Soil and water contamination by numerous pollutants has been increasingly posing threats to food, water, agriculture, and human health. Using novel nanoscale materials to develop rapid electrochemical sensors is very promising due to the discovery of a number of new two-dimensional (2D) electronic materials. Of particular importance is 2D transition-metal carbide MXene that has been shown to possess transformative properties pertaining to its physical, chemical, and environmental characteristics, leading to their potential sensor applications. Designing electrochemical sensors using MXene has the potential to pave the way for monitoring environmental pollutants. Here, a stacked layer of chemically exfoliated MXene (Ti 3 C 2 T x ) was demonstrated as an electrochemical sensor for detection of 4-nitrophenol (4-NP) with high sensitivity and a low limit of detection. Successful selective exfoliation of the MAX (Ti 3 AlC 2 ) phase of the material by chemical etching without oxidation is shown to be the key to achieving higher sensitivity and a lower detection limit. In the optimal conditions, the proposed MXene sensor electrodes were capable of detecting 4-NP in a broad concentration range from 500 nM to 100 μM with a good linear sensing range (regression fit, R = 0.995). The higher sensitivity and notable limit of detection reached about 16.35 μA μM −1 cm −2 and 42 nM/L, respectively, with good reproducibility and repeatability. The real-time application of the proposed MXene sensor electrodes was confirmed by testing in tap water samples with excellent recoveries of 95−99%.