This study was conducted to examine effect of calcination temperature on synthesis of calcium hydroxyphosphate (hydroxyapatite) from tilapia fish bones and scales for protein enhancement in wheat flour. The raw bones and scales were undergoing calcination process to produce hydroxyapatite powder. The obtained hydroxyapatite powder was characterized using several techniques such as Fourier-Transform infrared spectroscopy (FTIR), scanning electron microscope (SEM), proximate analysis and X-ray diffraction (XRD). The results indicate that temperature 1000 °C has the highest weight loss with 21.825 g compared to the temperature 800 °C and 900 °C. From FTIR analysis, the presence of characteristic peaks for hydroxyl group, phosphate groups and water molecule indicated that the powder were hydroxyapatite. SEM results showed that increasing temperature had led to more dense structure. The hydroxyapatite powder were analysed for their proximate composition. The results proved that temperature 1000 °C had higher ash and fat content than the wheat flour. The moisture and crude protein content were lower at temperature 1000 °C as compared to the wheat flour. The phase and stability of hydroxyapatite powder was confirmed by XRD analysis. Based on this study, it revealed that produced pure hydroxyapatite from natural resources at a suitable temperature was a good way and beneficial to food industry.