The excessive accumulation of heavy metals has adverse effects on the human body. Here, magnetic iron oxide‐impregnated carboxymethyl‐β‐cyclodextrin was synthesized. The synthesized material was employed as a magnetic solid‐phase extracting adsorbent for specific heavy metals like lead (Pb), nickel (Ni), copper (Cu), and cobalt (Co). Characterization was performed by X‐ray diffraction, energy dispersive X‐ray spectroscopy, scanning electron microscopy, Brunauer–Emmett–Teller, and Fourier‐transform infrared spectroscopy. The analytical merits, like detection limits (Pb: 1.38 ng/mL, Ni: 0.5 ng/mL, Co: 0.14 ng/mL, and Cu: 0.55 ng/mL) and quantification limits (Pb: 4.14 ng/mL, Ni: 1.62 ng/mL, Co: 1.85 ng/mL, and Cu: 1.82 ng/mL) were calculated. Similarly, the preconcentration and enhancement factors (15) and relative standard deviation (Pb: 3.5, Ni: 0.92, Co: 2.7, and Cu: 1.5) were also calculated. The interfering study shows that the method is highly selective. For validation, it was applied to certified reference materials such as the Institute of Nuclear Chemistry and Technology ornamental Basma tobacco leaves and trace metal double addition 63.4 environmental water with good percent recovery values (92%–99%). Real water and food samples were also used with satisfactory (90%–99%) recovery results.