Concentration of hydroxyl groups in dental apatites: a solid-state 1H MAS NMR study using inverse 31P →1H cross-polarization

Kolmas, Joanna; Kołodziejski, Wacław

doi:10.1039/b708317c

Cited by 54 publications

(90 citation statements)

References 25 publications

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“…[1] The inverse 31 P → 1 H CP has recently been performed on synthetic and dental apatites. [52] In this work, it is done on the apatite mineral of whole human bone (Fig. 5).…”

Section: A Singlementioning

confidence: 99%

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Kinetics of ¹H → ³¹P NMR cross‐polarization in bone apatite and its mineral standards

Kaflak

Kołodziejski

2008

Magnetic Reson in Chemistry

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Kinetics of NMR cross-polarization (CP) from protons to phosphorus-31 nuclei was studied in the following samples: mineral of whole human bone, apatite prepared from bone, natural brushite, synthetic hydroxyapatite (hydrated and calcined), and synthetic carbonatoapatite of type B with 9 wt% of CO(3) (2-). In order to avoid an effect of magic angle spinning on CP and relaxation, the experiments were carried out on static samples. Parameters of the CP kinetics were discussed for trabecular and cortical bone tissue from adult subjects in comparison to the synthetic mineral standards. It was found that carbonatoapatite shows similar CP behavior to the bone mineral. Both materials undergo two-component CP kinetics. The fast-relaxing classical component is from the surface of apatite crystals and the slow-relaxing nonclassical component comes from the crystal interior. The components have been unambiguously assigned using inverse CP from phosphorus-31 to protons. The study provides information on a structured water layer, which covers crystal surface of carbonato- and bone apatite. The layer encompasses ca 40% of apatite phosphorus and its thickness is more than ca 2 nm.

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“…[1] The inverse 31 P → 1 H CP has recently been performed on synthetic and dental apatites. [52] In this work, it is done on the apatite mineral of whole human bone (Fig. 5).…”

Section: A Singlementioning

confidence: 99%

“…The latter parameter reflects the 1 H-31 P dipolar couplings [51] and in the former publications [1,24,34,44,51,52] it has been designated by T 2 . For a rigid lattice λ = (n + 1) −1 , where n is the number of protons in close neighborhood of the observed 31 P nucleus.…”

Section: Theorymentioning

confidence: 99%

Kinetics of ¹H → ³¹P NMR cross‐polarization in bone apatite and its mineral standards

Kaflak

Kołodziejski

2008

Magnetic Reson in Chemistry

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“…Now, we would like to focus on the counting of the structural hydroxyl groups based on the 0.0 ppm signal area. The procedure for synthetic apatite was described in our former work [43]. In the present study, we used 1 H BD NMR under high-speed MAS with adamantane and NH 4 Cl as standards of the absolute proton intensity.…”

Section: H Mas Nmr Spectroscopymentioning

confidence: 99%

Incorporation of carbonate and magnesium ions into synthetic hydroxyapatite: The effect on physicochemical properties

Kolmas

Jaklewicz

Zima

et al. 2011

Journal of Molecular Structure

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“…Furthermore, using 31 P-1 H correlation experiments, a small quantity of HPO 4 2À anions 22,29,[35][36][37][38] in the surface regions of the mineral particles was evidenced, as well as an apparent lack of hydroxyl groups (OH À ) in the mineral phase relative to the ideal apatite structure. 26,39 NMR studies have also revealed that water has several different structural roles in the mineral, 40,41 and have allowed the local environment around minority anions like F À and CO 3 2À to be analysed. 23,[44][45][46][47] More recently, 13 C- 31 P correlation experiments have suggested that glycosaminoglycan molecules are located at the interface between the organic and mineral phases of bone and teeth.…”

Section: àmentioning

confidence: 99%

Probing the calcium and sodium local environment in bones and teeth using multinuclear solid state NMR and X-ray absorption spectroscopy

Laurencin

Wong

Chrzanowski

et al. 2010

Phys. Chem. Chem. Phys.

110

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International audienceDespite the numerous studies of bone mineral, there are still many questions regarding the exact structure and composition of the mineral phase, and how the mineral crystals become organised with respect to each other and the collagen matrix. Bone mineral is commonly formulated as hydroxyapatite, albeit with numerous substitutions, and has previously been studied by 31P and 1H NMR, which has given considerable insight into the complexity of the mineral structure. However, to date, there has been no report of an NMR investigation of the other major component of bone mineral, calcium, nor of common minority cations like sodium. Here, direct analysis of the local environment of calcium in two biological apatites, equine bone (HB) and bovine tooth (CT), was carried out using both 43Ca solid state NMR and Ca K-edge X-ray absorption spectroscopy, revealing important structural information about the calcium coordination shell. The 43Ca diso in HB and CT is found to correlate with the average Ca–O bond distance measured by Ca K-edge EXAFS, and the 43Ca NMR linewidths show that there is a greater distribution in chemical bonding around calcium in HB and CT, compared to synthetic apatites. In the case of sodium, 23Na MAS NMR, high resolution 3Q-MAS NMR, as well as 23Na{31P} REDOR and 1H{23Na} R3-HMQC correlation experiments give the first direct evidence that some sodium is located inside the apatite phase in HB and CT, but with a greater distribution of environments compared to a synthetic sodium substituted apatite (Na-HA)

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Concentration of hydroxyl groups in dental apatites: a solid-state 1H MAS NMR study using inverse 31P →1H cross-polarization

Abstract: The concentration of structural hydroxyl groups in the apatite mineral of enamel, dentin and cementum of healthy human teeth was estimated by reference to stoichiometric hydroxyapatite to be 73 +/- 3, 18 +/- 2 and 18 +/- 1%, respectively.

Cited by 54 publications

References 25 publications

Kinetics of ¹H → ³¹P NMR cross‐polarization in bone apatite and its mineral standards

Kinetics of ¹H → ³¹P NMR cross‐polarization in bone apatite and its mineral standards

Incorporation of carbonate and magnesium ions into synthetic hydroxyapatite: The effect on physicochemical properties

Probing the calcium and sodium local environment in bones and teeth using multinuclear solid state NMR and X-ray absorption spectroscopy

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Concentration of hydroxyl groups in dental apatites: a solid-state 1H MAS NMR study using inverse 31P →1H cross-polarization

Abstract: The concentration of structural hydroxyl groups in the apatite mineral of enamel, dentin and cementum of healthy human teeth was estimated by reference to stoichiometric hydroxyapatite to be 73 +/- 3, 18 +/- 2 and 18 +/- 1%, respectively.

Cited by 54 publications

References 25 publications

Kinetics of 1H → 31P NMR cross‐polarization in bone apatite and its mineral standards

Kinetics of 1H → 31P NMR cross‐polarization in bone apatite and its mineral standards

Incorporation of carbonate and magnesium ions into synthetic hydroxyapatite: The effect on physicochemical properties

Probing the calcium and sodium local environment in bones and teeth using multinuclear solid state NMR and X-ray absorption spectroscopy

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Kinetics of ¹H → ³¹P NMR cross‐polarization in bone apatite and its mineral standards

Kinetics of ¹H → ³¹P NMR cross‐polarization in bone apatite and its mineral standards