Herein, a self-assembled hierarchical structure of hematite (α-Fe2O3) was synthesized via a one-pot hydrothermal method. Subsequently, the nanomaterial was doped to obtain M x Fe2-x O3 (M = Mn-Co; x = 0.01, 0.05, and 0.1) at precise concentrations. An electrode was fabricated by coating the resulting nanocomposite onto a nickel foam (NF) substrate. Electrochemical characterization demonstrated the excellent performance of cobalt-doped α-Fe2O3, among which Co0.05Fe0.95O3 (CF5) exhibited a superior performance, showing a two-fold increase in sensitivity of 1364.2 μA mM-1 cm-2 (±0.03, n = 3) in 0.5 M KOH, a limit of detection (LOD) of ∼0.17 mM, and a limit of quantification (LOQ) of ∼0.58 mM. The Density Functional Theory (DFT) was performed to understand the doping prompting in the reduced bandgap. The fabricated electrode displayed a rapid response time of 2 s and demonstrated 95% stability, excellent reproducibility, and selectivity, as confirmed by tests with several interfering species. A comprehensive evaluation of the electrode's performance using human blood serum highlighted its robustness and reliability for cholesterol detection in clinical settings, making it a promising tool for clinical and pharmaceutical applications.

Department of Chemistry Catalysis and Materials Chemistry Laboratory National Institute of Technology Karnataka Surathkal D K Karnataka 575 025 India

Department of Condensed Matter Physics Faculty of Mathematics and Physics Charles University Ke Karlovu 3 Prague 12116 Czech Republic

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