Fast Fourier transformation with continuous cyclic voltammetry (FFTCV) in a flowing solution was applied as a detection system for the prompt Chloramphenicol (CAP) monitoring. In this method, the potential waveform consisted of two potential sections for cleaning of the electrode surface, accumulating CAP and potential ramp, which was continuously applied on a Pt-Au dual disk microelectrodes. The effects of various parameters on the sensitivity of the method were investigated. When the optimum conditions were imposed, this is a scan rate value of 70 V/s, an accumulation time of 500 ms, an accumulation potential of -300 mV and a pH value of 2. The method proved to be linear over the concentration range of 8.0 ×10 -9 -2.0 ×10 -5 mol/L (r = 0.9981) with a detection limit and a quantitation limit of 2.0 ×10 -9 and 6.6×10 -9 mol/L, respectively. Consequently, the method illustrates the requisite accuracy, sensitivity, precision and selectivity to assay CAP in its biological fluids. The proposed method has some advantages over other reported methods such as, no need for the removal of oxygen from the test solution, a sub-nanomolar detection limit, and finally the method is fast enough for the determination of any such compound, in a wide variety of chromatographic methods. As a result, FFTCV illustrates the benefits of precision, determination speed, cost-effectiveness, accuracy and simplicity, in comparison with formerly reported techniques.