Selective signal detection in solid-state NMR using rotor-synchronized dipolar dephasing for the analysis of hemicellulose in lignocellulosic biomass

Journal of Physical Chemistry Letters

Volumn 4, Issue 14, 2013, Pages 2279-2283

  Komatsu, Takanori ^a,b   Kikuchi, Jun ^a,b,c,d  

^a RIKEN Center for Sustainable Resource Science   (Japan)

^b YOKOHAMA CITY UNIVERSITY   (Japan)

^c RIKEN   (Japan)

^d NAGOYA UNIVERSITY   (Japan)

Author keywords

biomass; molecular motion; NMR spectroscopy; signal separation; spin relaxation

Indexed keywords

DIPOLAR DEPHASING; FILTERING EFFICIENCY; GLUCURONOARABINOXYLAN; LIGNOCELLULOSIC BIOMASS; MOLECULAR MOTIONS; SECONDARY CELL WALL; SIGNAL SEPARATION; SPIN RELAXATION;

BIOMASS; MAGIC ANGLE SPINNING; NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY;

CELLULOSE;

EID: 84880553589     PISSN: None     EISSN: 19487185     Source Type: Journal    
DOI: 10.1021/jz400978g     Document Type: Article

References (46)

1. Andronesi, O. C.; Becker, S.; Seidel, K.; Heise, H.; Young, H. S.; Baldus, M. Determination of Membrane Protein Structure and Dynamics by Magic-Angle-Spinning Solid-State NMR Spectroscopy J. Am. Chem. Soc. 2005, 127, 12965-12974
2. Asakura, T.; Ashida, J.; Yamane, T.; Kameda, T.; Nakazawa, Y.; Ohgo, K.; Komatsu, K. A Repeated Beta-Turn Structure In Poly(Ala-Gly) As A Model For Silk I Of Bombyx Mori Silk Fibroin Studied With Two-Dimensional Spin-Diffusion NMR Under Off Magic Angle Spinning And Rotational Echo Double Resonance J. Mol. Biol. 2001, 306, 291-305
3. 7 Pyrochlores J. Phys. Chem. B 2006, 110, 10358-10364
4. Deazevedo, E. R.; Saalwachter, K.; Pascui, O.; De Souza, A. A.; Bonagamba, T. J.; Reichert, D. Intermediate Motions as Studied by Solid-State Separated Local Field NMR Experiments J. Chem. Phys. 2008, 128
5. Simpson, A. J.; Simpson, M. J.; Soong, R. Nuclear Magnetic Resonance Spectroscopy and Its Key Role in Environmental Research Environ. Sci. Technol. 2012, 46, 11488-11496
6. Bardet, M.; Foray, M. F.; Tran, Q. K. High-Resolution Solid-State CPMAS NMR Study of Archaeological Woods Anal. Chem. 2002, 74, 4386-4390
7. Bardet, M.; Gerbaud, G.; Giffard, M.; Doan, C.; Hediger, S.; Le Pape, L. C-13 High-Resolution Solid-State NMR for Structural Elucidation of Archaeological Woods Prog. Nucl. Magn. Reson. Spectrosc. 2009, 55, 199-214
8. Ragauskas, A. J.; Williams, C. K.; Davison, B. H.; Britovsek, G.; Cairney, J.; Eckert, C. A.; Frederick, W. J.; Hallett, J. P.; Leak, D. J.; Liotta, C. L. The Path Forward for Biofuels and Biomaterials Science 2006, 311, 484-489
9. Mansfield, S. D.; Kim, H.; Lu, F. C.; Ralph, J. Whole Plant Cell Wall Characterization Using Solution-State 2D NMR Nat. Protoc. 2012, 7, 1579-1589
10. Kim, H.; Ralph, J. Solution-State 2D NMR of Ball-Milled Plant Cell Wall Gels in DMSO-d(6)/Pyridine-d(5) Org. Biomol. Chem. 2010, 8, 576-591
11. Watanabe, T.; Shino, A.; Akashi, K.; Kikuchi, J. Spectroscopic Investigation of Tissue-Specific Biomass Profiling for Jatropha Curcas L Plant Biotechnol. 2012, 29, 163-170
12. Ogata, Y.; Chikayama, E.; Morioka, Y.; Everroad, R. C.; Shino, A.; Matsushima, A.; Haruna, H.; Moriya, S.; Toyoda, T.; Kikuchi, J. ECOMICS: A Web-Based Toolkit for Investigating the Biomolecular Web in Ecosystems Using a Transomics Approach. Plos One 2012, 7.
13. Cheng, K.; Sorek, H.; Zimmermann, H.; Wemmer, D. E.; Pauly, M. Solution-State 2D NMR Spectroscopy of Plant Cell Walls Enabled by a Dimethylsulfoxide-d6/1-Ethyl-3-methylimidazolium Acetate Solvent Anal. Chem. 2013, 85, 3213-3221
14. Samuel, R.; Foston, M.; Jaing, N.; Cao, S. L.; Allison, L.; Studer, M.; Wyman, C.; Ragauskas, A. J. HSQC (Heteronuclear Single Quantum Coherence) C-13-H-1 Correlation Spectra of Whole Biomass in Perdeuterated Pyridinium Chloride-DMSO System: An Effective Tool for Evaluating Pretreatment Fuel 2011, 90, 2836-2842
15. Atalla, R. H.; Vanderhart, D. L. Native Cellulose: A Composite of Two Distinct Crystalline Forms Science 1984, 223, 283-285
16. Kono, H.; Erata, T.; Takai, M. Determination of the Through-Bond Carbon-Carbon and Carbon-Proton Connectivities of the Native Celluloses in the Solid State Macromolecules 2003, 36, 5131-5138
17. Kono, H.; Yunoki, S.; Shikano, T.; Fujiwara, M.; Erata, T.; Takai, M. CP/MAS C-13 NMR Study of Cellulose and Cellulose Derivatives. 1. Complete Assignment of the CP/MAS C-13 NMR Spectrum of the Native Cellulose J. Am. Chem. Soc. 2002, 124, 7506-7511
18. Cadars, S.; Lesage, A.; Emsley, L. Chemical Shift Correlations in Disordered Solids J. Am. Chem. Soc. 2005, 127, 4466-4476
19. Mori, T.; Chikayama, E.; Tsuboi, Y.; Ishida, N.; Shisa, N.; Noritake, Y.; Moriya, S.; Kikuchi, J. Exploring the Conformational Space of Amorphous Cellulose Using NMR Chemical Shifts Carbohydr. Polym. 2012, 90, 1197-1203
20. Witter, R.; Sternberg, U.; Hesse, S.; Kondo, T.; Koch, F. T.; Ulrich, A. S. C-13 Chemical Shift Constrained Crystal Structure Refinement of Cellulose I-alpha and Its Verification by NMR Anisotropy Experiments Macromolecules 2006, 39, 6125-6132
21. Okushita, K.; Chikayama, E.; Kikuchi, J. Solubilization Mechanism and Characterization of the Structural Change of Bacterial Cellulose in Regenerated States Through Ionic Liquid Treatment Biomacromolecules 2012, 13, 1323-1330
22. Castellani, F.; van Rossum, B.; Diehl, A.; Schubert, M.; Rehbein, K.; Oschkinat, H. Structure of a Protein Determined by Solid-State Magic-Angle-Spinning NMR Spectroscopy Nature 2002, 420, 98-102
23. Martin, R. W.; Zilm, K. W. Preparation of Protein Nanocrystals and Their Characterization by Solid State NMR J. Magn. Reson. 2003, 165, 162-174
24. Ketchem, R. R.; Hu, W.; Cross, T. A. High-Resolution Conformation of Gramicidin-a in a Lipid Bilayer by Solid-State NMR Science 1993, 261, 1457-1460
25. Fenwick, K. M.; Apperley, D. C.; Cosgrove, D. J.; Jarvis, M. C. Polymer Mobility in Cell Walls of Cucumber Hypocotyls Phytochemistry 1999, 51, 17-22
26. Tang, H. R.; Wang, Y. L.; Belton, P. S. C-13 CPMAS Studies of Plant Cell Wall Materials and Model Systems Using Proton Relaxation-Induced Spectral Editing Techniques Solid State Nucl. Mag. 2000, 15, 239-248
27. Mao, J. D.; Holtman, K. M.; Franqui-Villanueva, D. Chemical Structures of Corn Stover and Its Residue after Dilute Acid Prehydrolysis and Enzymatic Hydrolysis: Insight into Factors Limiting Enzymatic Hydrolysis J. Agr. Food Chem. 2010, 58, 11680-11687
28. Okushita, K.; Komatsu, T.; Chikayama, E.; Kikuchi, J. Statistical Approach for Solid-State NMR Spectra of Cellulose Derived From a Series of Variable Parameters Polym. J. 2012, 44, 895-900
29. Mao, J. D.; Schmidt-Rohr, K. Methylene Spectral Editing in Solid-State C-13 NMR by Three-Spin Coherence Selection J. Magn. Reson. 2005, 176, 1-6
30. Schmidt-Rohr, K.; Mao, J. D. Efficient Ch-Group Selection and Identification in C-13 Solid-State NMR by Dipolar Dept and H-1 Chemical-Shift Filtering J. Am. Chem. Soc. 2002, 124, 13938-13948
31. Opella, S. J.; Frey, M. H. Selection of Non-Protonated Carbon Resonances in Solid-State Nuclear Magnetic Resonance J. Am. Chem. Soc. 1979, 101, 5854-5856
32. Ebringerova, A.; Heinze, T. Xylan and Xylan Derivatives-Biopolymers With Valuable Properties, 1-Naturally Occurring Xylans Structures, Procedures and Properties Macromol. Rapid Commun. 2000, 21, 542-556
33. Nishiyama, Y.; Langan, P.; Chanzy, H. Crystal Structure and Hydrogen-Bonding System in Cellulose Ibeta from Synchrotron X-Ray and Neutron Fiber Diffraction J. Am. Chem. Soc. 2002, 124, 9074-9082
34. Gullion, T.; Schaefer, J. Detection of Weak Heteronuclear Dipolar Coupling by Rotational-Echo Double-Resonance Nuclear Magnetic Resonance Adv. Magn. Opt. Reson. 1989, 13, 57
35. Munowitz, M. G.; Griffin, R. G.; Bodenhausen, G.; Huang, T. H. Two-Dimensional Rotational Spin-Echo Nuclear Magnetic-Resonance in Solids-Correlation of Chemical-Shift and Dipolar Interactions J. Am. Chem. Soc. 1981, 103, 2529-2533
36. Mao, K. M.; Kennedy, G. J.; Althaus, S. M.; Pruski, M. Spectral Editing in C-13 Solid-State NMR at High Magnetic Field Using Fast Mas and Spin-Echo Dephasing Solid State Nucl. Mag. 2012, 47-48, 19-22
37. Hong, M.; Gross, J. D.; Griffin, R. G. Site-Resolved Determination of Peptide Torsion Angle Phi from the Relative Orientations of Backbone N-H and C-H Bonds by Solid-State NMR J. Phys. Chem. B 1997, 101, 5869-5874
38. Hong, M.; Gross, J. D.; Rienstra, C. M.; Griffin, R. G.; Kumashiro, K. K.; Schmidt-Rohr, K. Coupling Amplification in 2D MAS NMR and Its Application to Torsion Angle Determination in Peptides J. Magn. Reson. 1997, 129, 85-92
39. Dick-Perez, M.; Wang, T.; Salazar, A.; Zabotina, O. A.; Hong, M. Multidimensional Solid-State NMR Studies of the Structure and Dynamics of Pectic Polysaccharides in Uniformly C-13-Labeled Arabidopsis Primary Cell Walls Magn. Reson. Chem. 2012, 50, 539-550
40. Dick-Perez, M.; Zhang, Y. A.; Hayes, J.; Salazar, A.; Zabotina, O. A.; Hong, M. Structure and Interactions of Plant Cell-Wall Polysaccharides by Two- and Three-Dimensional Magic-Angle-Spinning Solid-State NMR Biochemistry 2011, 50, 989-1000
41. Mao, K. M.; Kennedy, G. J.; Althaus, S. M.; Pruski, M. Determination of the Average Aromatic Cluster Size of Fossil Fuels by Solid-State NMR at High Magnetic Field Energy Fuels 2013, 27, 760-763
42. York, W. S.; Kolli, V. S. K.; Orlando, R.; Albersheim, P.; Darvill, A. G. The Structures of Arabinoxyloglucans Produced by Solanaceous Plants Carbohydr. Res. 1996, 285, 99-128
43. Eda, S.; Kato, K. Studies on Chemical-Structure of Tobacco Hemicellulose 0.3. Arabinoxyloglucan Isolated from Midrib of Leaves of Nicotiana-Tabacum Agr. Biol. Chem. 1978, 42, 351-357
44. Bennett, A. E.; Ok, J. H.; Griffin, R. G.; Vega, S. Chemical-Shift Correlation Spectroscopy in Rotating Solids-Radio Frequency-Driven Dipolar Recoupling and Longitudinal Exchange J. Chem. Phys. 1992, 96, 8624-8627
45. Szeverenyi, N. M.; Sullivan, M. J.; Maciel, G. E. Observation of Spin Exchange by Two-Dimensional Fourier-Transform C-13 Cross Polarization-Magic- Angle Spinning J. Magn. Reson. 1982, 47, 462-475
46. Takegoshi, K.; Nakamura, S.; Terao, T. C-13-H-1 Dipolar-Assisted Rotational Resonance in Magic-Angle Spinning NMR Chem. Phys. Lett. 2001, 344, 631-637