Nuclear Magnetic Resonance Spin-Spin Relaxation of the Crystals of Bone, Dental Enamel, and Synthetic Hydroxyapatites

Wu, Yaotang; Ackerman, Jerome L.; Kim, Hyun‐Man; Rey, Christian; Barroug, Allal; Glimcher, Melvin J.

doi:10.1359/jbmr.2002.17.3.472

Cited by 126 publications

(134 citation statements)

References 30 publications

(28 reference statements)

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“…In general, models of osteoporosis [44] and osteoporotic tissues in humans [45,46] are characterized by a decreased mineral/matrix ratio. No significant disparities ( p > 0.05) were observed between the two sex groups regarding the degree of mineralization, confirming previous studies [47] that are also related to the Ca/P ratio as a critical mineralization biomarker [48,49]. Trabecular bone apatite, represented by rib samples, shows decreased mineral deposited in the bone matrix in a highly significant manner ( p = 0.0002) compared to the compact sections.…”

Section: Band Analysis and Quantificationsupporting

confidence: 84%

Infrared spectroscopic assessment of the inflammation-mediated osteoporosis (IMO) model applied to rabbit bone

2012

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A model of osteoporosis based on induced inflammation (IMO) was applied to rabbit bones. The structural heterogeneity and molecular complexity of bone significantly affect bone mechanical properties. A tool like Fourier transform infrared spectroscopy, able to analyze both the inorganic and organic phase simultaneously, could provide compositional information regarding cortical and trabecular sections under normal and osteoporotic conditions. In this study, we assessed the mineral/matrix ratio, carbonate and phosphate content and labile (i.e., non-apatitic) species contribution to bone mineral and collagen cross-linking patterns. Clear differences were observed between cortical and trabecular bone regarding mineral and carbonate content. Induced inflammation lowers the mineral/matrix ratio and increases the overall carbonate accumulation. Elevated concentrations of labile species were detected in osteoporotic samples, especially in the trabecular sections. Collagen cross-linking patterns were indirectly observed through the 1660/1690 cm −1 ratio in the amide I band and a positive correlation was found with the mineralization index. Principal component analysis (PCA) applied to female samples successfully clustered trabecular and osteoporotic cases. The important role played by the phosphate ions was confirmed by corresponding loadings plots. The results suggest that the application of the IMO model to rabbit bones effectively alters bone remodeling and forms an osteoporotic bone matrix with a dissimilar composition compared to the normal one.

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Section: Band Analysis and Quantificationsupporting

confidence: 84%

Infrared spectroscopic assessment of the inflammation-mediated osteoporosis (IMO) model applied to rabbit bone

2012

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“…While both NMR and magnetic resonance imaging (MRI) have been used to characterize bone in a number of studies [40,45,[48][49][50][51][52][53][54][55][56], the present work is the first to quantify water distribution in bone for two age groups. A previous study had actually characterized water distribution in dentin samples from a 20 year, 35 year, and 50 year old donor [50].…”

Section: Discussionmentioning

confidence: 99%

“…The 18 male donors had no known bone disease. Based on donor age, the femurs were divided into two groups: middle aged included 8 ages of 47,49,49,51,55,57,59, and 59 years, while the elderly included 10 ages of 67, 69, 76, 76, 77, 77, 79, 79, 81, and 87 years. Cut from the medial quadrant of each mid-diaphysis, a longitudinal strip of bone was machined, while maintaining hydration, into a standard paralellelepiped specimen such that the osteons ran in the direction of the long axis.…”

Section: Specimen Preparationmentioning

confidence: 99%

Measurements of mobile and bound water by nuclear magnetic resonance correlate with mechanical properties of bone

Nyman

Nicolella

et al. 2008

Bone

179

189

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Since clinical measures of bone mineral density do not necessarily predict whether a person will fracture a bone without an intervention, there is a need to find supplementary tools for assessing bone quality. Presently, we hypothesized that measures of mobile and bound water by a Nuclear Magnetic Resonance (NMR) technique are correlated with bone strength and toughness, respectively. To test this, bending specimens from the mid-diaphysis of 18 human femurs were collected from 18 male donors and divided into middle aged and elderly groups. After NMR measurements of each hydrated specimen, an inversion technique was used to convert the free induction decay data into a distribution of spin-spin (T2) relaxation rates. Then, the distribution resolved into three distinct components that likely represent solid hydrogen, water bound to bone tissue, and mobile water that occupy microscopic pores within the bone specimen. The integrated signal intensities of the bound and mobile components were normalized by the wet mass of the specimen. Following NMR measurements, three point bending tests were conducted to determine the modulus of elasticity, flexure strength, and work to fracture of each specimen. Next, the porosity, mineral-to-collagen ratio, and pentosidine concentration were measured. In this sample of human cortical bone, there was no age-related difference in the amount of mobile water, but the decrease in the amount of bound water with increasing age was statistically significant. Moreover, bound water was associated with both strength and work to fracture of bone, while mobile water was correlated with modulus of elasticity and appeared to quantify the level of microscopic pores within bone. On the other hand, bound water was correlated with the concentration of non-enzymatic collagen crosslinks. The results of this study indicate that quantifying mobile and bound water with magnetic resonance techniques could potentially serve as indicators of bone quality.

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“…The currently accepted model of bone mineral is ∼50-to 150-nmthick stacks of very closely packed apatitic platelets, each of order 2.5-4 nm in thickness (1)(2)(3)(4), arranged so that their large (100) faces are parallel to each other and their c axes are strongly ordered (parallel to collagen fibrils) (5). NMR studies show that, in addition to the largely ordered but nonstoichiometric apatitic phase, there is a substantial, highly hydrated, disordered phase containing up to 55% of the bone mineral phosphatic ions (6,7) but in the form of hydrogen phosphate or phosphate strongly hydrogen-bonded to water rather than apatitic orthophosphate (8). This phase has been assigned as a surface phase, but whether the surface in question is that of individual mineral platelets or the surface of the overall structure formed by a stack of such platelets is not yet clear.…”

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confidence: 99%

Citrate bridges between mineral platelets in bone

Davies

Müller

Wong

et al. 2014

Proc. Natl. Acad. Sci. U.S.A.

244

246

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We provide evidence that citrate anions bridge between mineral platelets in bone and hypothesize that their presence acts to maintain separate platelets with disordered regions between them rather than gradual transformations into larger, more ordered blocks of mineral. To assess this hypothesis, we take as a model for a citrate bridging between layers of calcium phosphate mineral a double salt octacalcium phosphate citrate (OCPcitrate). We use a combination of multinuclear solid-state NMR spectroscopy, powder X-ray diffraction, and first principles electronic structure calculations to propose a quantitative structure for this material, in which citrate anions reside in a hydrated layer, bridging between apatitic layers. To assess the relevance of such a structure in native bone mineral, we present for the first time, to our knowledge, 17 O NMR data on bone and compare them with 17 O NMR data for OCP-citrate and other calcium phosphate minerals relevant to bone. The proposed structural model that we deduce from this work for bone mineral is a layered structure with thin apatitic platelets sandwiched between OCP-citrate-like hydrated layers. Such a structure can explain a number of known structural features of bone mineral: the thin, plate-like morphology of mature bone mineral crystals, the presence of significant quantities of strongly bound water molecules, and the relatively high concentration of hydrogen phosphate as well as the maintenance of a disordered region between mineral platelets.NMR crystallography | biomineralization B one is a complex organic-inorganic composite material (1), in which calcium phosphate nanoparticles are held within a primarily collagen protein matrix. The mineral component is a poorly crystalline phase, closely related to hydroxyapatite. The currently accepted model of bone mineral is ∼50-to 150-nmthick stacks of very closely packed apatitic platelets, each of order 2.5-4 nm in thickness (1-4), arranged so that their large (100) faces are parallel to each other and their c axes are strongly ordered (parallel to collagen fibrils) (5). NMR studies show that, in addition to the largely ordered but nonstoichiometric apatitic phase, there is a substantial, highly hydrated, disordered phase containing up to 55% of the bone mineral phosphatic ions (6, 7) but in the form of hydrogen phosphate or phosphate strongly hydrogen-bonded to water rather than apatitic orthophosphate (8). This phase has been assigned as a surface phase, but whether the surface in question is that of individual mineral platelets or the surface of the overall structure formed by a stack of such platelets is not yet clear. There is, however, significant experimental evidence that is not explained by this model as it stands. First, there has never been any observation of an isolated mineral platelet in mature bone, even in preparations in which there have been attempts to disperse the mineral structures (9). This feature suggests that the mineral platelets are not independent structures-indeed, their ordered aggregati...

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Nuclear Magnetic Resonance Spin-Spin Relaxation of the Crystals of Bone, Dental Enamel, and Synthetic Hydroxyapatites

Cited by 126 publications

References 30 publications

Infrared spectroscopic assessment of the inflammation-mediated osteoporosis (IMO) model applied to rabbit bone

Infrared spectroscopic assessment of the inflammation-mediated osteoporosis (IMO) model applied to rabbit bone

Measurements of mobile and bound water by nuclear magnetic resonance correlate with mechanical properties of bone

Citrate bridges between mineral platelets in bone

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