Micro-Analytical Comparison on Elemental Composition of Nonstoichiometric Bovine Bone Derived Hydroxyapatite

Abstract:

Hydroxyapatite (HA) is one of the most common ceramic materials used for bone substitutions or reconstructions [1]. HA synthesis from natural sources is convenient relative to synthetic HA preparation while ensuring a similarity with viable bone tissue in terms of chemical composition and some other properties. One of the most important markers used for hydroxyapatite identification and differentiation from other calcium phosphates is the Ca/P ratio [2]. In order to perform a proper identification, this ratio should be evaluated with high accuracy, which involves a correct determination of the elemental concentrations. This study was made on a series of samples, derived from bovine osseous tissue, thermaly treated at 1000, 1100 and 1200°C. Establishing the influence of sample preparation on the Ca/P ratio assessment from the energy dispersion spectrometry (EDS) coupled with scanning electron microscopy determinations was intended. The samples were prepared by two completely different methods: mechanical fracture (without further preparation) and milling followed by homogenization. Regardless the sample preparation method, the analytical results represents the five measurements average performed on different spots.The EDS results showed that, within the same group, the compositional dissimilarities between the samples treated at different temperatures do not exceed 10% regardless of the sample preparation technique. For the same thermal treatment temperature, slight differences between the elemental chemical compositions of differently prepared samples were observed. The most important effect was a 20% decrease of the average Ca/P ratio for the samples prepared by milling and homogenization in regard to the mechanical fractured ones. Thereby, heat treated bovine bone samples’ milling and further homogenization for performing semi quantitative EDS analysis allows the Ca/P ratio assessment with a better accuracy.

• Periodical: Key Engineering Materials (Volume 638)
• Pages: 3-7
• DOI: https://doi.org/10.4028/www.scientific.net/KEM.638.3
• Online since: March 2015
• Authors: Florin Miculescu, Lucian Toma Ciocan, Marian Miculescu*, Aura Mocanu, Andreea Maidaniuc, Alin Purcaru, Oana Preda
• Keywords: Bovine Bone Derived Hydroxyapatite, Ca/P Ratio, EDS

References

[1] J. Brandt, S. Henning, G. Michler, W. Hein, A. Bernstein, M. Schulz, Nanocrystalline hydroxyapatite for bone repair: an animal study, J. Mater. Sci. Mater. Med. 21 (2010) 283-294.

DOI: 10.1007/s10856-009-3859-1

[2] S.V. Dorozhkin, Calcium Orthophosphates in Nature, Biology and Medicine, Materials 2 (2009) 399-498.

DOI: 10.3390/ma2020399

[3] M. Rajkumar, N. Meenakshi Sundaram, V. Rajendran, Preparation of size controlled, stoichiometric and bioresorbable hydroxyapatite nanorod by varying initial pH, Ca/P ratio and sintering temperature, Dig. J. Nanomater. Bios 6 (2011) 169-179.

[4] G. E. Stan, C. O Morosanu, D. A. Marcov, I. Pasuk, F. Miculescu, G. Reumont, Effect of annealing upon the structure and adhesion properties of sputtered bio-glass/titanium coatings, Applied Surface Science, 255 (2009) 9132-9138.

DOI: 10.1016/j.apsusc.2009.06.117

[5] S. Pramanik, A. S. M. Hanif, B. Pingguan-Murphy, N. A. Abu Osman, Morphological Change of Heat Treated Bovine Bone: A Comparative Study, Materials 6 (2013) 65-75.

DOI: 10.3390/ma6010065

[6] G. Nechifor, S.I. Voicu, A.C. Nechifor, S. Garea, Nanostructured hybrid membrane polysulfone-carbon nanotubes for hemodialysis, Desalination 241(1-3) (2009) 342-348.

DOI: 10.1016/j.desal.2007.11.089

[7] M. Figueiredo, A. Fernando, G. Martins, J. Freitas, F. Judas, H. Figueiredo, Effect of the calcination temperature on the composition and microstructure of hydroxyapatite derived from human and animal bone, Ceramics International 36 (2010).

DOI: 10.1016/j.ceramint.2010.07.016

[8] A. Sobczak, Z. Kowalski, Z. Wzorek, Preparation of hydroxyapatite from animal bones, Acta of Bioengineering and Biomechanics 11 (2009) 23-28.

[9] F. Miculescu, L.T. Ciocan, M. Miculescu, A. Ernuteanu, Effect of heating process on micro structure level of cortical bone prepared for compositional analysis, Dig. J. Nanomater. Bios. 6 (2011) 225-233.

[10] N. Kourkoumelis, I. Balatsoukas, M. Tzaphlidou, Ca/P concentration ratio at different sites of normal and osteoporotic rabbit bones evaluated by Auger and energy dispersive X-ray spectroscopy, J Biol Phys (2012) 38 279-291.

DOI: 10.1007/s10867-011-9247-3

[11] S.I. Voicu, A.C. Nechifor, B. Serban, G. Nechifor, M. Miculescu, Formylated Polysulfone. Membranes for Cell Immobilization, J. Opt. Adv. Mater. 9 (2007) 3423-3426.

[12] N. D. Pinchuk, L. A. Ivanchenko, Making calcium phosphate biomaterials, Powder Metallurgy and Metal Ceramics 42 (2003) 7-8.

DOI: 10.1023/b:pmmc.0000004155.75027.cc

[13] F. Miculescu, M. Miculescu, L.T. Ciocan, I. Pencea, A. Ernuteanu, E. Matei, Correlation of spectometric methods in hard tissue heavy elements concentration study, U.P.B. Sci. Bull A 75 (2013) 233-242.

DOI: 10.4028/www.scientific.net/ssp.188.37

[14] N.A.M. Barakat, K. A. Khalil F. A. Sheikh, A. M. Omran, B. Gaihre, Physiochemical characterizations of hydroxyapatite extracted from bovine bones by three different methods: extraction of biologically desirable Hap, Mater. Sci. Eng. C 28 (2008).

DOI: 10.1016/j.msec.2008.03.003

[15] G.E. Stan, S. Pina, D.U. Tulyaganov, DU J.M.F. Ferreira, I. Pasuk, I C.O. Morosanu, Biomineralization capability of adherent bio-glass films prepared by magnetron sputtering, Journal Of Materials Science-Materials In Medicine, 21(4) (2010).

DOI: 10.1007/s10856-009-3940-9

[16] C. Lorprayoon, Phases of cattle bones at elevated temperatures, J Sci Soc Thailad 12 (1986) 159-170.

[17] G. A. da Cruz, S. de Toledo, E. A. Sallum, A. F. M. de Lima, Morphological and Chemical Analysis of Bone Substitutes by Scanning Electron Microscopy and Microanalysis by Spectroscopy of Dispersion Energy, Braz Dent J 180 (2007) 129-133.

DOI: 10.1590/s0103-64402007000200008