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research article

Structural description of surfaces and interfaces in biominerals by DNP SENS

Azais, Thierry
•
Von Euw, Stanislas
•
Ajili, Widad
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October 1, 2019
Solid State Nuclear Magnetic Resonance

Biological mineralized tissues are hybrid materials with complex hierarchical architecture composed of biominerals often embedded in an organic matrix. The atomic-scale comprehension of surfaces and organo-mineral interfaces of these biominerals is of paramount importance to understand the ultrastructure, the formation mechanisms as well as the biological functions of the related biomineralized tissue. In this communication we demonstrate the capability of DNP SENS to reveal the fine atomic structure of biominerals, and more specifically their surfaces and interfaces. For this purpose, we studied two key examples belonging to the most significant biominerals family in nature: apatite in bone and aragonite in nacreous shell. As a result, we demonstrate that DNP SENS is a powerful approach for the study of intact biomineralized tissues. Signal enhancement factors are found to be up to 40 and 100, for the organic and the inorganic fractions, respectively, as soon as impregnation time with the radical solution is long enough (between 12 and 24 h) to allow an efficient radical penetration into the calcified tissues. Moreover, ions located at the biomineral surface are readily detected and identified through P-31 or C-13 HETCOR DNP SENS experiments. Noticeably, we show that protonated anions are preponderant at the biomineral surfaces in the form of HPO42- for bone apatite and HCO32- for nacreous aragonite. Finally, we demonstrate that organo-mineral interactions can be probed at the atomic level with high sensitivity. In particular, reliable C-13-{P-31} REDOR experiments are achieved in a few hours, leading to the determination of distances, molar proportion and binding mode of citrate bonded to bone mineral in native compact bone. According to our results, only 80% of the total amount of citrate in bone is directly interacting with bone apatite through two out of three carboxylic groups.

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Type
research article
DOI
10.1016/j.ssnmr.2019.06.001
Web of Science ID

WOS:000480802700002

Author(s)
Azais, Thierry
•
Von Euw, Stanislas
•
Ajili, Widad
•
Auzoux-Bordenave, Stephanie
•
Bertani, Philippe
•
Gajan, David
•
Emsley, Lyndon  
•
Nassif, Nadine
•
Lesage, Anne
Date Issued

2019-10-01

Publisher

ACADEMIC PRESS INC ELSEVIER SCIENCE

Published in
Solid State Nuclear Magnetic Resonance
Volume

102

Start page

2

End page

11

Subjects

Chemistry, Physical

•

Physics, Atomic, Molecular & Chemical

•

Physics, Condensed Matter

•

Spectroscopy

•

Chemistry

•

Physics

•

biomineralization

•

calcified tissues

•

biominerals

•

bone

•

nacre

•

solid state nmr

•

dnp sens

•

dynamic nuclear-polarization

•

state nmr-spectroscopy

•

collagen

•

crystals

•

apatite

•

c-13

•

relaxation

•

mechanisms

•

carbonate

Peer reviewed

REVIEWED

Written at

EPFL

EPFL units
ISIC-GE  
Available on Infoscience
August 29, 2019
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/160699
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