In recent years, fabrication of inorganic-organic composites mimicking the composite nature of real bone has attracted research interest in the field of bone regeneration. Investigations on composites composed of bioactive calcium phosphate phases and synthetic biodegradable polymers for biomedical applications appear to be an advanced topic in biomaterials research. The efforts include variation in composition, fabrication methods and clinical evaluation. In this study, Sr and Mg containing hydroxyapatite (HAp)-poly(vinyl alcohol) (PVA) microspheres were fabricated by spray drying method. The aim of this study was to evaluate the effect of preparation technique on the physico-chemical characteristic of microspheres. Microspheres were obtained using two different preparation techniques and their physic-chemical characteristics such as shape of the microspheres, morphology and particle size, chemical and phase composition were investigated.