Heteronuclear chemical shift correlation and J-resolved MAS NMR spectroscopy of lipid membranes

Vadim Zorin; Filip Ciesielski; David C. Griffin; Michael Rittig; Boyan B. Bonev

doi:10.1002/mrc.2690

Heteronuclear chemical shift correlation and J-resolved MAS NMR spectroscopy of lipid membranes

Vadim Zorin, Filip Ciesielski, David C. Griffin, Michael Rittig, Boyan B. Bonev

Research output: Journal Publication › Article › peer-review

12 Citations (Scopus)

Abstract

Direct observation of J-couplings remains a challenge in high-resolution solid-state NMR. In some cases, it is possible to use Lee-Goldburg (LG) homonuclear decoupling during rare spin observation in MAS NMR correlation spectroscopy of lipid membranes to obtain J-resolved spectra in the direct dimension. In one simple implementation, a wide line separation-type ¹³C-¹H HETCOR can provide high-resolution ¹H/¹³C spectra, which are J-resolved in both dimensions. Coupling constants, ¹J_HC, obtained from ¹H doublets, can be compared with scaled ¹J_CH-values obtained from the ¹³C multiplets to assess the LG efficiency and scaling factor. The use of homonuclear decoupling during proton evolution, LG-HETCOR-LG, can provide J-values, at least in the rare spin dimension, and allows measurements in less mobile membrane environments. The LG-decoupled spectroscopic approach is demonstrated on pure dioleoylphosphatidylcholine (DOPC) membranes and used to investigate lipid mixtures of DOPC/cholesterol and DOPC/cholesterol/sphingomyelin.

Original language	English
Pages (from-to)	925-934
Number of pages	10
Journal	Magnetic Resonance in Chemistry
Volume	48
Issue number	12
DOIs	https://doi.org/10.1002/mrc.2690
Publication status	Published - Dec 2010
Externally published	Yes

Keywords

HETCOR
J-coupling
Lee-Goldburg decoupling
high-resolution MAS
lipid membrane
solid-state NMR

ASJC Scopus subject areas

General Chemistry
General Materials Science

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10.1002/mrc.2690

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title = "Heteronuclear chemical shift correlation and J-resolved MAS NMR spectroscopy of lipid membranes",

abstract = "Direct observation of J-couplings remains a challenge in high-resolution solid-state NMR. In some cases, it is possible to use Lee-Goldburg (LG) homonuclear decoupling during rare spin observation in MAS NMR correlation spectroscopy of lipid membranes to obtain J-resolved spectra in the direct dimension. In one simple implementation, a wide line separation-type 13C-1H HETCOR can provide high-resolution 1H/13C spectra, which are J-resolved in both dimensions. Coupling constants, 1JHC, obtained from 1H doublets, can be compared with scaled 1JCH-values obtained from the 13C multiplets to assess the LG efficiency and scaling factor. The use of homonuclear decoupling during proton evolution, LG-HETCOR-LG, can provide J-values, at least in the rare spin dimension, and allows measurements in less mobile membrane environments. The LG-decoupled spectroscopic approach is demonstrated on pure dioleoylphosphatidylcholine (DOPC) membranes and used to investigate lipid mixtures of DOPC/cholesterol and DOPC/cholesterol/sphingomyelin.",

keywords = "HETCOR, J-coupling, Lee-Goldburg decoupling, high-resolution MAS, lipid membrane, solid-state NMR",

author = "Vadim Zorin and Filip Ciesielski and Griffin, {David C.} and Michael Rittig and Bonev, {Boyan B.}",

year = "2010",

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doi = "10.1002/mrc.2690",

language = "English",

volume = "48",

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T1 - Heteronuclear chemical shift correlation and J-resolved MAS NMR spectroscopy of lipid membranes

AU - Zorin, Vadim

AU - Ciesielski, Filip

AU - Griffin, David C.

AU - Rittig, Michael

AU - Bonev, Boyan B.

PY - 2010/12

Y1 - 2010/12

N2 - Direct observation of J-couplings remains a challenge in high-resolution solid-state NMR. In some cases, it is possible to use Lee-Goldburg (LG) homonuclear decoupling during rare spin observation in MAS NMR correlation spectroscopy of lipid membranes to obtain J-resolved spectra in the direct dimension. In one simple implementation, a wide line separation-type 13C-1H HETCOR can provide high-resolution 1H/13C spectra, which are J-resolved in both dimensions. Coupling constants, 1JHC, obtained from 1H doublets, can be compared with scaled 1JCH-values obtained from the 13C multiplets to assess the LG efficiency and scaling factor. The use of homonuclear decoupling during proton evolution, LG-HETCOR-LG, can provide J-values, at least in the rare spin dimension, and allows measurements in less mobile membrane environments. The LG-decoupled spectroscopic approach is demonstrated on pure dioleoylphosphatidylcholine (DOPC) membranes and used to investigate lipid mixtures of DOPC/cholesterol and DOPC/cholesterol/sphingomyelin.

AB - Direct observation of J-couplings remains a challenge in high-resolution solid-state NMR. In some cases, it is possible to use Lee-Goldburg (LG) homonuclear decoupling during rare spin observation in MAS NMR correlation spectroscopy of lipid membranes to obtain J-resolved spectra in the direct dimension. In one simple implementation, a wide line separation-type 13C-1H HETCOR can provide high-resolution 1H/13C spectra, which are J-resolved in both dimensions. Coupling constants, 1JHC, obtained from 1H doublets, can be compared with scaled 1JCH-values obtained from the 13C multiplets to assess the LG efficiency and scaling factor. The use of homonuclear decoupling during proton evolution, LG-HETCOR-LG, can provide J-values, at least in the rare spin dimension, and allows measurements in less mobile membrane environments. The LG-decoupled spectroscopic approach is demonstrated on pure dioleoylphosphatidylcholine (DOPC) membranes and used to investigate lipid mixtures of DOPC/cholesterol and DOPC/cholesterol/sphingomyelin.

KW - HETCOR

KW - J-coupling

KW - Lee-Goldburg decoupling

KW - high-resolution MAS

KW - lipid membrane

KW - solid-state NMR

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AN - SCOPUS:78649282749

SN - 0749-1581

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JO - Magnetic Resonance in Chemistry

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ER -

Heteronuclear chemical shift correlation and J-resolved MAS NMR spectroscopy of lipid membranes

Abstract

Keywords

ASJC Scopus subject areas

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