2-Pyridine carboxaldehyde furfuralhydrazone (PCFH) was newly synthesized and its ionization, IR and elemental analysis were established. An on-line separation and preconcentration systemwas developed for the flowinjection (FI) catalytic kinetic spectrofluorimetric determination of trace amounts of gold. The methodwas based on the fluorescence enhancing reaction of PCFH with potassium bromate, whichwas catalysed by Au3+ in aqueous medium at pH 4.20 and 35℃. Amicro polyamide resin columnwas used to separate and collect gold from sample solution. Under these experimental conditions, the oxidized product of PCFH had excitation and emission maxima at 296 and 404 nm, respectively. The linear range of this method was 0.53-144ngml−1 with the RSD of 1.6%. The detection limit was 0.16ngml−1. A high analysis rate of 15 samples h−1 was obtained. The proposed method had been applied successfully to the determination of gold in synthetic mixture and mineral sample with satisfactory results.