Designing efficient and economical nano-catalysts in the development of electrochemical sensors has been a constant challenge. The design of core–shell nanoarrays using natural asphalt (NA) as the core has not been found in reports. In this report, for the first time, flower-like nanostructures were synthesized by joining nickel–cobalt double hydroxide nanosheets (NiCo-LDH NSs) on NA as a precursor. The synthesis of flower-like nanostructures, abbreviated as NA@NiCo-LDH NSs, was done by an easy and one-step hydrothermal method. NA has characteristics such as availability, cost-effectiveness, high surface area due to its porous structure, and good interaction with the surface of carbon electrodes due to its carbonaceous nature. In addition, the growth of NiCo-LDH NSs on the NA leads to the improvement of electrocatalytic properties, the creation of a larger specific surface area, available active sites, and an increase of contact between analyte and nanostructures. The performance of synthetic nanostructures in the electrochemical determination of deferiprone (DFN) was evaluated satisfactorily. DFN is the first oral iron chelator and the first drug for thalassemia patient treatment. This strategy has some advantages such as cost-effectiveness, portability, good linear range (0.5–2500 µM), and low detection limit (0.19 µM) in the DFN determination. The proposed strategy can be a way to develop new nanomaterials derived from NA with green chemistry in mind. In addition, it can be a way to enter NA-based nanomaterials into other applications.
