In this report, we demonstrate a novel way to tune the fluorescence property of electrospun conjugated polymer fibers. The basic strategy is to use a soluble precursor polymer with gold nanoparticies for electrospinning, which is then cross-linked by applying potential cycles in an electrochemical cell. Electroactive carbazole units in electrospun precursor polymer fibers were converted to conjugated polymer fibers. Since the conjugated polymer fibers can be formed, the fluorescence from the conjugated polymer fibers can be tuned by the rate of the conversion and doping of the fibers. Furthermore, the quenching of the fluorescence, which overlaps with the plasmon band of the gold nanoparticles, was observed. The quenching of the fluorescence properties of the fibers was dependent on the amount of gold nanoparticles inside the fibers.