The preparation and electrochemical performance of the carbon nanotube paste electrode modified with ferrocene (FCMCNPE) was investigated for electrocatalytic behaviour toward oxidation ofN-acetylL-cysteine (NAC) in the presence of tryptophan (Trp) using cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The results showed an efficient electrocatalytic activity of FCMCNPE toward oxidation of NAC and Trp, as the electrooxidation of NAC and Trp together gave two well-defined anodic peaks, revealing the applicability of this modified electrode for simultaneous voltammetric detection of mentioned compounds in the same solution. The values of catalytic rate constant (k) and the apparent diffusion coefficient (Dapp) were also calculated using chronoamperometry. The DPV method was applied as a sensitive method for the quantitative detection of trace amounts of NAC and Trp. A linear dynamic range from 1.0 to 18.0μMforNAC and 2.0 to 150.0μM for Trp was obtained using DPV method in pH 7.00 buffered solution and the detection limit (3σ)was determined as 0.49μM and 0.54μM for NAC and Trp, respectively. The proposed method was also applied for analysis of NAC tablet, investigating the applicability of the proposed voltammetric method for determination of NAC in real sample.