A spectrofluorimetric analysis of procaine using fluorescamine as a fluorogenic reagent, has been developed. The analytical parameters for optimal reaction and sensitivity (pH, fluorescamine, concentration, temperature, reaction time), have minuciously been studied. The present method may be employed for the analysis of procaine by normal fluorescence, without interferences from other compounds. The minimum detectable quantity, using the later technique, is estimated as 7.7 ng ml^-1, with a relative standard deviation of 2.16% (10 determinations) for a procaine concentration of 100 ng ml^-1. Three pharmaceutical preparations have been satisfactorily analysed.