4.3 Article

Band-selective universal 90° and 180° rotation pulses covering the aliphatic carbon chemical shift range for triple resonance experiments on 1.2 GHz spectrometers

Journal

JOURNAL OF BIOMOLECULAR NMR
Volume 76, Issue 5-6, Pages 185-195

Publisher

SPRINGER
DOI: 10.1007/s10858-022-00404-1

Keywords

Triple resonance experiments; 1.2 GHz; Band-selective pulses; Universal rotations; Excitation; refocusing

Funding

  1. Deutsche Forschungsgemeinschaft [LU 835/13-1]
  2. HGF programme Information [P3T5, 43.35.02]

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Biomolecular NMR spectroscopy requires high magnetic field strengths for high spectral resolution. This study presents band-selective universal rotation pulses with a higher ratio of selective bandwidth to maximum rf-amplitude, which perform better than standard pulses according to simulations.
Biomolecular NMR spectroscopy requires large magnetic field strengths for high spectral resolution. Today's highest fields comprise proton Larmor frequencies of 1.2 GHz and even larger field strengths are to be expected in the future. In protein triple resonance experiments, various carbon bandwidths need to be excited by selective pulses including the large aliphatic chemical shift range. When the spectrometer field strength is increased, the length of these pulses has to be decreased by the same factor, resulting in higher rf-amplitudes being necessary in order to cover the required frequency region. Currently available band-selective pulses like Q3/Q5 excite a narrow bandwidth compared to the necessary rf-amplitude. Because the maximum rf-power allowed in probeheads is limited, none of the selective universal rotation pulses reported so far is able to cover the ful1 C-13 aliphatic region on 1.2 GHz spectrometers. In this work, we present band-selective 90 degrees and 180 degrees universal rotation pulses (SURBOP90 and SURBOP180) that have a higher ratio of selective bandwidth to maximum rf-amplitude than standard pulses. Simulations show that these pulses perform better than standard pulses, e. g. Q3/Q5, especially when rf-inhomogeneity is taken into account. The theoretical and experimental performance is demonstrated in offset profiles and by implementing the SURBOP pulses in an HNCACB experiment at 1.2 GHz.

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