosorbent were characterized by FTIR, FE-SEM/EDX before and after loading of metals. The biosorption capacities of E. profundum were determined as 49.83, 57.12, and 64.35 mg g−1 for Pb(II), Cu(II), and Ni(II), respectively. The LOD values were calculated as 0.031 ng mL−1, 0.042 ng mL−1, and 0.043 ng mL−1 for Cu(II), Ni(II), and Pb(II), respectively. The linear range was detected as 0.25–25 ng mL−1. RSD values were lower than 5%. The concentrations of metal ions in water and food samples were measured by ICP-OES.