Selective One-Dimensional 13C–13C Spin-Diffusion Solid-State Nuclear Magnetic Resonance Methods to Probe Spatial Arrangements in Biopolymers Including Plant Cell Walls, Peptides, and Spider Silk

Addison, Bennett; Stengel, Dillan; Bharadwaj, Vivek S.; Happs, Renee M.; Doeppke, Crissa; Wang, Tuo; Bomble, Yannick J.; Holland, Gregory P.; Harman-Ware, Anne E.

doi:10.1021/acs.jpcb.0c07759

Selective One-Dimensional ¹³C–¹³C Spin-Diffusion Solid-State Nuclear Magnetic Resonance Methods to Probe Spatial Arrangements in Biopolymers Including Plant Cell Walls, Peptides, and Spider Silk

Journal Article · Thu Oct 22 00:00:00 EDT 2020 · Journal of Physical Chemistry. B, Condensed Matter, Materials, Surfaces, Interfaces and Biophysical Chemistry

DOI:https://doi.org/10.1021/acs.jpcb.0c07759· OSTI ID:1817869

^[1]; ^[2]; ^[1]; Happs, Renee M. ^[1]; Doeppke, Crissa ^[1]; ^[3]; ^[4]; ^[2]; Harman-Ware, Anne E. ^[1]

National Renewable Energy Lab. (NREL), Golden, CO (United States). Renewable Resources and Enabling Sciences Center
San Diego State Univ., CA (United States)
Louisiana State Univ., Baton Rouge, LA (United States)
National Renewable Energy Lab. (NREL), Golden, CO (United States). Biosciences Center

Two-dimensional (2D) and 3D through-space ¹³C–¹³C homonuclear spin-diffusion techniques are powerful solid-state nuclear magnetic resonance (NMR) tools for extracting structural information from ¹³C-enriched biomolecules, but necessarily long acquisition times restrict their applications. In this work, we explore the broad utility and underutilized power of a chemical shift-selective one-dimensional (1D) version of a 2D ¹³C–¹³C spin-diffusion solid-state NMR technique. The method, which is called 1D dipolar-assisted rotational resonance (DARR) difference, is applied to a variety of biomaterials including lignocellulosic plant cell walls, microcrystalline peptide fMLF, and black widow dragline spider silk. 1D ¹³C–¹³C spin-diffusion methods described here apply in select cases in which the 1D ¹³C solid-state NMR spectrum displays chemical shift-resolved moieties. Furthermore, this is analogous to the selective 1D nuclear Overhauser effect spectroscopy (NOESY) experiment utilized in liquid-state NMR as a faster (1D instead of 2D) and often less ambiguous (direct sampling of the time domain data, coupled with increased signal averaging) alternative to 2D NOESY. Selective 1D ¹³C–¹³C spin-diffusion methods are more time-efficient than their 2D counterparts such as proton-driven spin diffusion (PDSD) and dipolar-assisted rotational resonance. The additional time gained enables measurements of ¹³C–¹³C spin-diffusion buildup curves and extraction of spin-diffusion time constants TSD, yielding detailed structural information. Specifically, selective 1D DARR difference buildup curves applied to ¹³C-enriched hybrid poplar woody stems confirm strong spatial interaction between lignin and acetylated xylan polymers within poplar plant secondary cell walls, and an interpolymer distance of ~0.45–0.5 nm was estimated. Additionally, Tyr/Gly long-range correlations were observed on isotopically enriched black widow spider dragline silks.

View Accepted Manuscript (DOE)

Research Organization:: National Renewable Energy Laboratory (NREL), Golden, CO (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Biological and Environmental Research (BER); USDOE Office of Science (SC), Basic Energy Sciences (BES); USDOE Office of Energy Efficiency and Renewable Energy (EERE); US Air Force Office of Scientific Research (AFOSR); US Army Research Office (ARO)

Grant/Contract Number:: AC36-08GO28308; SC0001090

OSTI ID:: 1817869

Report Number(s):: NREL/JA--2800-77093; MainId:26039; UUID:937ebf38-9cce-4b55-9d33-97814abaa533; MainAdminID:60611

Journal Information:: Journal of Physical Chemistry. B, Condensed Matter, Materials, Surfaces, Interfaces and Biophysical Chemistry, Journal Name: Journal of Physical Chemistry. B, Condensed Matter, Materials, Surfaces, Interfaces and Biophysical Chemistry Journal Issue: 44 Vol. 124; ISSN 1520-6106

Publisher:: American Chemical SocietyCopyright Statement

Country of Publication:: United States

Language:: English

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Selective One-Dimensional 13C–13C Spin-Diffusion Solid-State Nuclear Magnetic Resonance Methods to Probe Spatial Arrangements in Biopolymers Including Plant Cell Walls, Peptides, and Spider Silk

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Selective One-Dimensional ¹³C–¹³C Spin-Diffusion Solid-State Nuclear Magnetic Resonance Methods to Probe Spatial Arrangements in Biopolymers Including Plant Cell Walls, Peptides, and Spider Silk