1H MAS and 1H → 31P CP/MAS NMR study of human bone mineral
1H MAS and 1H → 31P CP/MAS NMR study of human bone mineral
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DOI：
10.1007/s00223-002-2111-5
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发表时间：
2003-11-01
影响因子：
4.2
通讯作者：
Kolodziejski, W
中科院分区：
文献类型：
--
作者：
Kaflak-Hachulska, A;Samoson, A;Kolodziejski, W
采用魔角旋转（MAS）固态核磁共振（NMR）技术研究了人骨矿物的化学结构。将成年受试者的骨小梁和骨皮质样本与矿物标准进行比较：羟基磷灰石（HA），水化和煅烧，B型碳酸磷灰石（ca -B）， CO32- (CHA-B)的9，Wt%，刷石（BRU）和HA与BRU的混合物。质子光谱以40 kHz的超高速MAS提供的优异光谱分辨率获得。在12 kHZ的快速MAS下，通过交叉极化（CP）实现了二维H-1-P-31核磁共振异核相关。P-31核磁共振与质子在1 kHz慢速MAS下的CP应用。分析了P-31旋转边带的形貌及其CP动力学。结果表明，CP谱的边带特别适合于磷灰石晶体表面状态的监测。骨样本似乎缺乏类似于HA的结构羟基。我们没有发现HPO42类刷状离子存在于骨矿物中的直接证据。后一个问题在文献中被广泛讨论。研究证明CHA-B与骨矿物质具有相似的核磁共振行为。
Chemical structure of human bone mineral Was studied by solid-state nuclear magnetic resonance (NMR) with magic-angle spinning (MAS). Trabecular and cortical bone samples from adult subjects were compared with mineral standards: hydroxyapatite (HA), hydrated and calcined, carbonatoapatite of type B with 9, Wt% of CO32- (CHA-B), brushite (BRU) and mixtures of HA with BRU. Proton spectra were acquired with excellent spectral resolution provided by ultra-high speed MAS at 40 kHz. 2D H-1-P-31 NMR heteronuclear correlation was achieved by cross-polarization (CP) under fast MAS at 12 kHZ. P-31 NMR was applied with CP from protons under slow MAS at 1 kHz. Appearance of P-31 rotational sidebands together with their CP kinetics were analyzed. It was suggested that the sidebands of CP spectra are particularly suitable for monitoring the state of apatite crystal surfaces. The bone samples appeared to be deficient in structural hydroxyl groups analogous to those in HA. We found no direct evidence that the HPO42 brushite-like ions are present in bone mineral. The latter problem is extensively discussed in the literature. The study proves there is a similarity between CHA-B and bone mineral expressed by their similar NMR behavior.