A poly(methyl red) film-modified glassy carbon electrode (PMRE) was fabricated for determination of norfloxacin (NFX). The electrochemical behavior of NFX was investigated and a well-defined oxidation peak with high sensitivity was observed at the film electrode. PMRE greatly enhanced the oxidation peak current of NFX owing to the extraordinary properties of poly(methyl red) film. Based on this, a sensitive and simple voltammetric method was developed for measurement of NFX. A sensitive linear voltammetric response for NFX was obtained in the concentration range of $1;{ imes};10^{-6};-;1;{ imes};10^{-4}$ mol/L and the detection limit was $1;{ imes};10^{-7}$ mol/L using linear sweep voltammetry (LSV). The proposed method possessed advantages such as low detection limit, fast response, low cost and simplicity. The practical application of this new analytical method was demonstrated with NFX pharmaceuticals.