Deconvoluted X-ray diffraction analysis of bone and mixtures of bone and particulate hydroxyapatite

Recent evidence suggests that bone phosphate exists almost entirely as hydroxyapatite (HA). The relative deficiency of calcium and presence of substantial HPO2-4 in bone phosphate indicates modification of the ideal HA structure, however. An inability to resolve closely spaced lines in fine grained materials, coupled with the limited periodicity of the thin mineral crystals of bone have prevented definitive characterization of the structure of bone mineral using standard X-ray diffraction (XRD) techniques. We have applied computer deconvolution XRD techniques to aid in the resolution of component overlapped profiles from bone, synthetic hydroxyapatite (HA) and mixtures of bone and synthetic HA resulting from implantation studies. In the course of this resolution process separate profiles were resolved from the (002) profile of bone derived HA. The ratio of integrated intensities of these profiles to the intensity of the profile of synthetic HA appears to provide an approximate measure of the ratio of bone to synthetic HA in a given sample. The finding of shoulders on the (002) peak of bone provides the basis for resolution into separate profiles. The asymmetry of these shoulders in mature bone cannot be attributed to crystallinity, particle size, or computer artifact. The same finding has been previously reported in hydrolyzed, deproteinated bone. Further work will be needed to resolve the question of whether the structural heterogeneity implied by profile geometry is the result of multiple HA phases, surface layer structure involving hydrolysis and calcium absences, or some other factor.