NiFe₂O₄/(S,N)-doped graphene oxide composite as efficient electrochemical sensor for determination of sibutramine in dietary supplements
Abstract
A novel electrochemical sensor based on a NiFe₂O₄/(S,N)-doped graphene oxide composite (NiF/GrO(S,N)) was developed to detect sibutramine (SBT). The composite material was successfully synthesized and characterized using X-ray diffraction, Raman spectroscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy, nitrogen adsorption/ /desorption isotherms, and vibrating sample magnetometry. Results confirmed the formation of a nanocrystalline NiFe₂O₄ structure uniformly dispersed on S,N-doped graphene sheets, providing a high surface area and numerous active sites. The NiF/GrO(S,N)-modified glassy carbon electrode (GCE) showed improved electrocatalytic activity toward SBT oxidation. Under optimized conditions, differential pulse voltammetry revealed two linear ranges from 0.5 to 8.9 µM and 8.9 to 19.6 µM, with a detection limit of 0.37 µM. The sensor also demonstrated good repeatability, reproducibility, and stability, along with effective anti-interference capabilities against common inorganic and organic substances. The practical applicability of the proposed sensor was successfully demonstrated by determining SBT in seven commercial dietary supplement samples. The obtained recoveries ranged from 96.38 to 104.83 %, and the results showed no statistically significant difference compared with those obtained using the standard HPLC method. These results suggest that the NiF/GrO(S,N)/GCE sensor is a promising platform for the rapid and reliable detection of SBT…
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