This work aimed to combine solid phase extraction (SPE) with inductively coupled plasma mass spectrometry for the determination of multi-elements (Pb, Cd, and Zn) simultaneously. This combination allows the purification of the solution by minimizing matrix effects, the separation of the analytes and a fast determination of multiple elements (Pb, Cd, and Zn) in seconds. A syringe-solid phase extraction (SYRINGE-SPE) method was developed based on adsorption/desorption of metals onto amino-functionalized hollow core mesoporous shell silica spheres (NH 2 -HCMSSs). The separation of NH 2 -HCMSSs from aqueous phase was assessed by capping the syringe with 0.2-mm filter. The results showed that the quantitative recovery of analytes was obtained at pH 6 by elution with 3 M HNO 3 . The developed method is applicable in the presence of different coexisting ions. The limit of detection was 0.021, 0.004, and 0.007 mg L À1 for Pb(II), Cd(II), and Zn(II) ions, respectively, whereas the limit of detection of the instrument without combination with the SYRINGE-SPE was 0.699, 0.123, and 0.24 mg L À1 for Pb(II), Cd(II), and Zn(II) ions, respectively. The relative standard deviations were 7.4, 6.2, and 5.4% for Pb(II), Cd(II), and Zn(II), respectively. The method was validated using corn bran (8433) certified reference material. The method was successfully applied for the determination of Pb(II), Cd(II), and Zn(II) in bottled water, tap water, beet, radish, carrot, potato, sweet potato, and turnip samples.Abbreviations: AAS, atomic absorption spectrometry; EDS, energydispersive X-ray spectroscopy; FTIR, Fourier transform infrared; ICP-MS, inductively coupled plasma mass spectrometry; LOD, limit of detection; LOQ, limit of quantification; NH 2 -HCMSS, amino-functionalized hollow core mesoporous shell silica sphere; SEM, scanning electron microscopy; SPE, solid-phase extraction; SYRINGE-SPE, syringe-solid phase extraction; TGA, thermal gravimetric analysis 720