Magnetic core-shell silica nanoparticles modified by 3-[2-(2-aminoethylamino)ethylaminolpropyl-trime thoxysilane (AAAPTS) were prepared and used as new adsorbent for simultaneous extraction and preconcentration of bismuth and lead ions through magnetic solid-phase extraction (MSPE) method. After adsorption, these ions were desorbed with nitric acid followed by determination with electrothermal atomic absorption spectrometry. Fourier transform infrared (FT-IR) spectroscopy, field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) spectrometry and vibrating sample magnetometer (VSM) were used to characterize the adsorbent. The MSPE conditions were optimized. The detection limits of 1.4 and 3.7 ng L-1 were obtained for bismuth and lead, respectively. The linear range was 0.003-0.200 ng mL(-1) for bismuth and 0.02-0.700 ng mL(-1) for lead. The relative standard deviations of the method for eight replicate determination of 0.07 and 0.35 ng mL(-1) of Bi(III) and Pb(II) were +/- 3.6% and +/- 3.1%, respectively. The method was applied for the determination of target ions in different samples with high recoveries. (C) 2015 Elsevier B.V. All rights reserved.