The purpose of this study is to find out an effective method to prepare natural hydroxyapatite (HA) from biological source, i.e., pig bones, pig teeth, and extracted human teeth. For the preparation of natural HA a calcining method with different temperatures was used, in combination with the thermal gravimetric analysis (TGA). Three analysis methods, i.e., Fourier transform infrared spectroscope (FTIR), X-ray diffraction (XRD), and inductively coupled plasma (ICP) have been used to investigate the characteristics of the prepared materials. The spectrum of the prepared material, obtained by means of FTIR and XRD, are consistent with the standard FTIR spectrum and JCPDS index of XRD of hydroxyapitite. It confirms that the material prepared is hydroxyapitite indeed. The natural HA obtained by calcining at 850°C shows a desired quality.