A solid-phase extraction method combined with flow injection (FI) on-line flame atomic absorption spectrometry (FAAS) for the determination of cadmium and nickel in tobacco samples is presented. The 2-aminothiophenol functionalized Amberlite XAD-4 (AT XAD) resin was synthesized by covalent coupling of the ligand with the copolymer through a methylene group. A minicolumn packed with AT XAD was connected into the automated on-line preconcentration system. Elution of metal ions from minicolumn can be made with 0.50 mol L-1 hydrochloric acid solution. With a consumption of 21.0 mL of sample solution, detection limits (3 s) of 0.3 (Cd) and 0.8 mu g L-1 (Ni) were achieved at a sample throughput of 18 h(-1). Enrichment factors (EF) of 99 (cadmium) and 43 (nickel) were obtained compared with the slope of the linear portion of the calibration curves before and after preconcentration. The contents of Cd and Ni in a certified reference material (NIST 1570a, spinach leaves) determined by the present method was in good agreement with the certified value. The developed procedure was also successfully applied to the determination of Cd and Ni in local tobacco samples. (c) 2007 Elsevier B.V. All rights reserved.