Optimal control derived sensitivity-enhanced CA-CO mixing
sequences for MAS solid-state NMR - Applications in sequential
protein backbone assignments

J 2023

Optimal control derived sensitivity-enhanced CA-CO mixing sequences for MAS solid-state NMR - Applications in sequential protein backbone assignments

BLAHUT, Jan, Matthias J BRANDL, Riddhiman SARKAR, Bernd REIF, Zdenek TOS et. al.

Basic information

Original name

Optimal control derived sensitivity-enhanced CA-CO mixing sequences for MAS solid-state NMR - Applications in sequential protein backbone assignments

Authors

BLAHUT, Jan, Matthias J BRANDL, Riddhiman SARKAR, Bernd REIF and Zdenek TOS (guarantor)

Edition

JOURNAL OF MAGNETIC RESONANCE OPEN, AMSTERDAM, ELSEVIER, 2023, 2666-4410

Other information

Language

English

Type of outcome

Článek v odborném periodiku

Field of Study

10609 Biochemical research methods

Country of publisher

Netherlands

Confidentiality degree

není předmětem státního či obchodního tajemství

References:

URL

RIV identification code

RIV/00216224:90242/23:00133764

DOI

http://dx.doi.org/10.1016/j.jmro.2023.100122

UT WoS

001134051900001

Keywords in English

FULLY PROTONATED PROTEINS; CROSS-POLARIZATION; SPECTROSCOPY; RESONANCE; DYNAMICS SIMULATION; NCO

Abstract

V originále

We have recently introduced optimal-control derived pulse sequences for sensitivity-enhanced heteronuclear correlation NMR experiments of solid proteins. Preservation of equivalent coherence transfer pathways using transverse-mixing pulses (TROP) in multidimensional pulse schemes allows to increase the sensitivity of the experiments by more than a factor of root 2 per each indirect dimension. In this article, we present homonuclear CA-CO transverse-mixing elements (homoTROP) that are based on dipolar interactions and achieve similar gains as the heteronuclear TROP pulses described previously. Both transfer elements were subsequently implemented in 3D se-hCAcoNH and se-hCOcaNH, that together with the previously introduced 3D se-hCANH and se-hCONH experiments yield a complete set of sensitivity-enhanced protein backbone assignment experiments. In contrast to the J-coupling based methods that are used at fast (60 kHz) and ultrafast MAS (>100 kHz), the homoTROP experiments employ about 10-times shorter mixing times making use of the larger magnitude of the dipolar coupling in comparison to the J couplings. The experiments are demonstrated using a microcrystalline, perdeuterated sample of the chicken alpha-spectrin SH3 domain in which all exchangeable sites are fully back-substituted with protons. We evaluated the gains in efficiency in all experiments site-specifically observing that the se-hCAcoNH and se-hCOcaNH experiments yield an increase in sensitivity by a factor of 1.36 +/- 0.09 and at least a factor of 1.8 with respect to the conventional hcoCAcoNH and hCOcaNH J-based experiments.

Links

90242, large research infrastructures

Name: CIISB III

Citovat

BLAHUT, Jan, Matthias J BRANDL, Riddhiman SARKAR, Bernd REIF and Zdenek TOS. Optimal control derived sensitivity-enhanced CA-CO mixing sequences for MAS solid-state NMR - Applications in sequential protein backbone assignments. JOURNAL OF MAGNETIC RESONANCE OPEN. AMSTERDAM: ELSEVIER, 2023, 16-17, Dec, p. 1-9. ISSN 2666-4410. Available from: https://dx.doi.org/10.1016/j.jmro.2023.100122.

@article{2383600,
   author = {Blahut, Jan and Brandl, Matthias J and Sarkar, Riddhiman and Reif, Bernd and Tos, Zdenek},
   article_location = {AMSTERDAM},
   article_number = {Dec},
   doi = {http://dx.doi.org/10.1016/j.jmro.2023.100122},
   keywords = {FULLY PROTONATED PROTEINS; CROSS-POLARIZATION; SPECTROSCOPY; RESONANCE; DYNAMICS SIMULATION; NCO},
   language = {eng},
   issn = {2666-4410},
   journal = {JOURNAL OF MAGNETIC RESONANCE OPEN},
   title = {Optimal control derived sensitivity-enhanced CA-CO mixing sequences for MAS solid-state NMR - Applications in sequential protein backbone assignments},
   url = {https://www.sciencedirect.com/science/article/pii/S2666441023000304?via%3Dihub},
   volume = {16-17},
   year = {2023}
}

TY  - JOUR
ID  - 2383600
AU  - Blahut, Jan - Brandl, Matthias J - Sarkar, Riddhiman - Reif, Bernd - Tos, Zdenek
PY  - 2023
TI  - Optimal control derived sensitivity-enhanced CA-CO mixing sequences for MAS solid-state NMR - Applications in sequential protein backbone assignments
JF  - JOURNAL OF MAGNETIC RESONANCE OPEN
VL  - 16-17
IS  - Dec
SP  - 1-9
EP  - 1-9
PB  - ELSEVIER
SN  - 26664410
KW  - FULLY PROTONATED PROTEINS
KW  - CROSS-POLARIZATION
KW  - SPECTROSCOPY
KW  - RESONANCE
KW  - DYNAMICS SIMULATION
KW  - NCO
UR  - https://www.sciencedirect.com/science/article/pii/S2666441023000304?via%3Dihub
N2  - We have recently introduced optimal-control derived pulse sequences for sensitivity-enhanced heteronuclear correlation NMR experiments of solid proteins. Preservation of equivalent coherence transfer pathways using transverse-mixing pulses (TROP) in multidimensional pulse schemes allows to increase the sensitivity of the experiments by more than a factor of root 2 per each indirect dimension. In this article, we present homonuclear CA-CO transverse-mixing elements (homoTROP) that are based on dipolar interactions and achieve similar gains as the heteronuclear TROP pulses described previously. Both transfer elements were subsequently implemented in 3D se-hCAcoNH and se-hCOcaNH, that together with the previously introduced 3D se-hCANH and se-hCONH experiments yield a complete set of sensitivity-enhanced protein backbone assignment experiments. In contrast to the J-coupling based methods that are used at fast (60 kHz) and ultrafast MAS (>100 kHz), the homoTROP experiments employ about 10-times shorter mixing times making use of the larger magnitude of the dipolar coupling in comparison to the J couplings. The experiments are demonstrated using a microcrystalline, perdeuterated sample of the chicken alpha-spectrin SH3 domain in which all exchangeable sites are fully back-substituted with protons. We evaluated the gains in efficiency in all experiments site-specifically observing that the se-hCAcoNH and se-hCOcaNH experiments yield an increase in sensitivity by a factor of 1.36 +/- 0.09 and at least a factor of 1.8 with respect to the conventional hcoCAcoNH and hCOcaNH J-based experiments.
ER  -

BLAHUT, Jan, Matthias J BRANDL, Riddhiman SARKAR, Bernd REIF and Zdenek TOS. Optimal control derived sensitivity-enhanced CA-CO mixing sequences for MAS solid-state NMR - Applications in sequential protein backbone assignments. \textit{JOURNAL OF MAGNETIC RESONANCE OPEN}. AMSTERDAM: ELSEVIER, 2023, 16-17, Dec, p.~1-9. ISSN~2666-4410. Available from: https://dx.doi.org/10.1016/j.jmro.2023.100122.

Detailed Information on Publication Record