A new fluorescent reagent, 2-hydroxy-1-naphthaldehydene-8-aminoquinoline (HNAAQ), was synthesized. The fluorescent reaction of this reagent with lead was also studied. Based on this chelation, a highly sensitive spectrofluorimetric method was developed for the determination of trace amounts of lead in a water-ethanol (5 + 1, v/v) medium at pH = 9.4. Under these conditions, the Pb-HNAAQ complex has excitation and emission maxima at 398 and 450 nm, respectively. The linear range of the method is from 0 to 100 microg l(-1) and detection limit is 0.28 microg l(-1) of lead. Interference of other ions was studied. In strongly basic media most interfering metal ions form precipitates of hydroxides or oxides and can be removed efficiently through filtration while the residual cations can be removed with a cation-exchange resin. Hence, the selectivity of the method can be increased considerably. The procedure can easily be performed and affords good precision and accuracy. The method was successfully applied to the determination of lead in wheat and rice flour.