Biphasic calcium phosphate (BCP) is a ceramic material that can promote bone regeneration. However, there are controversies about the proportions of the phases in which the BCP must be combined in order to maintain their biological activity. In this study, a novel biphasic calcium phosphate from fish otoliths containing mixed phases of hydroxyapatite/s-tricalcium phosphate (HA/s-TCP) was fabricated by aqueous precipitation technique. Three compositions of BCP and three compositions of hydroxyapatite (HA) from otoliths of teleost fish (Plagioscion squamosissimus) were studied. X-ray diffraction analysis revealed that, at low pH values, multiphase calcium phosphate compounds were formed, whereas at high pH values single-phase hydroxyapatite was formed after 96 h of precipitation time. SEM micrographs showed agglomeration of particles with porous structures, as well as the presence of nanosized particles. The different vibration modes3- of the P043- ion was identified by Raman spectroscopy and FTIR.