title: Sensitivity gains, linearity, and spectral reproducibility in nonuniformly sampled multidimensional MAS NMR spectra of high dynamic range.
abstract: Recently, we have demonstrated that considerable inherent sensitivity gains are attained in MAS NMR spectra acquired by nonuniform sampling (NUS) and introduced maximum entropy interpolation (MINT) processing that assures the linearity of transformation between the time and frequency domains. In this report, we examine the utility of the NUS/MINT approach in multidimensional datasets possessing high dynamic range, such as homonuclear (13)C-(13)C correlation spectra. We demonstrate on model compounds and on 1-73-(U-(13)C,(15)N)/74-108-(U-(15)N) E. coli thioredoxin reassembly, that with appropriately constructed 50% NUS schedules inherent sensitivity gains of 1.7-2.1-fold are readily reached in such datasets. We show that both linearity and line width are retained under these experimental conditions throughout the entire dynamic range of the signals. Furthermore, we demonstrate that the reproducibility of the peak intensities is excellent in the NUS/MINT approach when experiments are repeated multiple times and identical experimental and processing conditions are employed. Finally, we discuss the principles for design and implementation of random exponentially biased NUS sampling schedules for homonuclear (13)C-(13)C MAS correlation experiments that yield high-quality artifact-free datasets.
authors.affiliation: Department of Chemistry and Biochemistry, University of Delaware, Newark, DE, 19716, USA, csuiter@udel.edu.
authors.forename: Christopher L
authors.initials: CL
authors.lastname: Suiter
authors.forename: Sivakumar
authors.initials: S
authors.lastname: Paramasivam
authors.forename: Guangjin
authors.initials: G
authors.lastname: Hou
authors.forename: Shangjin
authors.initials: S
authors.lastname: Sun
authors.forename: David
authors.initials: D
authors.lastname: Rice
authors.forename: Jeffrey C
authors.initials: JC
authors.lastname: Hoch
authors.forename: David
authors.initials: D
authors.lastname: Rovnyak
authors.forename: Tatyana
authors.initials: T
authors.lastname: Polenova
mesh_terms: D066241:Carbon-13 Magnetic Resonance Spectroscopy; D030562:Databases, Protein; D006639:Histidine / Q000737:chemistry; D019906:Nuclear Magnetic Resonance, Biomolecular; D010455:Peptides / Q000737:chemistry; D015203:Reproducibility of Results; D013879:Thioredoxins / Q000378:metabolism
chemical_list: D010455:Peptides; D006639:Histidine; D013879:Thioredoxins
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