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

Kaflak, Agnieszka; Chmielewski, Dariusz; Górecki, Andrzej; Ślósarczyk, A.; Kołodziejski, Wacław

doi:10.1016/j.ssnmr.2005.11.005

Cited by 27 publications

(18 citation statements)

References 28 publications

(34 reference statements)

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“…Additional experiments are underway to corroborate this interpretation. In a recent 31 P{ 1 H} CPMAS study of the chemical interaction of phosphoric acid ester with HAp, the signal of pyrophosphate at ca -15 ppm was observed, showing that P-O-P linkages are formed between the ester molecules and the phosphate groups on the HAp surface. [39] In our system, we have no spectroscopic evidence for any P-O-P linkages.…”

Section: Discussionmentioning

confidence: 99%

“…The pulse sequence is taken from the literature. [43] During the cross-polarization (CP) contact time (0.5 ms), the 1 H nutation frequency was set to 50 kHz and that of 31 P was ramped through the Hartmann-Hahn matching condition. [44] Recycle delay was set to 4 s. The durations of the magic-angle pulse and π /2 pulse were set to 3.0 and 5.0 µs, respectively.…”

Section: Solid-state Nmrmentioning

confidence: 99%

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Solid‐state P‐31 NMR study of the formation of hydroxyapatite in the presence of glutaric acid

Tseng

Mou

Chen

et al. 2008

Magnetic Reson in Chemistry

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We demonstrate that glutaric acid can be used to prepare nanorods of hydroxyapatite under hydrothermal condition at 100 degrees C with a Ca(2+):glutaric acid molar ratio of 1:4. Frequency-switched Lee-Goldburg irradiation is employed to obtain high-resolution (31)P{(1)H} correlation spectra of the reaction mixture at two different reaction periods, from which it is shown that octacalcium phosphate is the precursor phase of the final hydroxyapatite product. In addition, the spectra show that a substantial amount of water molecules is trapped between the glutaric acid and the hydroxyapatite surface, indicating that water molecules may play a prominent role in the noncovalent interaction of the glutaric acid and the HAp surface.

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Section: Discussionmentioning

confidence: 99%

Section: Solid-state Nmrmentioning

confidence: 99%

Solid‐state P‐31 NMR study of the formation of hydroxyapatite in the presence of glutaric acid

Tseng

Mou

Chen

et al. 2008

Magnetic Reson in Chemistry

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“…This, in turn, implies adequate resemblance between the apatite structures, in accordance with many earlier publications, including our NMR works. [1,24,34,48] They showed that the bone apatite is in fact carbonatoapatite and that it is deficient in the structural OH groups. If the apatite crystals are very small, e.g.…”

Section: Discussionmentioning

confidence: 99%

“…[24,34,35,48] Stoichiometric HA was synthesized by the wet chemical method with the Ca/P ratio of 1.67. [49] It was predried in air to give as-synthesized sample HAh.…”

Section: Methodsmentioning

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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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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“…The mineral has been classified by solid-state nuclear magnetic resonance (NMR) as a biological carbonate apatite of either type A or type B, due to its heterogenic composition [Kolodziejski, 2005;Kaflak et al, 2006]. In comparison to enamel, dentine consists of a larger variety of proteins [Linde, 1989;Fujisawa and Kuboki, 1990;Linde and Goldberg, 1993], where linkages to the mineral appear to arise from acidic non-collagenous proteins [Boskey, 1989;Butler and Ritchie, 1995;Duer et al, 2009;Iline et al, 2015].…”

mentioning

confidence: 99%

Molecular Insights into Covalently Stained Carious Dentine Using Solid-State NMR and ToF-SIMS

Almhöjd

Lingström²,

Nilsson³

et al. 2017

Caries Res

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Dyes currently used to stain carious dentine have a limited capacity to discriminate normal dentine from carious dentine, which may result in overexcavation. Consequently, finding a selective dye is still a challenge. However, there is evidence that hydrazine-based dyes, via covalent bonds to functional groups, bind specifically to carious dentine. The aim of this study was to investigate the possible formation of covalent bonds between carious dentine and ¹⁵N₂-hydrazine and the hydrazine-based dye, ¹⁵N₂-labelled Lucifer Yellow, respectively. Powdered dentine from extracted carious and normal teeth was exposed to the dyes, and the staining reactions were analysed using time-of-flight secondary ion mass spectrometry (ToF-SIMS), solid-state ¹³C-labelled nuclear magnetic resonance (NMR) and ¹⁵N-NMR spectroscopy. The results showed that ¹⁵N₂-hydrazine and ¹⁵N₂-labelled Lucifer Yellow both bind to carious dentine but not to normal dentine. It can thus be concluded that hydrazine-based dyes can be used to stain carious dentine and leave normal dentine unstained.

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

Cited by 27 publications

References 28 publications

Solid‐state P‐31 NMR study of the formation of hydroxyapatite in the presence of glutaric acid

Solid‐state P‐31 NMR study of the formation of hydroxyapatite in the presence of glutaric acid

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

Molecular Insights into Covalently Stained Carious Dentine Using Solid-State NMR and ToF-SIMS

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

Cited by 27 publications

References 28 publications

Solid‐state P‐31 NMR study of the formation of hydroxyapatite in the presence of glutaric acid

Solid‐state P‐31 NMR study of the formation of hydroxyapatite in the presence of glutaric acid

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

Molecular Insights into Covalently Stained Carious Dentine Using Solid-State NMR and ToF-SIMS

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