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@ARTICLE{Stief:1025608,
author = {Stief, Tobias and Vormann, Katharina and Lakomek,
Nils-Alexander},
title = {{S}ensitivity-enhanced {NMR} 15{N} {R}1 and {R}1ρ
relaxation experiments for the investigation of
intrinsically disordered proteins at high magnetic fields},
journal = {Methods},
volume = {223},
issn = {1046-2023},
address = {Orlando, Fla.},
publisher = {Academic Press},
reportid = {FZJ-2024-03002},
pages = {1 - 15},
year = {2024},
abstract = {NMR relaxation experiments provide residue-specific
insights into the structural dynamics of proteins. Here, we
present an optimized set of sensitivity-enhanced 15N R1 and
R1ρ relaxation experiments applicable to fully protonated
proteins. The NMR pulse sequences are conceptually similar
to the set of TROSY-based sequences and their HSQC
counterpart (Lakomek et al., J. Biomol. NMR 2012). Instead
of the TROSY read-out scheme, a sensitivity-enhanced HSQC
read-out scheme is used, with improved and easier optimized
water suppression. The presented pulse sequences are applied
on the cytoplasmic domain of the SNARE protein
Synpatobrevin-2 (Syb-2), which is intrinsically disordered
in its monomeric pre-fusion state. A two-fold increase in
the obtained signal-to-noise ratio is observed for this
intrinsically disordered protein, therefore offering a
four-fold reduction of measurement time compared to the
TROSY-detected version. The inter-scan recovery delay can be
shortened to two seconds. Pulse sequences were tested at 600
MHz and 1200 MHz 1H Larmor frequency, thus applicable over a
wide magnetic field range. A comparison between protonated
and deuterated protein samples reveals high agreement,
indicating that reliable 15N R1 and R1ρ rate constants can
be extracted for fully protonated and deuterated samples.
The presented pulse sequences will benefit not only for IDPs
but also for an entire range of low and medium-sized
proteins.},
cin = {IBI-7},
ddc = {540},
cid = {I:(DE-Juel1)IBI-7-20200312},
pnm = {5244 - Information Processing in Neuronal Networks
(POF4-524)},
pid = {G:(DE-HGF)POF4-5244},
typ = {PUB:(DE-HGF)16},
pubmed = {38242384},
UT = {WOS:001175269700001},
doi = {10.1016/j.ymeth.2024.01.008},
url = {https://juser.fz-juelich.de/record/1025608},
}