Accurate monitoring of vitamins is an indispensable tool in predicting the health condition of humans rapidly. In this work, electrochemical determination of vitamin C was investigated using a glassy carbon electrode modified with molybdenum disulfide (MoS2) transition metal dichalcogenides. To study the electrochemical sensing of MoS2 toward vitamin C, three different synthesis temperatures, 400°, 450°, and 500 °C were adopted. MoS2 prepared at 450 °C (MS450) exhibited low oxidation potential (0.25 V vs Ag/AgCl) toward electrochemical sensing of vitamin C. The electrochemical sensing behavior was linear in the range of 90 to 590 nM with a sensitivity of 5.83 × 10−2
μA μM−1 and a detection limit of 0.041 μM. The electrode exhibited anti-interference properties even in artificial urine samples. The results show that MoS2 can be a promising candidate for developing vitamin C electrochemical sensors.