A novel bifunctional electrochemical nanosensor for simultaneous detection of glucose and insulin based on NiO/Co₃O₄@CuAl LDH-MWCNT nanocomposite-modified carbon paste electrode

The appropriate development of electrocatalytic nanomaterials is a significant step for constructing high-quality non-enzymatic electrochemical sensors. In this work, we presented effective copper aluminum layered double hydroxide (CuAl LDH)-based nanoparticles with two consecutive optimization steps through nickel oxide/cobalt oxide (NiO/Co₃O₄) merging and subsequent assembly with multi-walled carbon nanotubes (MWCNT). The obtained nanostructures were characterized by using Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction pattern (XRD), and field emission scanning electron microscope images (FE-SEM). The synthesized nanomaterials were used as a carbon paste electrode (CPE) material for simultaneous dual-signal evaluation of glucose and insulin. The response of the modified electrode was investigated by some electrochemical approaches, including cyclic voltammetry (CV), electrical impedance (EI), differential pulse voltammetry (DPV), and amperometric titration. The NiO/Co₃O₄ CuAl LDH@MWCNT electrode displayed multi-functional properties through two well-defined separated peaks toward glucose and insulin detection with a linear range of 0.01–26.5 mM and 0.02–70.0 nM, respectively. The detection limit values were obtained as 2.8 µM for glucose and 17.3 pM for insulin. The sensor showed good tolerance to common interfering agents, excellent sensitivity, and appropriate stability during 30 days of dry storage at room temperature. This sensor was also used for the quantification of glucose and insulin in human serum samples, obtaining the recovery rate of 101.0 %-103.7 % and 98.0 %-106.0 %, respectively, with all the RSD values below 3.0 %. This study represented an efficient simultaneous sensing platform for glucose and insulin detection, which warrants its operational application in clinical samples.