Validated Approaches for Quantification of Bone Mineral Crystallinity Using Transmission Fourier Transform Infrared (FT-IR), Attenuated Total Reflection (ATR) FT-IR, and Raman Spectroscopy

Querido, William; Ailavajhala, Ramyasri; Padalkar, Mugdha V.; Pleshko, Nancy

doi:10.1177/0003702818789165

Cited by 40 publications

(31 citation statements)

References 59 publications

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“…The raw samples exhibited broad peaks, and after calcination, their width decreases. Figure shows that raw samples are constituted by ordered crystals; consequently, their peak widths are the result of elastic and inelastic diffraction contributions and are not due to a low crystalline quality (order) as have been previously pointed out . It is clear that if the raw crystals are nanometric and ordered, these have to influence the vibrational states of the IR and Raman spectra.…”

Section: Resultssupporting

confidence: 55%

“…Figure 1 shows that raw samples are constituted by ordered crystals; consequently, their peak widths are the result of elastic and inelastic diffraction contributions and are not due to a low crystalline quality (order) as have been previously pointed out. [18,25,26] It is clear that if the raw crystals are nanometric and ordered, these have to influence the vibrational states of the IR and Raman spectra. Figure 4a-d shows the IR bands located between 400 to 4,000 cm −1 for raw and calcinated samples and Sigma-Aldrich.…”

Section: Sem Analysismentioning

confidence: 99%

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Effect of the crystal size on the infrared and Raman spectra of bio hydroxyapatite of human, bovine, and porcine bones

Londoño‐Restrepo

Zubieta‐Otero

Jeronimo‐Cruz

et al. 2019

J Raman Spectroscopy

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The optical properties of hydroxyapatites (HAps) and bio HAps have been studied using Raman and infrared (IR) spectroscopies to describe their crystalline quality. However, the size of the HAp crystals and their crystalline order effects have not been considered yet. This paper focuses on the study of the effect of the change in the crystallites size have on the width of the IR and Raman spectra for defatted and deproteinized bones as well as incinerated biogenic HAp obtained from bovine, porcine, and human bones. Bone samples were analyzed through Raman and IR spectroscopies, X‐ray diffraction (XRD), transmission electron microscopy (TEM), inductively coupled plasma (ICP), and scanning electron microscopy (SEM). The Raman and IR spectra for raw samples showed broad bands but, after calcination at 720 °C, became narrow and well defined. TEM images showed that all raw crystallites are ordered nanoplates contrary to the so far well‐established concept that biogenic HAps have low crystalline quality. XRD data confirmed that raw samples display broad peaks that correlated with the HRTEM images of ordered nanocrystals. This fact confirmed that the broad Raman and IR bands of raw clean bones come from nanocrystal plates. SEM analysis confirmed the increase in the crystal size after calcination from nanomicron to submicron dimensions due to a coalescence phenomenon. These results imply that the interpretation of Raman and IR spectra in the case of HAp nanoparticles has been erroneous. These results contribute to the design of biomaterials for tissue engineering based on biogenic HAp for bone regeneration.

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Section: Resultssupporting

confidence: 55%

Section: Sem Analysismentioning

confidence: 99%

Effect of the crystal size on the infrared and Raman spectra of bio hydroxyapatite of human, bovine, and porcine bones

Londoño‐Restrepo

Zubieta‐Otero

Jeronimo‐Cruz

et al. 2019

J Raman Spectroscopy

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“…The strength of bone is governed not only by the mineral content, but is also influenced by the degree of mineral crystallinity [37,38]. The ν 2 PO 4 3− /amide III ratio is the most reliable determinant of the mineral-to-matrix ratio [39], while mineral crystallinity can be estimated from both the position and the width of the ν 1 PO 4 3− peak [40]. In synthetic carbonated apatites, an inverse relationship exists between the carbonate content and mineral crystallinity (i.e.…”

Section: Discussionmentioning

confidence: 99%

Does Smoking Impair Bone Regeneration in the Dental Alveolar Socket?

et al. 2019

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Smoking is a major risk factor for dental implant failure. In addition to higher marginal bone loss around implants, the cellular and molecular responses to injury and implant physicochemical properties are also differentially affected in smokers. The purpose of this work is to determine if smoking impairs bone microstructure and extracellular matrix composition within the dental alveolar socket after tooth extraction. Alveolar bone biopsies obtained from Smokers (> 10 cigarettes per day for at least 10 years) and Ctrl (never-smokers), 7-146 months after tooth extraction, were investigated using X-ray micro-computed tomography, backscattered electron scanning electron microscopy, and Raman spectroscopy. Both Smokers and Ctrl exhibited high inter-and intra-individual heterogeneity in bone microstructure, which varied between dense cortical and porous trabecular architecture. Regions of disorganised/woven bone were more prevalent during early healing. Remodelled lamellar bone was predominant at longer healing periods. Bone mineral density, bone surface-to-volume ratio, mineral crystallinity, the carbonate-to-phosphate ratio, the mineral-to-matrix ratio, the collagen crosslink ratio, and the amounts of amino acids phenylalanine and proline/hydroxyproline were also comparable between Smokers and Ctrl. Bone microstructure and composition within the healing dental alveolar socket are not significantly affected by moderate-to-heavy smoking.

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“…This includes studying changes in chemistry or crystallinity associated with bone mineralization disorders; see Boskey (2002) for a short review. However, these techniques also produce complimentary information about structural ordering within the crystallites (Querido et al, 2018;Londoñ o-Restrepo et al, 2019), as vibrational spectroscopy is sensitive to short-range order (Wopenka & Pasteris, 2005), whereas XRD can be used to examine changes in long-range order (Bazin et al, 2009). Whilst vibrational spectroscopy can be conducted on cross-sectioned bone samples, XRD analysis is typically conducted in powder form, resulting in a loss of spatial information.…”

Section: Introductionmentioning

confidence: 99%

Correlative vibrational spectroscopy and 2D X-ray diffraction to probe the mineralization of bone in phosphate-deficient mice

Tommasini

Rodríguez‐Navarro

et al. 2019

J Appl Cryst

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Bone crystallite chemistry and structure change during bone maturation. However, these properties of bone can also be affected by limited uptake of the chemical constituents of the mineral by the animal. This makes probing the effect of bone-mineralization-related diseases a complicated task. Here it is shown that the combination of vibrational spectroscopy with two-dimensional X-ray diffraction can provide unparalleled information on the changes in bone chemistry and structure associated with different bone pathologies (phosphate deficiency) and/or health conditions (pregnancy, lactation). Using a synergistic analytical approach, it was possible to trace the effect that changes in the remodelling regime have on the bone mineral chemistry and structure in normal and mineral-deficient (hypophosphatemic) mice. The results indicate that hypophosphatemic mice have increased bone remodelling, increased carbonate content and decreased crystallinity of the bone mineral, as well as increased misalignment of crystallites within the bone tissue. Pregnant and lactating mice that are normal and hypophosphatemic showed changes in the chemistry and misalignment of the apatite crystals that can be related to changes in remodelling rates associated with different calcium demand during pregnancy and lactation.

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Validated Approaches for Quantification of Bone Mineral Crystallinity Using Transmission Fourier Transform Infrared (FT-IR), Attenuated Total Reflection (ATR) FT-IR, and Raman Spectroscopy

Cited by 40 publications

References 59 publications

Effect of the crystal size on the infrared and Raman spectra of bio hydroxyapatite of human, bovine, and porcine bones

Effect of the crystal size on the infrared and Raman spectra of bio hydroxyapatite of human, bovine, and porcine bones

Does Smoking Impair Bone Regeneration in the Dental Alveolar Socket?

Correlative vibrational spectroscopy and 2D X-ray diffraction to probe the mineralization of bone in phosphate-deficient mice

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