This study examined the gradual replacement of Ca2+ with a small amount of Mg2+ ions (0-1 wt.%) in selected calcium phosphates commonly used in regenerative medicine: hydroxyapatite Ca10(PO4)6(OH)2, brushite CaHPO4∙2H2O, and β-tricalcium phosphate (βTCP) Ca3(PO4)2. These compounds were obtained using precipitation reactions from aqueous solutions, followed by appropriate thermal treatment (drying or furnace heating). The microstructure and physicochemical properties of the materials were thoroughly analysed using powder X-ray diffraction (PXRD), scanning and transmission electron microscopy (SEM and TEM), and mid-infrared spectroscopy (FT-IR). Additionally, the release of Mg2+ ions from the selected materials was investigated, and a preliminary in vitro toxicity assessment was performed.The results showed that the introduction of magnesium ions up to 1 wt.% was achieved with relatively high efficiency (63-82% for brushite, 77-97% for hydroxyapatite, and 88-100% for β-tricalcium phosphate). The entire series of hydroxyapatites was phase-homogeneous, but monetite was observed as an additional phase in the case of brushite samples. In contrast, several βTCP samples were contaminated with a small amount of calcium oxide and hydroxide. The incorporation of Mg2+ ions significantly impacted the unit cell parameters of each type of calcium phosphate and the ultrastructure of the obtained powders. With an increase in the amount of introduced magnesium, the resulting crystals became smaller and showed a greater tendency to form aggregates. The obtained results indicate that it is possible to obtain calcium phosphate materials containing Mg2+ ions with a gradual release of ions. The fastest ions release occurred from the brushite sample, while the slowest was from the apatitic powder, which is in great accordance with the solubility of the materials. All samples, except for Mg0.5-Bru, were non-cytotoxic.