Aromatic SOFAST-HMBC for proteins at natural 13C abundance

被引：2

作者：

Vallet, Alicia ^{[1
]}

Favier, Adrien ^{[1
]}

Brutscher, Bernhard ^{[1
]}

机构：

[1] Univ Grenoble Alpes, CEA, CNRS, IBS, F-38000 Grenoble, France

来源：

JOURNAL OF MAGNETIC RESONANCE | 2019年 / 300卷

关键词：

SOFAST; Protein; Aromatics; Resonance assignment; Longitudinal relaxation optimization; Cryogenic probe; High field NMR; 2-DIMENSIONAL NMR EXPERIMENTS; RESONANCE ASSIGNMENT; SIDE-CHAINS; SPECTROSCOPY; RESIDUES; ACIDS;

D O I：

10.1016/j.jmr.2019.01.009

中图分类号：

Q5 [生物化学];

学科分类号：

071010 ; 081704 ;

摘要：

We propose here SOFAST-HMBC as a new complementary NMR tool for aromatic side chain assignment of protein samples at natural C-13 abundance. The characteristic peak patterns detected in SOFAST-HMBC for each aromatic side chain allow straightforward assignment of all protons and carbons (including quaternary ones) of the aromatic ring, and for tyrosine and phenylalanine, connection to the CB of the aliphatic chain. The performance of SOFAST-HMBC is demonstrated for three small proteins (7-14 kDa) at millimolar sample concentration using modern high-field NMR instruments equipped with cryogenically cooled probes. Despite the low amount of NMR-active C-13 nuclei in these samples, H-1-C-13 multiple-bond correlation spectra of good quality were obtained in reasonable experimental times of typically less than 24 h. (C) 2019 Elsevier Inc. All rights reserved.

引用

页码：95 / 102

页数：8

共 50 条

[11] In Situ Hyperpolarization Enables 15N and 13C Benchtop NMR at Natural Isotopic Abundance [J].

Kircher, Raphael ;

Xu, Jingyan ;

Barskiy, Danila A. .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2023, 146 (01) :514-520

[12] The influence of thermochemical treatments on the lignocellulosic structure of wheat straw as studied by natural abundance 13C NMR [J].

Habets, S. ;

de Wild, P. J. ;

Huijgen, W. J. J. ;

van Eck, E. R. H. .

BIORESOURCE TECHNOLOGY, 2013, 146 :585-590

[13] 15N and 13C- SOFAST-HMQC editing enhances 3D-NOESY sensitivity in highly deuterated, selectively [1H,13C]-labeled proteins [J].

Paolo Rossi ;

Youlin Xia ;

Nandish Khanra ;

Gianluigi Veglia ;

Charalampos G. Kalodimos .

Journal of Biomolecular NMR, 2016, 66 :259-271

[14] Characterization of Stratum Corneum Molecular Dynamics by Natural-Abundance 13C Solid-State NMR [J].

Bjorklund, Sebastian ;

Nowacka, Agnieszka ;

Bouwstra, Joke A. ;

Sparr, Emma ;

Topgaard, Daniel .

PLOS ONE, 2013, 8 (04)

[15] 15N and 13C- SOFAST-HMQC editing enhances 3D-NOESY sensitivity in highly deuterated, selectively [1H,13C]-labeled proteins [J].

Rossi, Paolo ;

Xia, Youlin ;

Khanra, Nandish ;

Veglia, Gianluigi ;

Kalodimos, Charalampos G. .

JOURNAL OF BIOMOLECULAR NMR, 2016, 66 (04) :259-271

[16] A 13C Labeling Strategy Reveals a Range of Aromatic Side Chain Motion in Calmodulin [J].

Kasinath, Vignesh ;

Valentine, Kathleen G. ;

Wand, A. Joshua .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2013, 135 (26) :9560-9563

[17] Triple resonance-based 13Cα and 13Cβ CEST experiments for studies of ms timescale dynamics in proteins [J].

Long, Dong ;

Sekhar, Ashok ;

Kay, Lewis E. .

JOURNAL OF BIOMOLECULAR NMR, 2014, 60 (04) :203-208

[18] Measuring 13C/15N chemical shift anisotropy in [13C,15N] uniformly enriched proteins using CSA amplification [J].

Hung, Ivan ;

Ge, Yuwei ;

Liu, Xiaoli ;

Liu, Mali ;

Li, Conggang ;

Gan, Zhehong .

SOLID STATE NUCLEAR MAGNETIC RESONANCE, 2015, 72 :96-103

[19] Probing the Natural-Abundance 13C Populations of Insoluble Elastin Using 13C-1H Heteronuclear Correlation (HETCOR) NMR Spectroscopy [J].

Ohgo, Kosuke ;

Niemczura, Walter P. ;

Kumashiro, Kristin K. .

MACROMOLECULES, 2009, 42 (18) :7024-7030

[20] δ13C of aromatic compounds in sediments, oils and atmospheric emissions: A review [J].

Holman, Alex, I ;

Grice, Kliti .

ORGANIC GEOCHEMISTRY, 2018, 123 :27-37

← 1 2 3 4 5 →