antispasmodic and anticholinergic drug, a medication that reduces the effect of acetylcholine on smooth muscles. DcCl is used to treat or prevent spasms in the muscles of the gastrointestinal tract in the irritable bowel syndrome [1,2]. DcCl has been determined by several techniques including spectrophotometry, gas chromatography and NMR spectroscopy [3][4][5][6][7]. However, most of these methods have some disadvantages such as expensive equipment, involve the use of complex procedures and long analysis times. These disadvantages make them unsuitable for routine analysis. Electrochemical techniques with excellent merits of rapid response and simple operation have attracted a lot of interest in the detection of biomolecules [8][9][10][11].Modified electrodes are being used frequently in the voltammetric determination of organic and inorganic compounds because of their efficiency and the selectivity that can be obtained by varying the modifier [12][13][14][15]. The application of nanoparticles in various fields of science and technology has been extensively developed due to the unique properties of these materials. These materials are being employed in electrochemistry to improve the performance of electrochemical techniques due to excellent electrocatalytic properties. There is currently an intense interest in the use of nanoparticles for the fabrication of modified electrodes and a wide range of bioscience applications. The fabrication of electrodes modified with nanoparticles has been the focus of recent attention owing to enhancement of the response signal, increased sensitivity and better reproducibility [12,16].Carbon-based nanostructures such as carbon nanofibers, carbon nanotubes (CNTs), and mesoporous carbons have been extensively used in fabrication of modified electrodes for applications in both analytical and industrial electrochemistry, because in addition to their low price, they exhibit suitable electrocatalytic activity for a variety Abstract In the present study a glassy carbon electrode, modified with nanocomposite of gold nanoparticles/multiwalled carbon nanotubes (GNPs/MWCNTs/GCE), was used for determination of dicyclomine hydrochloride (DcCl). The results showed that synergetic effects of GNPs and MWCNTs highly improved electrochemical response and sensitivity of the sensor. The electrochemical oxidation of DcCl was investigated by cyclic voltammetry and differential pulse voltammetry. Also, scanning electron microscopy and energy dispersive x-ray spectroscopy were used to evaluate microstructure of electrochemical sensor. The effect of various experimental parameters including pH and scan rate on the voltammetric response of DcCl were investigated. Under the optimal conditions linear response was observed in range of 1.0-1.2 × 10 2 µmol L −1 for DcCl. The lower detection limit was found to be 0.40 µmol L −1 for DcCl. The investigated method showed good stability, reproducibility and repeatability. The proposed sensor was successfully applied to the determination of DcCl in real samples.