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Solid-State (31)P and (1)H NMR Investigations of Amorphous and Crystalline Calcium Phosphates Grown Biomimetically From a Mesoporous Bioactive Glass
Stockholms universitet, Naturvetenskapliga fakulteten, Institutionen för material- och miljökemi (MMK), Avdelningen för fysikalisk kemi.
Stockholms universitet, Naturvetenskapliga fakulteten, Institutionen för material- och miljökemi (MMK), Avdelningen för fysikalisk kemi.
Stockholms universitet, Naturvetenskapliga fakulteten, Institutionen för material- och miljökemi (MMK), Avdelningen för oorganisk kemi och strukturkemi.
Vise andre og tillknytning
2011 (engelsk)Inngår i: The Journal of Physical Chemistry C, ISSN 1932-7447, E-ISSN 1932-7455, Vol. 115, nr 42, s. 20572-20582Artikkel i tidsskrift (Fagfellevurdert) Published
Abstract [en]

By exploiting (1)H and (31)P magic-angle spinning nuclear magnetic resonance (NMR) spectroscopy, we explore the proton and orthophosphate environments in biomimetic amorphous calcium phosphate (ACP) and hydroxyapatite (HA), as grown in vitro at the surface of a 10CaO-85SiO(2)-5P(2)O(5) mesoporous bioactive glass (MBG) in either a simulated body fluid or buffered water. Transmission electron microscopy confirmed the presence of a calcium phosphate layer comprising nanocrystalline HA Two-dimensional (1)H-(31)P heteronudear correlation NMR established predominantly (1)H(2)O <->(31)PO(4)(3-) and O(1)H <->(31)PO(4)(3-) contacts in the amorphous and crystalline component, respectively, of the MBG surface-layer; these two pairs exhibit distinctly different (1)H <->(31)P cross-polarization dynamics, revealing a twice as large squared effective (1)H-(31)P dipolar coupling constant in ACP compared with HA. These respective observations are mirrored in synthetic (well-crystalline) HA, and the amorphous calcium orthophosphate (CaP) clusters that are present in the pristine MBG pore walls: besides highlighting very similar local (1)H and (31)P environments in synthetic and biomimetic HA, our findings evidence closely related NMR characteristics, and thereby similar local structures, of the CaP clusters in the pristine MBG relative to biomimetic ACP.

sted, utgiver, år, opplag, sider
2011. Vol. 115, nr 42, s. 20572-20582
HSV kategori
Forskningsprogram
fysikalisk kemi
Identifikatorer
URN: urn:nbn:se:su:diva-69910DOI: 10.1021/jp206237nISI: 000296205600031OAI: oai:DiVA.org:su-69910DiVA, id: diva2:479653
Merknad

authorCount :8

Tilgjengelig fra: 2012-01-18 Laget: 2012-01-15 Sist oppdatert: 2017-12-08bibliografisk kontrollert
Inngår i avhandling
1. Composition-Structure Correlations of Bioactive Glasses Explored by Multinuclear Solid-state NMR Spectroscopy
Åpne denne publikasjonen i ny fane eller vindu >>Composition-Structure Correlations of Bioactive Glasses Explored by Multinuclear Solid-state NMR Spectroscopy
2015 (engelsk)Doktoravhandling, med artikler (Annet vitenskapelig)
Abstract [en]

This PhD thesis presents a study of structure-composition correlations of bioactive glasses (BGs) by employing solid-state Nuclear Magnetic Resonance (NMR) spectroscopy.

Silicate-based Na2O−CaO−SiO2−P2O5 BGs are utilized clinically and are extensively investigated for bone regeneration purposes. Once implanted in the human body, they facilitate bone regeneration by partially dissolving in the body fluids, followed by the formation of a biomimetic surface-layer of calcium hydroxy-carbonate apatite (HCA). Eventually, the implanted BG totally integrates with the bone. The bioactivity of melt-prepared BGs depends on their composition and structure, primarily on the phosphorus content and the average silicate-network connectivity (NC). We explored these composition-structure relationships for a set of BGs for which the NC and phosphorus contents were varied independently.

The short-range structural features of the glasses were explored using 29Si and 31P magic-angle-spinning (MAS) NMR spectroscopy. 31P MAS NMR revealed that the orthophosphate content is directly proportional to the total P content of the glass, with a linear correlation observed between the orthophosphate content and the silicate network connectivity. The bearings of the results for future BG design are discussed.

By using multiple-quantum coherence-based 31P NMR experiments, the spatial distribution of orthophosphate groups was probed in the melt prepared BGs, as well as in two mesoporous bioactive glasses prepared by an evaporation-induced self-assembly technique. The results evidence randomly distributed orthophosphate groups in the melt-prepared BGs, whereas the pore-walls of the mesoporous bioactive glasses constitute nanometer-sized clusters of calcium phosphate. The distribution of Na+ ions among the phosphate/silicate groups were studied by heteronuclear dipolar-based 23Na−31P NMR experiments, verifying that sodium is dispersed nearly randomly in the glasses.

The phosphorus and proton environments in biomimetically grown HCA were investigated by using 1H and 31P MAS NMR experiments. Our studies revealed that the biomimetic HCA shared many local structural features with synthetic and well-ordered hydroxy-apatite.

sted, utgiver, år, opplag, sider
Stockholm: Department of Materials and Environmental Chemistry (MMK), Stockholm University, 2015. s. 68
Emneord
bioactive glasses, glass structure, orthophosphate distribution, solid-state NMR, dipolar interactions, dipolar recoupling, multiple-quantum spin counting, READOR, REAPDOR
HSV kategori
Forskningsprogram
fysikalisk kemi
Identifikatorer
urn:nbn:se:su:diva-116232 (URN)978-91-7649-174-4 (ISBN)
Disputas
2015-06-03, Magnéli Hall, Arrhenius Laboratories, Svante Arrhenius väg 16 B, Stockholm, 13:00 (engelsk)
Opponent
Veileder
Merknad

At the time of the doctoral defense, the following paper was unpublished and had a status as follows: Paper 4: Accepted.

Tilgjengelig fra: 2015-05-11 Laget: 2015-04-15 Sist oppdatert: 2019-10-02bibliografisk kontrollert

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