Superparamagnetic starch functionalized maghemite nanoparticles (SMhNPs) were synthesised by a co-precipitation method via in situ functionalization and used as nano-adsorbents for the removal of Cr(VI) from aqueous waste. The characterization of the prepared nanoparticles was done by XRD, FTIR, TEM and VSM techniques. Adsorption of Cr(VI) on the surface of superparamagnetic starch functionalized maghemite nano-adsorbents was investigated and the removal was higher in acidic pH as compared to that exhibited in basic medium. The adsorption of Cr(VI) by the SMhNPs followed pseudo-second order kinetics and the adsorption isotherm data fits well the Freundlich adsorption isotherm. The 𝐾F value for Cr(VI) removal by SMhNPs is found to be 24.76 mg.g−1, which is significantly better than the adsorption capacities reported in literature for maghemite nanoparticles. Thermodynamic studies revealed that the adsorption of Cr(VI) onto the superparamagnetic starch functionalized maghemite nano-adsorbents is spontaneous and endothermic in nature.