A new magnetic dispersive solid-phase microextraction technique was established using a Fe3O4@MIL-53-(Fe)@Ti3AlC2 nanocomposite to separation-preconcentration of cadmium. The novel nanocomposite was characterized using X-ray diffraction, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, and field emission scanning electron microscopy- energy dispersive X-ray analysis. The analytical parameters were optimized, including pH (5.0), adsorbent amount (15 mg), eluent concentration and volume (0.5 mL of 3 mol L−1 HNO3), sample volume (20 mL), etc. Also, matrix effects were investigated. The limit of detection and quantification were calculated as 3.6 ng mL−1 and 12.2 ng mL−1, respectively. The analysis of certified reference materials checked the validation of the procedure. The preconcentration factor was calculated as 40 times. The method was successfully applied to determine cadmium in water and edible offal samples.