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Pure and Applied Chemistry

The Scientific Journal of IUPAC

Ed. by Burrows, Hugh / Stohner, Jürgen


IMPACT FACTOR 2017: 5.294

CiteScore 2017: 3.42

SCImago Journal Rank (SJR) 2017: 1.212
Source Normalized Impact per Paper (SNIP) 2017: 1.546

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1365-3075
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Volume 81, Issue 8

Issues

Solid-state NMR characterization of drug-model molecules encapsulated in MCM-41 silica

Thierry Azaïs
  • Corresponding author
  • Université Pierre et Marie Curie-Paris6 and CNRS, UMR 7574, Laboratoire Chimie de la Matière Condensée de Paris, Paris, F-75005, France
  • Other articles by this author:
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/ Geoffrey Hartmeyer
  • Corresponding author
  • Université Pierre et Marie Curie-Paris6 and CNRS, UMR 7574, Laboratoire Chimie de la Matière Condensée de Paris, Paris, F-75005, France
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/ Sandrine Quignard
  • Corresponding author
  • Université Pierre et Marie Curie-Paris6 and CNRS, UMR 7574, Laboratoire Chimie de la Matière Condensée de Paris, Paris, F-75005, France
  • Other articles by this author:
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/ Guillaume Laurent
  • Corresponding author
  • Université Pierre et Marie Curie-Paris6 and CNRS, UMR 7574, Laboratoire Chimie de la Matière Condensée de Paris, Paris, F-75005, France
  • Other articles by this author:
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/ Corine Tourné-Péteilh
  • Corresponding author
  • UMR 5253 CNRS/ENSCM/UM2/UM1, Institut Charles Gerhardt Montpellier, 8 rue de l'Ecole Normale, 34296 Montpellier Cedex 5, France
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/ Jean-Marie Devoisselle
  • Corresponding author
  • UMR 5253 CNRS/ENSCM/UM2/UM1, Institut Charles Gerhardt Montpellier, 8 rue de l'Ecole Normale, 34296 Montpellier Cedex 5, France
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/ Florence Babonneau
  • Corresponding author
  • Université Pierre et Marie Curie-Paris6 and CNRS, UMR 7574, Laboratoire Chimie de la Matière Condensée de Paris, Paris, F-75005, France
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Published Online: 2009-07-19 | DOI: https://doi.org/10.1351/PAC-CON-08-11-10

In this contribution, we present a solid-state NMR approach to characterize drug-model molecules as ibuprofen, benzoic acid and lauric acid, encapsulated in MCM-41 silica and submitted to strong confinement effects. In particular, we show that by a careful choice of the solid-state NMR sequences, it is possible to efficiently characterize these highly mobile molecules and their interactions with the pore surface. Thus, we demonstrate that 13C NMR spectroscopy is a powerful tool to characterize and even quantify entrapped and non-entrapped species by using either single-pulse excitation (SPE) or cross-polarization (CP). Whereas the standard {1H}-13C CP experiment is of poor efficiency for mobile species, we show that 13C signal-to-noise (S/N) ratio can be significantly improved through 1H-13C cross-relaxation (namely, nuclear Overhauser effect, nOe) by using a 1H power-gated technique. The long transversal relaxation times [T2(1H) up to 22 ms] observed allow the set-up of J-coupling based experiments such as 2D {1H}-13C heteronuclear multiple-quantum coherence (HMQC) in order to fully characterize the encapsulated molecules. Thus, we demonstrate that the use of sequences derived from solution-state NMR such as these two latter experiments is highly efficient to characterize highly mobile organic molecules trapped in mesopores. Finally, we show that 1H spin diffusion-based experiments can give useful informations on the proximities between trapped molecules and the silica surface.

Keywords: confinement; drug delivery; encapsulation; porous silica; solid-state NMR

Conference

Conference on Solid State Chemistry, Conference on Solid State Chemistry , SSC, Solid State Chemistry , 8th, Bratislava, Slovakia, 2008-07-06–2008-07-11

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About the article

Published Online: 2009-07-19

Published in Print: 2009-07-19


Citation Information: Pure and Applied Chemistry, Volume 81, Issue 8, Pages 1345–1355, ISSN (Online) 1365-3075, ISSN (Print) 0033-4545, DOI: https://doi.org/10.1351/PAC-CON-08-11-10.

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