Abstract: | Synthesis of nanomaterials using cheap and highly efficient material is an important aspect of nanotechnology. In this present work, we have used the carbon black (CB) as a highly conductive and inexpensive carbonaceous material for the fabrication of the electrochemical sensor. However, the poor dispersion in water obstructs the usage of CB in electrochemical sensor and biosensor applications. Hence, the CB was functionalized by simple reflux method and the functionalized CB (f‐CB) nanospheres hybrids with hydrothermally synthesized MoS2 nanoclusters by simple ultrasonication process. In addition, the various suitable spectrometric techniques used to probe the surface morphology and chemical modification of the prepared materials. The prepared MoS2 and f‐CB nanohybrids (f‐CB/MoS2) applied for the electrocatalytic reduction of toxic chloramphenicol (CAP). Fascinatingly, the f‐CB/MoS2 modified electrode showed a competitive electrocatalytic performance comparing with other modified electrodes. At the optimized condition, the sensor exhibited the LOD about 0.002 μM, wider linear range 0.015 to 1370 μM with the sensitivity of 3400 μA μM−1 cm−2 for the determination of CAP. Moreover, the practical viability of the sensor was exploited in milk powder and honey samples. |