Abstract3-methyl-4-nitrophenol (MNP) is the main by-product of the organophosphate insecticide fenitrothion (FT), used in locust control. MNP is highly toxic because it is an endocrine disruptor and then may cause adverse in the biological systems. Then, it is necessary to develop analytical methods for determination of this pollutant in the environment. In this sense, we reported herein the development of an electrochemical sensor for the detection of 3-methyl-4-nitrophenol (MNP), one of the metabolites of fenitrothion (FT), by using naked and modified carbon fiber microelectrode (CFME) by nickel tetrasulfonated phthalocyanine polymer (CFME/p-NiTSPc). The voltammogram showed that MNP presents one irreversible anodic peak corresponding to the oxidation of the phenol group at 0.9 V vs Ag/AgCl. The effect of pH of the buffer on the peak current and SWV parameters such as frequency, scan increment and pulse amplitude were investigated in order to optimize the electrochemical response of the sensor. The obtained results lead to the following optimum value: pH = 6; frequency = 25 Hz, pulse amplitude = 50 mV, scan increment = 10 mV. With these optimum values, the calibration curves show that the peak current varied linearly upon MNP concentration leading to a limit of detection (LoD) for naked CFME close to 3 µg/L whereas for CFME modified by p-NiTSPc, it reaches 0.75 µg/L. This results prove that the presence of p-NiTSPc increasing the sensitivity of the sensor could be used to monitor 3-methyl-4-nitro-phenol residue in real matrix.