Two-dimensional spin-exchange solid-state NMR studies of 13C-enriched wood

Bardet, Michel; Emsley, Lyndon; Vincendon, M.

doi:10.1016/s0926-2040(96)01273-8

Cited by 73 publications

(62 citation statements)

References 9 publications

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“…The different 13 C signals of wood spectrum have been perfectly identified for more than 20 years ago, their assignments are reported in Table 2 (Bardet et al, 1986(Bardet et al, , 1997Mannu, 2002). On the spectrum D two new signals are assigned to PEG: the intense signal at 72 ppm, noted PEG, is attributed to the carbons in CH 2 O group that composes the bulk of PEG 400 and 4000 and the smaller signal overlapping with the wood signal at 61.7 ppm is assigned to terminal CH 2 bound to an hydroxyl group.…”

Section: Resultsmentioning

confidence: 99%

Study of interactions between polyethylene glycol and archaeological wood components by 13C high-resolution solid-state CP-MAS NMR

Bardet

Gerbaud

Trân

et al. 2007

Journal of Archaeological Science

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Section: Resultsmentioning

confidence: 99%

Study of interactions between polyethylene glycol and archaeological wood components by 13C high-resolution solid-state CP-MAS NMR

Bardet

Gerbaud

Trân

et al. 2007

Journal of Archaeological Science

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“…The full widths at half maximum, the peak heights, and the integrals of the deconvoluted peaks are reported in Supplemental Table S2. 2D 1 H-driven 13 C spin diffusion (PDSD) spectra were measured at 296 K under 13.5-kHz MAS (Meier, 1994;Bardet et al, 1997). Then 1 ms 1 H-13 C CP was used to create the initial 13 C magnetization.…”

Section: Solid-state Nmr Spectroscopymentioning

confidence: 99%

The Target of β-Expansin EXPB1 in Maize Cell Walls from Binding and Solid-State NMR Studies

et al. 2016

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The wall-loosening actions of b-expansins are known primarily from studies of EXPB1 extracted from maize (Zea mays) pollen. EXPB1 selectively loosens cell walls (CWs) of grasses, but its specific binding target is unknown. We characterized EXPB1 binding to sequentially extracted maize CWs, finding that the protein primarily binds glucuronoarabinoxylan (GAX), the major matrix polysaccharide in grass CWs. This binding is strongly reduced by salts, indicating that it is predominantly electrostatic in nature. For direct molecular evidence of EXPB1 binding, we conducted solid-state nuclear magnetic resonance experiments using paramagnetic relaxation enhancement (PRE), which is sensitive to distances between unpaired electrons and nuclei. By mixing 13 C-enriched maize CWs with EXPB1 functionalized with a Mn 2+ tag, we measured Mn 2+ -induced PRE. Strong 1 H and 13 C PREs were observed for the carboxyls of GAX, followed by more moderate PREs for carboxyl groups in homogalacturonan and rhamnogalacturonan-I, indicating that EXPB1 preferentially binds GAX. In contrast, no PRE was observed for cellulose, indicating very weak interaction of EXPB1 with cellulose. Dynamics experiments show that EXPB1 changes GAX mobility in a complex manner: the rigid fraction of GAX became more rigid upon EXPB1 binding while the dynamic fraction became more mobile. Combining these data with previous results, we propose that EXPB1 loosens grass CWs by disrupting noncovalent junctions between highly substituted GAX and GAX of low substitution, which binds cellulose. This study provides molecular evidence of b-expansin's target in grass CWs and demonstrates a new strategy for investigating ligand binding for proteins that are difficult to express heterologously.

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“…The reaction mixture was decanted from the spent catalyst and rotary evaporated to recover the methanol-d 4 and to give a crude yellow liquid. The product was vacuum distilled (with assistance of a microcapillary) to recover 1-methyl-d 3 This exchange is derived from a combination of prior published methods. [27,28] Briefly, dry palladium catalyst (1 g Pd/C) was well stirred for 1 hr in a double-necked flask purged with nitrogen followed by capping one neck of the flask with a 230-mm round balloon full of hydrogen.…”

Section: Synthesis Of 1-methyl-d 3 -Imidazolementioning

confidence: 99%

“…Degradative methods may be applied to the whole cell wall material, but study of individual components typically requires their separation. Improved solid-state NMR has been useful for examining the intact plant cell walls [1][2][3][4] ; however, the decreased relaxation times and low peak dispersion with solid-state NMR limit its use for thorough characterization of intact polymers. As solution-state NMR instrumentation and experiments become more developed, higher sensitivity and resolution permit the detailed structural analysis of cell wall polymeric components more effectively.…”

Section: Introductionmentioning

confidence: 99%

Characterization of nonderivatized plant cell walls using high‐resolution solution‐state NMR spectroscopy

Yelle

Ralph

Frihart

2008

Magnetic Reson in Chemistry

164

179

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A recently described plant cell wall dissolution system has been modified to use perdeuterated solvents to allow direct in-NMR-tube dissolution and high-resolution solution-state NMR of the whole cell wall without derivatization. Finely ground cell wall material dissolves in a solvent system containing dimethylsulfoxide-d 6 and 1-methylimidazole-d 6 in a ratio of 4 : 1 (v/v), keeping wood component structures mainly intact in their near-native state. Two-dimensional NMR experiments, using gradient-HSQC (heteronuclear single quantum coherence) 1-bond 13 C-1 H correlation spectroscopy, on nonderivatized cell wall material from a representative gymnosperm Pinus taeda (loblolly pine), an angiosperm Populus tremuloides (quaking aspen), and a herbaceous plant Hibiscus cannabinus (kenaf) demonstrate the efficacy of the system. We describe a method to synthesize 1-methylimidazole-d 6 with a high degree of perdeuteration, thus allowing cell wall dissolution and NMR characterization of nonderivatized plant cell wall structures.

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Two-dimensional spin-exchange solid-state NMR studies of 13C-enriched wood

Cited by 73 publications

References 9 publications

Study of interactions between polyethylene glycol and archaeological wood components by 13C high-resolution solid-state CP-MAS NMR

Study of interactions between polyethylene glycol and archaeological wood components by 13C high-resolution solid-state CP-MAS NMR

The Target of β-Expansin EXPB1 in Maize Cell Walls from Binding and Solid-State NMR Studies

Characterization of nonderivatized plant cell walls using high‐resolution solution‐state NMR spectroscopy

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