Solid-State 13C Nuclear Magnetic Resonance Characterization of Cellulose in the Cell Walls of Arabidopsis thaliana Leaves

Newman, Roger H.; Davies, Lynette M.; Harris, Philip J.

doi:10.1104/pp.111.2.475

Cited by 100 publications

(80 citation statements)

References 33 publications

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“…Bacterial cellulose is rich in the I a allomorph, while the secondary walls of higher plants mainly contain the I b allomorph (Atalla and Vanderhart, 1984), whose conformations and hydrogen-bonding patterns differ from those of the I a allomorph (Nishiyama et al, 2002(Nishiyama et al, , 2003. In Arabidopsis leaves, the cellulose 13 C signals indicate the presence of both I a and I b allomorphs, with slightly higher I b contents (Newman et al, 1996). The detailed structures of primary wall microfibrils are still unknown, but in silico results suggest that cellulose chains in small microfibrils differ from those in extended crystalline phases in terms of chain tilts and various dihedral angles (Oehme et al, 2015).…”

Section: Discussionmentioning

confidence: 99%

Cellulose-Pectin Spatial Contacts Are Inherent to Never-Dried Arabidopsis Primary Cell Walls: Evidence from Solid-State Nuclear Magnetic Resonance

et al. 2015

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The structural role of pectins in plant primary cell walls is not yet well understood because of the complex and disordered nature of the cell wall polymers. We recently introduced multidimensional solid-state nuclear magnetic resonance spectroscopy to characterize the spatial proximities of wall polysaccharides. The data showed extensive cross peaks between pectins and cellulose in the primary wall of Arabidopsis (Arabidopsis thaliana), indicating subnanometer contacts between the two polysaccharides. This result was unexpected because stable pectin-cellulose interactions are not predicted by in vitro binding assays and prevailing cell wall models. To investigate whether the spatial contacts that give rise to the cross peaks are artifacts of sample preparation, we now compare never-dried Arabidopsis primary walls with dehydrated and rehydrated samples. Onedimensional 13 C spectra, two-dimensional 13 C-13 C correlation spectra, water-polysaccharide correlation spectra, and dynamics data all indicate that the structure, mobility, and intermolecular contacts of the polysaccharides are indistinguishable between never-dried and rehydrated walls. Moreover, a partially depectinated cell wall in which 40% of homogalacturonan is extracted retains cellulose-pectin cross peaks, indicating that the cellulose-pectin contacts are not due to molecular crowding. The cross peaks are observed both at 220°C and at ambient temperature, thus ruling out freezing as a cause of spatial contacts. These results indicate that rhamnogalacturonan I and a portion of homogalacturonan have significant interactions with cellulose microfibrils in the native primary wall. This pectin-cellulose association may be formed during wall biosynthesis and may involve pectin entrapment in or between cellulose microfibrils, which cannot be mimicked by in vitro binding assays.

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Section: Discussionmentioning

confidence: 99%

Cellulose-Pectin Spatial Contacts Are Inherent to Never-Dried Arabidopsis Primary Cell Walls: Evidence from Solid-State Nuclear Magnetic Resonance

et al. 2015

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“…Questions of quantitative reliability and optimization of contact or delay times have been widely discussed elsewhere, and there has been no attempt cover other techniques such as RAMP (noted previously), or separation of subspectra based on differences in 13 C and 1 H relaxation times Newman 1992, 1995;Newman and Condron 1995;Newman et al 1996;Golchin et al 1997a, b;Condron and Newman 1998;Mao et al 1998;Nelson et al 1999;Smernik and Oades 1999;Smernik et al 2000). The aim has been to focus on basic applications most common in SOM studies, from fresh litter to low-C organo-mineral complexes.…”

Section: Discussionmentioning

confidence: 99%

Carbon-13 solid-state NMR of soil organic matter - using the technique effectively

Preston¹

2001

Can. J. Soil. Sci.

112

104

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).Preston, C. M. 2001. Carbon-13 solid-state NMR of soil organic matter -using the technique effectively. Can. J. Soil Sci. 81: 255-270. Solid-state 13 C CPMAS NMR offers many options for characterizing carbon in soil organic matter (SOM). Its effectiveness, however, is often limited by a poor understanding of the techniques, and lack of hands-on access and training opportunities for students. Of nearly 250 modern NMR systems in Canada, approximately one is genuinely available for SOM studies, and there is poor communication between NMR operators and SOM users. While quantitative reliability can be addressed to some extent by multiple contact-time experiments or single-pulse (Bloch decay) spectra, it is also important to consider the effects of spectrometer background, spinning sidebands (especially with higher magnetic fields) and processing operations such as linebroadening, phasing and baseline correction. In many studies, more consideration needs to be given to instrument specifications, the type of information needed, and whether sample fractionation or pretreatment should be used. Structural information can be greatly enhanced by dipolar-dephasing and sideband suppression sequences. Sequences based on relaxation differences can reveal pools of carbon with different structures. Data analysis can be enhanced by principal component analysis, spectrum deconvolution and difference spectra. Studies of xenobiotics and C metabolism can be greatly aided by 13 C-labeling. However, a key limitation to SOM applications remains the gap in culture and expectations of the users.Key words: Soil organic matter, 13 C CPMAS NMR, Bloch decay, dipolar dephasing, spinning sidebands Preston, C. M. 2001. Analyse de la matière organique du sol par RMN au 13 C électronique -de l'importance de bien utiliser la technique. Can. J. Soil Sci. 81: 255-270. La RMN CPMAS 13 C électronique permet de caractériser le carbone présent dans la matière organique du sol (MOS) de diverses manières. Il arrive souvent cependant que cette technique perde de son efficacité parce qu'on la connaît mal et parce que les étudiants n'ont pas eu la chance de l'examiner ou de l'expérimenter. Sur les 250 systèmes modernes de RMN existant au Canada, un seul, à peu près, est vraiment réservé à l'étude de la MOS; de plus, la communication passe mal entre les opérateurs de systèmes RMN et les utilisateurs de MOS. Bien qu'on puisse remédier dans une certaine mesure au problème de la fiabilité quantitative en multipliant les expériences sur la durée de contact ou en recourant au spectre obtenu après une seule impulsion (décroissance de Bloch), il ne faut pas négliger les effets de l'arrière-plan du spectromètre, de la rotation des bandes latérales (surtout quand le champ magnétique est puissant) et des opérations de traitement comme l'élargissement des lignes, la mise en phase et la correction de la ligne de base. Dans de nombreux cas, on devrait accorder plus d'attention aux paramètres de l'instrument, au genre de données requises et à la nécessité de fractionner et...

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“…In particular, proton spin relaxation editing using T 1r H has provided the best discrimination between cellulose and other cell wall components. 28 Additionally, from a study using model systems and plant cell walls, it has been shown that long T 1r H components are associated with crystalline cellulose, implying that the proton spin diffusion between the cellulose crystalline microfibrils and the surface amorphous cellulose is less efficient on the time scale of T 1r H than on that of T 1 H . 29 A further improved method for collecting spectra could be applied to support the assignments from the CP spectra, such as the example described above for the C5 amorphous structure signal candidate.…”

Section: Future Improvement Of This Methodsmentioning

confidence: 99%

Statistical approach for solid-state NMR spectra of cellulose derived from a series of variable parameters

Okushita

Komatsu

Chikayama

et al. 2012

Polym J

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Principle component analysis (PCA) was used to extract components from the solid-state nuclear magnetic resonance (NMR) spectra of bacterial cellulose (BC). Polymers such as cellulose have several domain structures, and their structure and dynamics are reflected in the variety of solid-state spectra derived from different parameters. The complexity of the obtained spectra makes the analysis of spectra from relaxation measurements difficult. Multivariate analysis, such as PCA, has been suggested as an option to improve NMR spectral analyses. In this study, we attempted to extract peak components from cross polarization (CP) experiment data from the variable contact time spectra of BC by using PCA. The extracted peaks were annotated according to previous reports, and the existence of crystalline Ia was clearly recognized. The important components of the BC structure (that is, crystalline Ia, amorphous form and mobility) were separated in the PCA-loading plot and CP curve.

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Solid-State 13C Nuclear Magnetic Resonance Characterization of Cellulose in the Cell Walls of Arabidopsis thaliana Leaves

Cited by 100 publications

References 33 publications

Cellulose-Pectin Spatial Contacts Are Inherent to Never-Dried Arabidopsis Primary Cell Walls: Evidence from Solid-State Nuclear Magnetic Resonance

Cellulose-Pectin Spatial Contacts Are Inherent to Never-Dried Arabidopsis Primary Cell Walls: Evidence from Solid-State Nuclear Magnetic Resonance

Carbon-13 solid-state NMR of soil organic matter - using the technique effectively

Statistical approach for solid-state NMR spectra of cellulose derived from a series of variable parameters

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