Herein, a facile route to fabrication of carbon nanofibers/polyaniline/Au nanofibers (CPANFs) with tunable densities of gold nanoparticles (AuNPs) was proposed, and the potential application of the CPANFs as efficient electrochemical detector of H 2 O 2 was demonstrated. First, carbon nanofibers (CNFs) were successfully obtained through the carbonization procedure using electrospun polyacrylonitrile (PAN) nanofibers as a precursor. Then, polyaniline (PANI) nanorods were coated on the CNFs by an in situ polymerization of aniline, in which AuNPs were homogenously distributed via gold-thiol binding interactions. Finally, an aqueous nafion solution was used to attach HRP-modified CPANFs to the pretreated glassy carbon electrode (GCE) for H 2 O 2 detection. The fabricated electrochemical detectors for H 2 O 2 exhibited a high sensitivity for detection of H 2 O 2 with a detection limit of 0.18 μM at signal-to-noise ratio of 3.Nanoelectrode-based biosensors have been researched widely in recent years, since nanoelectrodes possess considerable advantages over conventional electrodes, such as higher spatial resolution, lower background noise, and voltammetric time scales. Due to these advantages, biosensors based on nanoelectrodes have gradually been incorporated into target detection for various fields. Hydrogen peroxide (H 2 O 2 ) is of particular interest because, as a strong oxidant and an industrial waste product, excess amounts of H 2 O 2 in rain and groundwater could negatively impact the environment. [1][2][3] As reported in the literature, sensors are often composed of two functional materials to achieve the recognition and transduction processes. Therefore, the majority of recent research on biosensors has focused on the development of modified electrode materials with high sensitivity and transduction. As a type of conducting polymer, PANI has become an attractive class of materials for a variety of advanced properties similar to metal materials, while retaining the flexibility and processability of conventional polymers. Typically, the use of individual materials has intrinsic defects, 4-6 so to improve upon electronic transduction, scientists combine PANI with carbon materials to form nanocomposites with superior performance. 7-13 CNFs are one of the most promising materials for fabrication of nanoelectrodes because of their chemical stability, high surface area, electrical conductivity, and relatively low cost.AuNPs are known to exhibit excellent optical and electronic properties in addition to their pronounced biocompatibility, which have been introduced onto the surface of conducting polymers for gene delivery 14,15 and development of biosensors. 16 Furthermore, AuNPs have been extensively used in electrochemical sensors due to their unique physicochemical properties. [17][18][19][20][21][22] With regards to small, welldispersed AuNPs grafted onto substrate materials, the fabrication of biosensors with low detection limits and a wide dynamic range for H 2 O 2 has become an intractable challenge for scienti...