Fluorometric determination of dl-Methylephedrine hydrochloride from complex preparation were studied. According to the experimental results and considerations obtained the results for the following. (1) dl-Methylephedrine hydrochloride in Hydrochloric acid media occurs the fluorescens by Picrolonic acid and Cuppric acetate. (2) The maximum absorption fluorescence wave length of dl-Methylephedrine hydrochloride standard solution is $365m{mu}$. (3) The relationship between the fluorescence proportions to concentration of standard solution at range of $4.2{ imes}10^{-4};M$. $6{ imes}10^{-4}M$. (4) dl-Methylephedrine hydrochloride was precisely determined even in the presence of various components, especially Chloropheniramine maleate, Dextromethorphan hydrobromide and Diphenylhydramine hydrochloride. (5) This method has high sensitivity and is simple in precedure. (6) This method be applicable with 99.79% accuracy and was 99.5% in complex preparation.