A spectrophotometric method for determination microgram level of procainamide hydrochloride in tablets was described. The method was based on coloured Schiff’s base formation between procainamide and p-dimethylaminobenzaldehyde. The reaction proceeded quantitatively in acidic and ethanolic medium at room temperature in twenty minutes. The absorption maximum was at 449 nm. A linear relationship existed between absorbance and concentration over the range of 1-4 mcg.ml-1 of procainamide hydrochloride. The results of the analysis of procainamide hydrochloride tablets so obtained correlated well with those obtained by the USP XVIII method at 95% of confidence level. Keywords :