A tricalcium phosphate (TCP) material was produced from sardine and mackerel waste using a heat treatment method after a Soxhlet extraction to obtain the non-soluble portion of fish waste. The bones were annealed at temperatures between 400°C and 1200°C. The thermal analysis (TG-DTA) was carried out to investigate the thermal stability of TCP and to confirm the removal of organic matter from the raw fish. The calcined bones were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), and field emission scanning electron microscopy (FE-SEM). The calcium to phosphorous weight ratio was determined by ICP-AES. FT-IR and XRD confirmed the similarities to synthetic β-TCP (JCPDS-09-169), FE-SEM results revealed the formation of nanostructured TCP. These results suggest that varying the isolation temperature between 600-1200°C has tremendous impact on the production of TCP from fish bone waste with the required properties.