A biomass-derived adsorbent was simply prepared and applied as efficient and low-cost solid-phase supports. The adsorbent material was characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), surface area analysis and Fourier transform infrared (FTIR) spectroscopy. The amorphous structure of the prepared adsorbent was indicated from the XRD. The prepared adsorbent exhibited surface functional groups such as carbonyl and hydroxyl groups, which enhance the application of DSPE. An accurate separation and preconcentration of Cr(III), Fe(III), Co(II) and Ni(II) prior to ICP-MS detection was achieved using the biomass-derived adsorbent. The extraction process was performed at pH 4 using 1 mL of 0.5 N nitric acid for elution and recovery of ions. The prepared biomass-derived adsorbent showed efficient performance for extraction application, exhibiting a preconcentration factor of 50 and LODs of 1.4, 2.4, 1.9 and 3.0 µg.L−1 for Cr(III), Fe(III), Co(II) and Ni(II), respectively, while the LOQs were reported as 4.1, 7.3, 5.7 and 8.9 µg.L−1 for Cr(III), Fe(III), Co(II) and Ni(II), respectively. The DSPE procedure presented was successfully applied to the determination of the Cr(III), Fe(III), Co(II) and Ni(II) contamination in some food samples.