Utilizing afterglow magnetization from cross-polarization magic-angle-spinning solid-state NMR spectroscopy to obtain simultaneous heteronuclear multidimensional spectra

James R. Banigan, Nathaniel Traaseth

Research output: Contribution to journalArticle

Abstract

The time required for data acquisition and subsequent spectral assignment are limiting factors for determining biomolecular structure and dynamics using solid-state NMR spectroscopy. While strong magnetic dipolar couplings give rise to relatively broad spectra lines, the couplings also mediate the coherent magnetization transfer via the Hartmann-Hahn cross-polarization (HH-CP) experiment. This mechanism is used in nearly all backbone assignment experiments for carrying out polarization transfer between 1H, 15N, and 13C. In this Article, we describe a general spectroscopic approach to use the residual or "afterglow" magnetization from the 15N to 13C selective HH-CP experiment to collect a second multidimensional heteronuclear data set. This approach allowed for the collection of two commonly used sequential assignment experiments (2D NCA and NCO or 3D NCACX and NCOCX) at the same time. Our "afterglow" technique was demonstrated with uniformly [13C,15N] and [1,3- 13C] glycerol-labeled ubiquitin using instrumentation available on all standard solid-state NMR spectrometers configured for magic-angle-spinning. This method is compatible with several other sensitivity enhancement experiments and can be used as an isotopic filtering tool to reduce the spectral complexity and decrease the time needed for assignment.

Original languageEnglish (US)
Pages (from-to)7138-7144
Number of pages7
JournalJournal of Physical Chemistry B
Volume116
Issue number24
DOIs
StatePublished - Jun 21 2012

Fingerprint

Magic angle spinning
cross polarization
afterglows
metal spinning
Nuclear magnetic resonance spectroscopy
Magnetization
Polarization
solid state
magnetization
nuclear magnetic resonance
spectroscopy
Experiments
glycerols
Magnetic couplings
data acquisition
line spectra
Ubiquitin
Glycerol
spectrometers
Spectrometers

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Materials Chemistry
  • Surfaces, Coatings and Films

Cite this

@article{ec54791ffe604758bb558d13be8192b3,
title = "Utilizing afterglow magnetization from cross-polarization magic-angle-spinning solid-state NMR spectroscopy to obtain simultaneous heteronuclear multidimensional spectra",
abstract = "The time required for data acquisition and subsequent spectral assignment are limiting factors for determining biomolecular structure and dynamics using solid-state NMR spectroscopy. While strong magnetic dipolar couplings give rise to relatively broad spectra lines, the couplings also mediate the coherent magnetization transfer via the Hartmann-Hahn cross-polarization (HH-CP) experiment. This mechanism is used in nearly all backbone assignment experiments for carrying out polarization transfer between 1H, 15N, and 13C. In this Article, we describe a general spectroscopic approach to use the residual or {"}afterglow{"} magnetization from the 15N to 13C selective HH-CP experiment to collect a second multidimensional heteronuclear data set. This approach allowed for the collection of two commonly used sequential assignment experiments (2D NCA and NCO or 3D NCACX and NCOCX) at the same time. Our {"}afterglow{"} technique was demonstrated with uniformly [13C,15N] and [1,3- 13C] glycerol-labeled ubiquitin using instrumentation available on all standard solid-state NMR spectrometers configured for magic-angle-spinning. This method is compatible with several other sensitivity enhancement experiments and can be used as an isotopic filtering tool to reduce the spectral complexity and decrease the time needed for assignment.",
author = "Banigan, {James R.} and Nathaniel Traaseth",
year = "2012",
month = "6",
day = "21",
doi = "10.1021/jp303269m",
language = "English (US)",
volume = "116",
pages = "7138--7144",
journal = "Journal of Physical Chemistry B",
issn = "1520-6106",
publisher = "American Chemical Society",
number = "24",

}

TY - JOUR

T1 - Utilizing afterglow magnetization from cross-polarization magic-angle-spinning solid-state NMR spectroscopy to obtain simultaneous heteronuclear multidimensional spectra

AU - Banigan, James R.

AU - Traaseth, Nathaniel

PY - 2012/6/21

Y1 - 2012/6/21

N2 - The time required for data acquisition and subsequent spectral assignment are limiting factors for determining biomolecular structure and dynamics using solid-state NMR spectroscopy. While strong magnetic dipolar couplings give rise to relatively broad spectra lines, the couplings also mediate the coherent magnetization transfer via the Hartmann-Hahn cross-polarization (HH-CP) experiment. This mechanism is used in nearly all backbone assignment experiments for carrying out polarization transfer between 1H, 15N, and 13C. In this Article, we describe a general spectroscopic approach to use the residual or "afterglow" magnetization from the 15N to 13C selective HH-CP experiment to collect a second multidimensional heteronuclear data set. This approach allowed for the collection of two commonly used sequential assignment experiments (2D NCA and NCO or 3D NCACX and NCOCX) at the same time. Our "afterglow" technique was demonstrated with uniformly [13C,15N] and [1,3- 13C] glycerol-labeled ubiquitin using instrumentation available on all standard solid-state NMR spectrometers configured for magic-angle-spinning. This method is compatible with several other sensitivity enhancement experiments and can be used as an isotopic filtering tool to reduce the spectral complexity and decrease the time needed for assignment.

AB - The time required for data acquisition and subsequent spectral assignment are limiting factors for determining biomolecular structure and dynamics using solid-state NMR spectroscopy. While strong magnetic dipolar couplings give rise to relatively broad spectra lines, the couplings also mediate the coherent magnetization transfer via the Hartmann-Hahn cross-polarization (HH-CP) experiment. This mechanism is used in nearly all backbone assignment experiments for carrying out polarization transfer between 1H, 15N, and 13C. In this Article, we describe a general spectroscopic approach to use the residual or "afterglow" magnetization from the 15N to 13C selective HH-CP experiment to collect a second multidimensional heteronuclear data set. This approach allowed for the collection of two commonly used sequential assignment experiments (2D NCA and NCO or 3D NCACX and NCOCX) at the same time. Our "afterglow" technique was demonstrated with uniformly [13C,15N] and [1,3- 13C] glycerol-labeled ubiquitin using instrumentation available on all standard solid-state NMR spectrometers configured for magic-angle-spinning. This method is compatible with several other sensitivity enhancement experiments and can be used as an isotopic filtering tool to reduce the spectral complexity and decrease the time needed for assignment.

UR - http://www.scopus.com/inward/record.url?scp=84862697344&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=84862697344&partnerID=8YFLogxK

U2 - 10.1021/jp303269m

DO - 10.1021/jp303269m

M3 - Article

VL - 116

SP - 7138

EP - 7144

JO - Journal of Physical Chemistry B

JF - Journal of Physical Chemistry B

SN - 1520-6106

IS - 24

ER -