The simultaneous determination of harman, harmaline and norharman has been described using synchronous fluorescence technique. The method has been based on their natural fluorescence. It is difficult to analyze and determine their contents by conventional fluorescence method because of their similar molecular structures. The synchronous spectrum, maintaining a constant wavelength difference of ${Delta}{lambda}=185nm$ between the excitation and emission monochromators, was selected as optimum to perform the determination. The method was also performed in aqueous medium at pH 4.0 and in presence of sodium dodecyl sulfate (SDS), $1{ imes}10^{-5}M$. Under the optimum conditions, each analyte has the linear determination range of $1{ imes}10^{-7}M-;1{ imes}10^{-4}M$.