In this work, toner powder as a magnetic adsorbent coupled with a dispersive solid phase extraction (DSPE) method was proposed for the pre‐concentration and separation of Pb2+, Cd2+, and Zn2+ in vegetable samples and aqueous environments. Flame atomic absorption spectrometry (FAAS) was used for the final analysis of the ions. Adsorbent characterization was studied by scanning electron microscope (SEM), transmission electron microscopy (TEM), Fourier‐transform infrared spectroscopy (FTIR), X‐ray diffraction analysis (XRD), and vibrating‐sample magnetometer (VSM). The effect of experimental factors on the extraction efficiency was investigated by Box‐Behnken design (BBD). The maximum recovery percentage was found to be 95.40%, 95.40%, and 97.40% for Pb2+, Cd2+, and Zn2+, respectively. In the optimum conditions, the linearity ranges were obtained 12–200, 1–150, 0.4–100 μg L−1 for the Pb, Cd, and Zn ions, respectively. The limit of detection (LOD) of the method was found 3.60, 0.30, and 0.11 μg L−1 for the Pb2+, Cd2+, and Zn2+, respectively. The suggested procedure indicated to be appropriate, cost‐effective, and eco‐friendly for extraction of mentioned metal ions in different vegetables and water samples with high precision and accuracy.