In this study, a method to produce a fine volatile powder extracted from shiitake mushrooms using spray freeze-drying (SFD) was investigated. The analysis of the water-soluble aromatic compounds was carried out by headspace solid phase micro-extraction (HS-SPME) coupled withgas chromatography-mass spectrometry (GC-MS). Scanning electron microscopy (SEM) and laser particle size analysis were applied to characterizethe physical structure and size distribution of the SFD-derivedparticles. Eleven key volatile compounds were identified in the extracts of shiitake mushroomspre- and post-SFD. Recoveries of aromatic volatiles ranging from 30.9 - 82.9% were observed in the overall flavor profile results from the powder obtained with SFD. SEM analysis demonstrated that the particles of the aromatic powderwere spherical in nature, having highly porous surfaces andmean diameters of 19.3 μm.