<p>Accurate non-invasive glucose monitoring is crucial for health diagnostics. However, the development of high-performance non-enzymatic electrochemical sensors for this application remains a significant challenge. To address this issue, a novel material, FeOOH encapsulated within zeolitic imidazolate framework-67 (ZIF-67)-derived copper-cobalt-layered double hydroxide (FeOOH@CuCo-LDH), was developed through a vapor-assisted deprotonation process for FeOOH encapsulation, followed by a hydrothermal reaction to synthesize the hollow composite. The synergistic interactions between the multi-metallic composition and the hollow structure significantly enhance glucose oxidation-reduction reactions. This enables the sensor to achieve a wide linear detection range (0.5–722&#xa0;μmol·L⁻¹ and 722–4222&#xa0;μmol·L⁻¹), high sensitivity (4.05 and 1.43&#xa0;μA·L·μmol⁻¹·cm⁻²), and a low limit of detection (0.83&#xa0;μmol·L⁻¹). The sensor demonstrated excellent performance in practical applications, accurately detecting glucose in saliva under physiological conditions. This study highlights the potential of FeOOH@CuCo-LDH as an excellent electrode material for non-enzymatic electrochemical glucose sensing, offering promising applications in diabetes prevention and diagnosis.</p> Graphical abstract <p></p>