High-resolution 14N-edited 1H–13C correlation NMR experiment to study biological solids

An efficient NMR method for the characterisation of 14N sites through indirect 13C detection

“…These efficiencies are comparable with efficiencies reported by other authors for indirect detection of 14 N in when applied to systems with similar quadrupolar interactions. 8–17,19–21 …”

“…10,12,13,15–17 In the studies presented, the coherence order of interest has been isolated purely by means of phase cycling, as shown in Fig. 1.…”

Very fast magic angle spinning 1H-14N 2D solid-state NMR: Sub-micro-liter sample data collection in a few minutes

“…Detecting dynamics on 100 ns time scale [18] has also been achieved using the molecular motion sensitive SQ coherences in the 1 H-14 N HMQC experiment. 1 H-14 N D-HMQC filtering methods for spectral editing [19,20], and three dimensional correlation among 1 H, 13 C, and 14 N [11] have also been reported.…”

Rapid analysis of isotopically unmodified amino acids by high-resolution 14N-edited 1H–13C correlation NMR spectroscopy

“…11 However, the efficiency of 13 C -14 N -13 C transfer was very weak (4-5%) and the experiment lasted 85 h on a 18.8 T spectrometer. It was recently pointed out 12 that in case of small or medium sized molecules, peak assignment could be extracted from three 2D spectra instead of a much longer 3D experiment: (i) a 1 H-14 N D-HMQC spectrum, (ii) a 1 H-13 C CP-HETCOR spectrum and (iii) a 14 N-edited 1 H-13 C CP-HETCOR spectrum. 14 N edition allows selecting crosspeaks resulting from 13 C nuclei in proximity to a nitrogen atom.…”

“…In ref. 12, the 2D 14 N-edited 1 H-13 C CP-HETCOR spectrum was obtained from a 2D version of the 3D 1 H-13 C-14 N previous experiment that was improved by using a more robust heteronuclear dipolar recoupling 14 and 1 H homonuclear dipolar decoupling. 15 Nonetheless, as stated before, the 13 C-14 N- 13 C HMQC filter transfer remains only E5% efficient and the 14 N-edited 1 H- 13 C spectrum lasted 340 min at 18.8 T for 13 C-labeled histidine.…”