A simple sensitive and quick assay for simultaneously determining magnolol (MOL) and honokiol (HOL) has been described based on their natural fluorescence. This method is based on the fact that synchronous fluorometry could resolve the overlapping of fluorescence spectra, which was aroused by their similar molecular structures. In this work, the synchronous spectrum, maintaining a constant difference of ?λ =10 nm between the emission and excitation wavelengths, has been selected for the determination of HOL and MOL. Under the optimum conditions, the fluorescence intensity is proportional to the concentration of MOL and HOL in solution over the range 0.075-0.7 μg/mL and 0.05-0.9 μg/mL with the detection limit of 0.029 μg/mL and 0.019 μg/mL, respectively. The method was applied to the simultaneous determination of MOL and HOL in pharmaceutical dosage with satisfactory results. A simple sensitive and quick assay for simultaneously determining magnolol (MOL) and honokiol (HOL) has been based on the fact that synchronous fluorometry could resolve the overlapping of fluorescence spectra, which was aroused by their similar molecular structures. In this work, the synchronous spectrum, maintaining a constant difference of? = 10 nm between the emission and the excitation wavelengths, has been selected for the determination of HOL and MOL. Under the optimum conditions, the fluorescence intensity is proportional to the concentration of MOL and HOL in solution over the range 0.075-0.7 μg / mL and 0.05-0.9 μg / mL with the detection limit of 0.029 μg / mL and 0.019 μg / mL, respectively. The method was applied to the simultaneous determination of MOL and HOL in pharmaceutical dosage with satisfactory results.