Composites of multiwall carbon nanotubes (MWNTs), polyaniline (PANI), and gold nanoparticles were prepared by one pot synthesis. Based on the interaction between aniline monomers and MWNTs, aniline molecules were adsorbed and polymerized on the surface of MWNTs. The nanocomposites were characterized by transmission electron microscopy (TEM), X-ray diffraction analysis (XRD), Fourier transform infrared spectroscopy (FT-IR), and X-ray photoemission spectroscopy (XPS). The sensors based on Au/PANI/MWNT nanocomposites were tested for on-line monitoring of ammonia gas. The results show that the as-prepared sensors have superior sensitivity, and good repeatability upon repeated exposure to ammonia gas.