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Summary A novel method for separating and concentrating magnolol and honokiol from Magnoliae Cortex by solvent sublation and analysis of the compounds by high-performance liquid chromatography (HPLC) has been established. The optimum conditions for solvent sublation were use of n-butanol as sublation solvent, sample solution at pH 2, nitrogen flow 50 mL min–1, and sublation time 50 min. The floating product obtained under the optimum conditions was determined by HPLC analysis on a C18 reversed-phase column, with 22:78 (%, v/v) water-methanol as isocratic mobile phase at a flow rate of 1.00 mL min–1. When the method was used for quantification of magnolol and honokiol in Magnoliae Cortex recovery ranged from 98.1 to 106.1%, RSD was from 3.07 to 4.80%, and LOD for honokiol and magnolol were 0.94 and 1.14 ng mL–1, respectively.