Tthe composition and structure of composite particles obtained by PGSS (Particle from Gas Saturated Solution particles produced from gas-saturated solutions) method were investigated. The melting temperature of the particles was determined by thermogravimetric analysis. The structures of the particles were determined by X-ray analysis. Investigated the composition of composite particles by gas chromatography-mass spectrometry for the determination of electron ionization ibuprofen content and mass spectrometry Matrix-assisted laser desorption / ionization (MALDI) for determining the content of polyethylene glycol 4000 (PEG 4000).