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      Understanding sterol-membrane interactions, part II: complete 1H and 13C assignments by solid-state NMR spectroscopy and determination of the hydrogen-bonding partners of cholesterol in a lipid bilayer.

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          Abstract

          The complete assignment of cholesterol 1H and 13C NMR resonances in a lipid bilayer environment (Lalpha-dimyristoylphosphatidylcholine/cholesterol 2:1) has been obtained by a combination of 1D and 2D MAS NMR experiments: 13C spectral editing, ge-HSQC, dipolar HETCOR and J-based HETCOR. Specific chemical shift variations have been observed for the C1-C6 atoms of cholesterol measured in CCl4 solution and in the membrane. Based on previous work (F. Jolibois, O. Soubias, V. Reat, A. Milon, Chem. Eur. J. 2004, 10, preceding paper in this issue: DOI: 10.1002/chem.200400245) these variations were attributed to local changes around the cholesterol hydroxy group, such as the three major rotameric states of the C3-O3 bond and different hydrogen bonding partners (water molecules, carboxy and phosphodiester groups of phosphatidylcholine). Comparison of the experimental and theoretical chemical shifts obtained from quantum-chemistry calculations of various transient molecular complexes has allowed the distributions of hydrogen bonding partners and hydroxy rotameric states to be determined. This is the first time that the probability of hydrogen bonding occurring between cholesterol's hydroxy group and phosphatidylcholine's phosphodiester has been determined experimentally.

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          Author and article information

          Journal
          Chemistry
          Chemistry (Weinheim an der Bergstrasse, Germany)
          Wiley
          0947-6539
          0947-6539
          Nov 19 2004
          : 10
          : 23
          Affiliations
          [1 ] Institut de Pharmacologie et de Biologie Structurale, CNRS and University P. Sabatier, 205 rte de Narbonne, Toulouse, France.
          Article
          10.1002/chem.200400246
          15497136
          7b8a8cb6-0e91-44dc-9399-6bc640ad26f3
          History

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