Solid state NMR - An indispensable tool in organic-inorganic biocomposite characterization; refining the structure of octacalcium phosphate composites with the linear metabolic di-acids succinate and adipate

Solid State Nuclear Magnetic Resonance
Yang LiJerry C C Chan

Abstract

Octacalcium phosphate (OCP; Ca8(HPO4)2(PO4)4. 5H2O) is a plausible precursor phase of biological hydroxyapatite, which composites with a number of biologically relevant organic metabolites. Widely used material science physicochemical structure determination techniques successfully characterize the mineral component of these composites but leave details of the structure, and interactions with mineral, of the organic component almost completely obscure. The metabolic linear di-acids succinate (SUC) and adipate (ADI) differentially expand the hydrated (100) layer of OCP. 13C13C correlation (proton driven spin diffusion, PDSD) experiments on OCP composited with (U-13C4)-SUC, and (U13C6)-ADI, show that the two di-acids per unit cell adopt non-centrosymmetric but mutually identical structures. 13C{31P}, rotational echo double resonance (REDOR) shows that one end of each linear di-acid is displaced further from the surface of the apatitic OCP layer relative to the other end. Overall the results indicate two di-acids per unit cell disposed perpendicularly across the OCP hydrated layer with one carboxylate of each di-acid substituting a hydrated surface OCP phosphate group. This study re-affirms the unique advantages of ssNMR in elucid...Continue Reading

Citations

Apr 2, 2021·Journal of Colloid and Interface Science·Rita GelliPiero Baglioni
Mar 18, 2021·Magnetic Resonance in Chemistry : MRC·Danielle LaurencinChristian Bonhomme
Apr 24, 2020·Solid State Nuclear Magnetic Resonance·Christel GervaisDanielle Laurencin

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Methods Mentioned

BETA
NMR
X-ray

Software Mentioned

REDOR
ssNMR

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