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Based on microwave-assisted extraction (MAE) and headspace solid-phase microextraction (HS-SPME) followed by gas chromatography mass spectrometry (GC-MS) was developed for the fast determination of volatile chemical compositions of Polygala furcata Royle, the experimental parameters of the MAE-HS-SPME were optimized by orthogonal experimental design. The results indicated that the optimum condition of the determination of the volatile compounds in P. furcata Royle. was achieved with the experimental parameters including microwave power of 400 W and irradiation time of 4 min, sample size 2.0 g. Under the optimal conditions, for the Wrst time, 52 volatile compounds were separated and identiWed from the fresh plants of P. furcata Royle. The highest content component of the 52 compounds was 2-hydroxybenzoic acid methyl ester (21.65%). The relative standard deviation values <7% showed that the method of MAE-HS-SPME followed by GC-MS has good precision. The experimental results demonstrated that it is a simple, time-saving and solvent-free method, and it is a potential analytic tool for the determination of the volatile compounds of the vegetations materials and other materials.

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