Simultaneous α/β spin-state selection for ¹³C and ¹⁵N from a time-shared HSQC-IPAP experiment

Authors: Nolis, Pau; Parella, Teodor

Source: Journal of Biomolecular NMR, Volume 37, Number 1, January 2007 , pp. 65-77(13)

Publisher: Springer

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Abstract:

Two novel HSQC-IPAP approaches are proposed to achieve α/β spin-state editing simultaneously for ¹³C and ¹⁵N in a single NMR experiment. The pulse schemes are based on a time-shared (TS) 2D ¹H,¹³C/¹H,¹⁵N-HSQC correlation experiment that combines concatenated echo elements for simultaneous J(CH) and J(NH) coupling constants evolution, TS evolution of ¹³C and ¹⁵N chemical shifts in the indirect dimension and heteronuclear α/β-spin-state selection by means of the IPAP principle. Heteronuclear α/β-editing for all CH_n (n = 1-3) and NH_n (1-2) multiplicities can be achieved in the detected F2 dimension of a single TS-HSQC-F2-IPAP experiment. On the other hand, an alternative TS-HSQC-F1-IPAP experiment is also proposed to achieve α/β-editing in the indirect F1 dimension. Experimental and simulated data is provided to evaluate these principles in terms of sensitivity and performance simultaneously on backbone and side-chain CH, CH₂, CH₃, NH, and NH₂ spin systems in uniformly ¹³C/¹⁵N-labeled proteins and in small natural-abundance peptides.

Keywords: NMR; HSQC; Spin-state selection; Coupling constants; IPAP; Time-sharing

Document Type: Research article

DOI: http://dx.doi.org/10.1007/s10858-006-9104-z

Affiliations: 1: Email: teodor.parella@uab.es

Publication date: 2007-01-01