Journal
JOURNAL OF MAGNETIC RESONANCE
Volume 214, Issue -, Pages 91-102Publisher
ACADEMIC PRESS INC ELSEVIER SCIENCE
DOI: 10.1016/j.jmr.2011.10.009
Keywords
Sparse sampling; Four-dimensional spectroscopy; Signal separation algorithm; CLEAN; HCCH-TOCSY; C. N-edited NOESY; Engrailed 2
Funding
- Bio-NMR Project [261863]
- European Commission
- Access to Research Infrastructures activity of FP7 [228461]
- TGE RMN THC [Fr3050]
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The development of non-uniform sampling (NUS) strategies permits to obtain high-dimensional spectra with increased resolution in significantly reduced experimental time. We extended a previously proposed signal separation algorithm (SSA) to process sparse four-dimensional NMR data. It is employed for two experiments carried out for a partially unstructured 114-residue construct of chicken Engrailed 2 protein, namely 4D HCCH-TOCSY and 4D C, N-edited NOESY. The SSA allowed us to obtain high-quality spectra using only as little as 0.16% of the available samples, with low sampling artefacts approaching the thermal noise level in most spectral regions. It is demonstrated that NUS 4D HCCH-TOCSY is dominated by sampling noise and requires efficient artefact suppression. On the other hand, 4D C, N-edited NOESY is a particularly attractive experiment for NUS, as the absence of diagonal peaks renders the problem of artefacts less critical. We also present a transverse-relaxation optimized sequence for HMQC that is especially designed for longer evolution periods in the indirectly detected proton dimension in high-dimensional pulse sequences. In conjunction with novel sampling strategies and efficient processing methods, this improvement enabled us to obtain unique structural information about aliphatic-amide contacts. (C) 2011 Elsevier Inc. All rights reserved.
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