The electrocatalytic reduction of thiamphenicol (TAP) and florfenicol (FF) was investigated with multi-walled carbon nanotubes (MWCNTs) modified electrode. MWCNTs was dispersed in pure water with the assistance of dihexadecyl phosphate (DHP), and then modified on glassy carbon electrode (GCE). The electrocatalytic reduction conditions, such as bias voltage, supporting electrolyte and its initial pH, and the initial concentrations of TAP and FF, were also optimized. The experimental results indicated that the removal efficiencies of 2 mgL(-1) TAP and FF in 0.1 M NH3 center dot H2O-NH4Cl solution (pH 7.0) reached 87% and 89% at a bias voltage of -1.2V after 24h electrocatalytic reduction, respectively. The removal process could be described by pseudo first order kinetic model, and the removal rate constants of TAP and FF were obtained as 0.0837 and 0.0915 h(-1\), respectively. The electrocatalytic reduction products of TAP and FF were identified by liquid chromatography-tandem mass spectrometry (LC-MS/MS), and the possible reduction mechanisms were preliminarily analyzed. Electrocatalytic reduction is promising to remove low-concentration TAP and FF in wastewater with the MWCNTs modified electrode, and may cut down their toxicity through dehalogenation and carbonyl reduction. (C) 2017 Elsevier B.V. All rights reserved.