Subcritical water is an environmentally friendly method with a wide range of applications, such as extraction, hydrolysis, and wet oxidation of organic compounds. Here, water at subcritical conditions was applied to extract polysaccharides from Ganoderma lucidum (G. lucidum) and barley grains at 120 -180 o C and 4.0 MPa using a semi-batch system. The liquid products were directly micronized and contacted with hot air to form microsphere particles. During extraction process, cell wall disruptions of G. lucidum and barley grains took place, allowing the removal of the polysaccharides isolating other constituents in G. lucidum and barley grains via autohydrolysis. Scanning electron microscope (SEM) images described that the particle products produced had sphere and wrinkled morphology of particles with diameters varying from 1 to 10 µm. The experimental result revealed that the particles formed from G. lucidum and barley grains extract contained 40-45% and 30-35% weight β-glucan, respectively.