Parallel acquisition of multi-dimensional spectra in protein NMR

Abstract

We introduce the use of multiple receivers applied in parallel for simultaneously recording multi-dimensional data sets of proteins in a single experiment. The utility of the approach is established through the introduction of the 2D (15)N,(1)H(N)||(13)CO HSQC experiment in which a pair of two-dimensional (15)N,(1)H(N) and (15)N,(13)CO spectra are recorded. The methodology is further extended to higher dimensionality via the 3D (1)H(N)||(13)CO HNCA in which a pair of data sets recording (13)C(α),(15)N,(1)H(N) and (13)C(α),(15)N,(13)CO chemical shifts are acquired. With the anticipated increases in probe sensitivity it is expected that multiple receiver experiments will become an important approach for efficient recording of NMR data.

Multiple Parallel 2D NMR Acquisitions in a Single Scan

“…[4][5][6][7][8][9][10][11] Following the introduction of parallel NMR spectroscopy, it was shown that one of its main advantages results from its use to collect two or more different kinds of multidimensional correlation experiments, within the time duration that would normally entail to collect a single spectrum. [5][6][7] These "parallel acquisition NMR, all-in-one combination of experimental applications" (PANACEA) strategies, have since been extended to systems of various heteronuclei [8,9] and adapted to protein liquid-state [10,11] and solid-state NMR experiments. [5][6][7] These "parallel acquisition NMR, all-in-one combination of experimental applications" (PANACEA) strategies, have since been extended to systems of various heteronuclei [8,9] and adapted to protein liquid-state [10,11] and solid-state NMR experiments.…”

Sequential acquisition of multi-dimensional heteronuclear chemical shift correlation spectra with 1H detection

“…{HACANH & HACACO} and {HACACO & HACACONH}, has been demonstrated employing both parallel12 and sequential13 data acquisition procedures. However, as noted already in the literature1112, all other aspects being equal, e.g. magnetisation transfer and relaxation characteristics, the signal intensities seen in the 1 H and 13 C detected data sets would differ because of the difference in the gyromagnetic ratios of the two nuclei.…”

“…In this context, a variety of techniques are currently being explored for reducing data acquisition times78910. One of the approaches that has received considerable attention in the study of proteins, both in solution11121314 and in the solid state151617, involves the simultaneous collection of different chemical shift correlation spectra. For example, using dual receivers with 1 H and 13 C acquisition in the direct dimension, the simultaneous collection of chemical shift correlation spectra, e.g.…”

Parallel NMR spectroscopy with simultaneous detection of 1H and 19F nuclei

“…e): where η > 2. One such example is the H,C'‐N PANSY HSQC experiment that records H‐N and C'‐N 2D correlation experiments in parallel . Assuming that 1 H N nuclei relax twice as fast as the 13 C=O nuclei and the experiment times are dominated by the recovery delays d 1 (H) and d 1 (C') the two 2D spectra are recorded three times faster as compared with the two conventional H‐N and C'‐N correlation experiments whereas the interleaved experiments can be recorded only 1.5 times faster in this particular case.…”