An efficient adsorbent, N-[(3trimethoxysilyl)propyl]ethylenediamine triacetic acid functionalized magnetic core-shell silica nanoparticles (Fe 3 O 4 /SiO 2 /TMS-EDTA), was synthesized and used as an adsorbent for the simultaneous extraction and pre-concentration of Pb and Cd from water samples through magnetic solidphase extraction (MSPE). After adsorption, these ions were desorbed with hydrochloric acid, followed by the determination with hydride generation atomic fluorescence spectrometry (HG-AFS). The sorbent was characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR). Several important parameters influencing the extraction efficiency, such as pH, amount of adsorbent, adsorption and elution time, elution concentration and volume, sample volume, interfering ions and adsorption capacity, were studied and optimized. The detection limits for Pb and Cd of 0.03 and 0.028 ng mL −1 , respectively, were obtained. The linear range was 0.12-15.0 ng mL −1 for Pb and 0.10-4.0 ng mL −1 for Cd and the relative standard deviations were 3.72% and 2.41% (n=7), respectively. The pre-concentration factor was 83.3 for Pb and 66.7 and Cd, respectively. The method was applied for the determination of target ions in different samples with high recoveries.