The electrosynthesis and characterisation of polypyrrole(PPy) films with a micro-tubular structure decorated with gold nanoparticles is described. The PPy films were characterised by means of voltammetric and electro-chemical impedance spectroscopy measurements. The tubular structure of the PPy films were obtained under potentiostatic conditions in freshly prepared sodium salicylate solutions. Voltammetric response of the PPy films shows that its behavior turns more reversible as the electropolymerization charge of the film increases. SEM images show the appearance of the tubular structure for an electrodeposition time higher than 2 min. The tubular-structured PPy film showed an rms of ca. 600 nm as determined from AFM imaging. These PPy films were subsequently decorated with gold nanoparticles obtained by a double step potentiostatic electrodeposition routine that allowed fine control of deposit characteristics. Analysis of deposits was performed by means of SEM and AFM nanoscopy. Statistical analysis of particles size distribution show that the maximum value appeared for 60 nm, but a significant amount of particles between 100-200 nm were also observed. The sensing capability of these composite electrodes was tested for the determination of hydroxylamine, nitrite and their mixture in solutions of different pH. Results showed a successful route of synthesis of a nanocomposite electrode with promising applications in electrochemical sensing.