Through-Bond Heteronuclear Single-Quantum Correlation Spectroscopy in Solid-State NMR, and Comparison to Other Through-Bond and Through-Space Experiments

Lesage, Anne; Emsley, Lyndon

doi:10.1006/jmre.2000.2249

Cited by 96 publications

(81 citation statements)

References 23 publications

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“…[37][38][39][40] The transfer through J coupling provides well resolved and selective chemical-shift correlation between directly bound proton-carbon pairs, provided that the coherences involved decay more slowly than the delay required for efficient polarization transfer. [41,42] For the particular case of sterols in membranes, we have recently used the gain in sensitivity brought about by inverse detection to detect all the expected one-bond cross peaks of natural abundance cholesterol in a DMPC/cholesterol lipid mixture. [43] However, fast relaxation processes have so far prevented long-range J-couplingbased experiments and the observation of multiple-bond connectivity.…”

Section: Resultsmentioning

confidence: 99%

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

Soubias

Jolibois

Réat

et al. 2004

Chemistry A European J

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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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Section: Resultsmentioning

confidence: 99%

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

Soubias

Jolibois

Réat

et al. 2004

Chemistry A European J

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“…Thus, even when identifying throughbond connectivities used for assignment studies it is the nearest neighbor dipolar interactions which are exploited in preference to the J-couplings. A range of polarization transfer methods which exploit J-couplings have been developed (49)(50)(51), and their application may be useful in highly dynamics systems. Examples of polarization transfer methods (both homo-and hetero-nuclear) which are routinely employed to study ligand/receptor interactions are highlighted below.…”

Section: Nmr Methodology Employed For Ligand-binding Studiesmentioning

confidence: 99%

Solid‐state NMR for the analysis of high‐affinity ligand/receptor interactions

Williamson¹

2009

Concepts Magnetic Resonance

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The rational development of drugs which target integral membrane proteins relies intimately on our understanding of their interactions with their binding sites. Advances in solid-state NMR methodology coupled to improved expression and purification strategies for membrane proteins now enable us to probe the structure, dynamics, and binding modes of these drugs with ever-increasing resolution. This article seeks to highlight these advances demonstrating how improvements in protein expression and purification can be coupled with recent developments in instrumentation and pulse sequences in magic-angle spinning, static, and oriented sample solid-state NMR to reveal structural and dynamic information of high-affinity drugs/ligands within their binding sites on membrane proteins. Furthermore, we will highlight some of the major experimental considerations associated with performing these studies.

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“…MAS-J-HMQC, [166] MAS-J-HSQC [167] and refocused INEPT [168] enable the high-resolution determination of the 1 H chemical shifts of hydrogen atoms directly bonded to carbons, with applications at natural abundance in 13 C including a tripeptide, [169] celluloses, [157,158] maltose anomers [52] and a penicillin G K þ salt. [170] As an example, Figure 11b presents a 13 C-1 H MAS-J-HMQC (recorded in 34 h experimental time at 7.0 T) spectrum of tunicate cellulose at natural abundance.…”

Section: Identification Of Through-bond Connectivitiesmentioning

confidence: 99%

Recent Advances in Solid‐State MAS NMR Methodology for Probing Structure and Dynamics in Polymeric and Supramolecular Systems

Brown

2009

Macromol. Rapid Commun.

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This article reviews recent applications of novel (1) H, (2) H, (13) C, (15) N and (17) O solid-state MAS NMR methods that provide new insight into the structural and dynamic processes that determine the bulk properties of polymeric and supramolecular materials. The review highlights methods that exploit the sensitivity to structure and dynamics of the NMR chemical shift and quadrupolar coupling as well as the through-space dipolar coupling and through-bond J coupling. In particular, it is shown that solid-state NMR exhibits marked sensitivity to key intra- and intermolecular hydrogen-bonding and π-π interactions, allowing, for example, the very accurate determination of internuclear distances as well as the probing of dynamics over a very wide range of timescales.

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Through-Bond Heteronuclear Single-Quantum Correlation Spectroscopy in Solid-State NMR, and Comparison to Other Through-Bond and Through-Space Experiments

Cited by 96 publications

References 23 publications

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

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

Solid‐state NMR for the analysis of high‐affinity ligand/receptor interactions

Recent Advances in Solid‐State MAS NMR Methodology for Probing Structure and Dynamics in Polymeric and Supramolecular Systems

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Through-Bond Heteronuclear Single-Quantum Correlation Spectroscopy in Solid-State NMR, and Comparison to Other Through-Bond and Through-Space Experiments

Cited by 96 publications

References 23 publications

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

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

Solid‐state NMR for the analysis of high‐affinity ligand/receptor interactions

Recent Advances in Solid‐State MAS NMR Methodology for Probing Structure and Dynamics in Polymeric and Supramolecular Systems

Contact Info

Product

Resources

About

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

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