High-resolution J-coupled 13C MAS NMR spectroscopy of lipid membranes

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

doi:10.1016/j.chemphyslip.2009.07.001

Cited by 12 publications

(35 citation statements)

References 55 publications

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“…The HETCOR-LG approach with undecoupled evolution is applicable to membrane systems in the liquid crystalline phase, in which rapid molecular and segmental motions disrupt partially the inter-proton and carbon-proton dipolar couplings and allow LG decoupling to reveal multiplet structures. [13] Similar effects are observed in adamantane, in which molecular mobility within the crystal leads to partial self-decoupling, [31,38] as well as in lipids at higher MAS speeds. [14] We report results from HETCOR-LG studies of hydrated bilayers including pure dioleoylphosphatidylcholine (DOPC) and mixed bilayers consisting of DOPC/cholesterol and DOPC/cholesterol/sphingomyelin.…”

Section: Introductionsupporting

confidence: 62%

“…2) were investigated by WISE-type heteronuclear 13 C-1 H correlation spectroscopy [37] to obtain highresolution 13 C and 1 H chemical shift-resolved spectra ( Fig. 3(A)).…”

Section: Dopc: Wise Spectroscopymentioning

confidence: 99%

“…Natural abundance 13 C DOPC (1,2-dioleoyl-sn-glycero-3-phosphatidylcholine) sphingomyelin was purchased from Avanti Polar Lipids (Alabaster, AL, USA) and cholesterol was purchased from Sigma (Poole, Dorset, UK); all lipids were used as obtained, without further purification. Pure lipid was suspended in distilled water and mixed vigorously for 15 min at 45…”

Section: Sample Preparationmentioning

confidence: 99%

“…[23 -25] The effects of cholesterol on membrane lipids have been investigated by NOESY-MAS. [15] Chemical shift-correlated spectra from sterol-containing membranes have been obtained using refocused wide line separation (WISE)-type experiments with or without MREV-8 homonuclear decoupling during evolution, followed by CP or INEPT transfer to 13 C. [26,27] Under free evolution, Hong et al [28,29] have observed WISE-type heteronuclear chemical shift correlation spectra, which show J-resolved proton doublets.…”

Section: Introductionmentioning

confidence: 98%

“…Here, we use LG decoupling during acquisition to obtain 2D high-resolution J-resolved 13 C MAS NMR spectra from fluid bilayer membranes. A simple 2D WISE-type CP-MAS HETCOR experiment [37] allows simultaneous observation of unscaled 1 J HCcouplings and off-resonance magic angle nutation-scaled 1 J θ CH multiplets (Fig.…”

Section: Introductionmentioning

confidence: 99%

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

Zorin

Ciesielski

Griffin

et al. 2010

Magnetic Reson in Chemistry

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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 (13)C-(1)H HETCOR can provide high-resolution (1)H/(13)C spectra, which are J-resolved in both dimensions. Coupling constants, (1)J(HC), obtained from (1)H doublets, can be compared with scaled (1)J(θ)(CH)-values obtained from the (13)C 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.

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Section: Introductionsupporting

confidence: 62%

“…2) were investigated by WISE-type heteronuclear 13 C-1 H correlation spectroscopy [37] to obtain highresolution 13 C and 1 H chemical shift-resolved spectra ( Fig. 3(A)).…”

Section: Dopc: Wise Spectroscopymentioning

confidence: 99%

Section: Sample Preparationmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 98%

Section: Introductionmentioning

confidence: 99%

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

Zorin

Ciesielski

Griffin

et al. 2010

Magnetic Reson in Chemistry

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Wheat straw, corn stover, sugarcane, and Agave biomasses: chemical properties, availability, and cellulosic‐bioethanol production potential in Mexico

Hernández

Escamilla‐Alvarado

Sánchez

et al. 2019

Biofuels Bioprod Bioref

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Mexico is one of the largest agricultural producers in Latin America and generates a large amount of agricultural residue. The aim of this study was to establish the usefulness of four of the main Mexican crops (corn, wheat, sugarcane, and Agave) as feedstock for lignocellulosic bioethanol production. The lignocellulosic residue ratio (RR), defined as weight of residue (in tons) per ton of product, was measured by sampling crop fields in 11 geographic regions of Mexico. The chemical composition, assessed by Fourier-transform infrared spectroscopy (FTIR) and carbon-13 nuclear magnetic resonance ( 13 C NMR), and structural composition (extractives, cellulose, hemicellulose, and lignin contents), heating value, and metal content of these lignocellulosic residues were measured. Biorefinery locations, and their theoretical bioethanol production, were suggested using the gravity center method and techno-economic criteria. The highest RR (1.1 ton of straw per ton of grain) was obtained for wheat straw followed by corn 1144

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High-Resolution Solid-State NMR of Lipid Membranes

Bonev

2013

A Tribute to Marin D. Mitov

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High-resolution J-coupled 13C MAS NMR spectroscopy of lipid membranes

Cited by 12 publications

References 55 publications

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

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

Wheat straw, corn stover, sugarcane, and Agave biomasses: chemical properties, availability, and cellulosic‐bioethanol production potential in Mexico

High-Resolution Solid-State NMR of Lipid Membranes

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