A facile one-pot synthesis of magnetic iron oxide nanoparticles embed N-doped graphene modified magnetic screen printed electrode for electrochemical sensing of chloramphenicol and diethylstilbestrol

Trace determination of antibacterial agents is crucial to minimize risks of human intoxication and in the prevention of serious environmental impacts. Herein, a simple one-pot solvothermal synthesis approach for a magnetic iron oxide embed nitrogen-doped graphene (MIO@NG) nanohybrid was fabricated without the addition of any extra reductant and its application towards ultrasensitive chloramphenicol (CAP) and diethylstilbestrol (DES) electrochemical sensor is demonstrated to screen for antibiotic residue contamination in milk samples. The prepared nanohybrid was modified on a magnetic screen-printed electrode (MSPE) to make it portable for on-site detection. The determination of two additive drugs, CAP and DES, was achieved based on the reduction current response at MIO@NG modified MSPE (MIO@NG/MSPE) to eliminate interference as far as possible. Uniform dispersed MIO nanoparticles are grown in situ on the surface of nitrogen-doped graphene sheets. The morphology of MIO@NG was confirmed by transmission electron microscopy (TEM) analysis. The chemical structure of the prepared MIO@NG was characterized by x-ray diffraction (XRD), x-ray photoemission spectroscopy (XPS), Raman spectroscopy, and extended x-ray absorption fine structure (EXAFS). Moreover, the superparamagnism property was investigated by vibrating sample magnetometry (VSM). The electrochemical properties of MIO@NG were evaluated with cyclic voltammetry (CV) and square wave voltammetry (SWV). Sensor performance was evaluated by testing the electrochemical activity of CAP and DES in the presence of interferences. The MIO@NG modified electrode presented superior electrochemical performance, including high sensitivity, high catalytic activity, ultimate sensitivity, very fast detection, selectivity, and excellent performance. The MIO@NG modified electrode demonstrated a detection limit of 10 nM for the detection of CAP and 6.5 nM for DES with satisfactory recovery in real samples.