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An excellent magnetic multi-walled carbon nanotubes (MMWCNT) containing carboxyl material modified with ferroferric oxide (Fe3O4) nanoparticles was synthesized as the adsorbent for magnetic solid-phase extraction (MSPE) of five heavy metal ions (Pb2+, Cu2+, Co2+, Cd2+, Cr4+) in water samples followed by on-line inductively coupled plasma mass spectrometry (ICP-MS) detection. The characteristics of the adsorbent were analyzed using Fourier transform infrared spectroscopy (FT-IR), Scanning electron microscope (SEM), and Vibrating sample magnetometer (VSM). Some factors affecting extraction efficiency including pH of sample solution, the amount of adsorbent, extraction method and time, concentration and volume of desorption solvent, desorption time and evaluation of coexisting ions were optimized. Under the optimum conditions, good linearity (r ≥ 0.9951) was obtained within the range of0.1–50.0 ng·mL−1. The limits of detection (LODs) and limits of quantification (LOQs) were 4.0–25.0 ng·L−1 and 15.0–80.0 ng·L−1, respectively. And satisfactory recoveries of five heavy metal ions ranged from 81.11% to 105.53% were acquired, and the relative standard deviations (RSDs) were no more than 6.05%. The MMWCNT synthesized had strong adsorption force for the five investigated heavy metal ions, respectively. Hence, the proposed method was so suitable and sensitive that it can be applied to the determination of trace analysis of heavy metals in water samples.