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

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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.

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Acknowledgments

This work was supported by MCYT (project BQU2003-01677). The authors are grateful to the Servei de Ressonància Magnètica Nuclear, UAB, for allocating instrument time to this project and to Dr. W. Bermel for providing us a TS pulse program code. P.N thanks “Generalitat de Catalunya” for a predoctoral grant.

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Authors and Affiliations

  1. Servei de Ressonància Magnètica Nuclear, Facultat de Ciències, Universitat Autònoma de Barcelona, E-08193, Bellaterra, Barcelona, Spain

    Pau Nolis & Teodor Parella

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  1. Pau Nolis
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  2. Teodor Parella
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Correspondence to Teodor Parella.

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Nolis, P., Parella, T. Simultaneous α/β spin-state selection for 13C and 15N from a time-shared HSQC-IPAP experiment. J Biomol NMR 37, 65–77 (2007). https://doi.org/10.1007/s10858-006-9104-z

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  • DOI: https://doi.org/10.1007/s10858-006-9104-z

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