The efficiencies and performances of silver nanoparticle loaded activated carbon modified with 2-(4-isopropylbenzylideneamino)thiophenol (IPBATP-Ag-NP-AC) and activated carbon modified with IPBATP (IPBATP-AC), as new sorbents, were evaluated for separation and preconcentration of Cu2+, Zn2+, Co2+, Cd2+ and Pb2+ ions from real environmental samples. The retained metals content was reversibly eluted using 5mL of CH3COOH (6.0molL1) and/or 10mL of 4.0molL1 HNO3 for IPBATP-Ag-NP-AC and IPBATP-AC, respectively. The experimental parameters influence the recoveries of metal ions including pH, amounts of ligand and supports, condition of eluents, sample and eluent flow rates of has been investigated. The preconcentration factors were found to be 100 for Zn2+, Cd2+, Co2+, Cu2+ and 50 for Pb2+ ions using IPBATP-Ag-NP-AC, and 50 for Zn2+, Cd2+, Co2+, Cu2+ and 25 for Pb2+ ions using IPBATP-AC. The detection limit of both SPE-based sorbents was between 1.62.5ngmL1 for IPBATP-AC and 1.32.5ngmL1 for IPBATP-Ag-NP-AC. The proposed methods have been successfully applied for the extraction and determination of the understudy metal ions content in some real samples with extraction efficiencies higher than 90% and relative standard deviations (RSD) lower than 2.4%.