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Herein, we report the electrochemical detection of roxarsone (ROX) on a two-dimensional (2D) activated carbon (AC)-modified glassy carbon electrode (GCE). Meso/microporous 2D-AC is synthesized from a natural biomass Desmostachya bipinnata, commonly known as Kusha in India. This environment-friendly material is synthesized by chemical activation using potassium hydroxide (KOH) and used as a sensitive electrochemical platform for the determination of ROX. It is an arsenic-based medicine, also used as a coccidiostat drug. It is widely used in poultry production as a feed additive to increase weight gain and improve feed efficiency. Long-term exposure to arsenic leads to serious health problems in humans and demands an urgent call for sensitive detection of ROX. Therefore, the green synthesis of 2D-AC is introduced as new carbon support for the electrochemical sensing of ROX. It provides a large surface area and efficiently supports enhanced electron transfer. Its electrocatalytic activity is seen in potassium ferri/ferrocyanide by cyclic voltammetry, where the 2D-AC-modified GCE delivered five to six times higher electrochemical performance as compared to the unmodified GCE. Electrochemical impedance spectroscopy is also performed to show that the prepared material has faster electron transfer and permits a diffusion-controlled process. It works well in real samples and also on disposable screen-printed carbon electrodes, thereby showing great potential for its application in clinical diagnosis. Our results exemplify a modest and innovative style for the synthesis of excellent electrode material in the electrochemical sensing platform and thus offer an inexpensive and highly sensitive novel approach for the electrochemical sensing of ROX and other similar drugs.