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A novel Gd2O3 nanosheet was synthesized by the template-free chemical coprecipitation method. Interestingly, upon calcination at 600 °C, nanoparticles were transformed into a nanosheet, as observed from field emission scanning electron microscopy (FESEM) images. An increase in the calcination temperature to 600 °C increases the particle size to 50 nm, which results in aggregation. A sheetlike Gd2O3 exhibits superparamagnetism from 300 K. The highly selective nonenzymatic sensing of riboflavin (RF) was studied using a modified glassy carbon electrode with Gd2O3 nanosheets, and its various applications were made possible by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The redox behavior of the RF was determined. The newly fabricated sensor showed high sensitivity, stability, and reproducibility and was also tested with a commercial vitamin B2 tablet and a milk powder sample.