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Int. J. Mol. Sci. 2015, 16(5), 11452-11464; doi:10.3390/ijms160511452

A Solid-State NMR Study of Selenium Substitution into Nanocrystalline Hydroxyapatite

Department of Inorganic and Analytical Chemistry, Faculty of Pharmacy with the Laboratory Medicine Division, Medical University of Warsaw, ul. Banacha 1, 02-097 Warsaw, Poland
These authors contributed equally to this work.
These authors contributed equally to this work.
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Author to whom correspondence should be addressed.
Academic Editor: Mohamed N. Rahaman
Received: 1 March 2015 / Revised: 9 April 2015 / Accepted: 29 April 2015 / Published: 19 May 2015
(This article belongs to the Special Issue Biomaterials for Tissue Engineering)
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Abstract

The substitution of selenium oxyanions in the hydroxyapatite structure was examined using multinuclear solid-state resonance spectroscopy (ssNMR). The study was supported by powder X-ray diffractometry (PXRD) and wavelength dispersion X-ray fluorescence (WD-XRF). Samples of pure hydroxyapatite (HA300) and selenate (HA300-1.2SeO4) or selenite (HA300-1.2SeO3) substituted hydroxyapatites were synthesized using the standard wet method and heated at 300 °C to remove loosely bonded water. PXRD data showed that all samples are single-phase, nanocrystalline hydroxyapatite. The incorporation of selenite and selenate ions affected the lattice constants. In selenium-containing samples the concentration of Se was very similar and amounted to 9.55% and 9.64%, for HA300-1.2SeO4 and HA300-1.2SeO3, respectively. PXRD and ssNMR data showed that the selenite doping significantly decreases the crystallite size and crystallinity degree. 31P and 1H NMR experiments demonstrated the developed surface hydrated layer in all samples, especially in HA300-1.2SeO3. 1H NMR studies showed the dehydroxylation of HA during the selenium oxyanions substitution and the existence of hydrogen bonding in structural hydroxyl group channels. 1H→77Se cross polarization NMR experiments indicated that selenites and selenates are located in the crystal lattice and on the crystal surface. View Full-Text
Keywords: biomaterials; calcium phosphates; hydroxyapatite; selenium oxyanions; solid-state nuclear magnetic resonance; powder diffractometry biomaterials; calcium phosphates; hydroxyapatite; selenium oxyanions; solid-state nuclear magnetic resonance; powder diffractometry
This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. (CC BY 4.0).

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MDPI and ACS Style

Kolmas, J.; Kuras, M.; Oledzka, E.; Sobczak, M. A Solid-State NMR Study of Selenium Substitution into Nanocrystalline Hydroxyapatite. Int. J. Mol. Sci. 2015, 16, 11452-11464.

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