Using a cross-coil to reduce RF heating by an order of magnitude in triple-resonance multinuclear MAS at high fields

Doty, F. David; Kulkarni, Jatin; Turner, Christopher J.; Entzminger, George; Bielecki, Anthony

doi:10.1016/j.jmr.2006.06.031

Cited by 69 publications

(96 citation statements)

References 17 publications

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“…The experiments are carried out using a standard Bruker 3.2 mm probe. It is obvious that probes for which the electric field is excluded from the active sample volume will show reduced uptake of heat [24][25][26]. Probe design, however, cannot be the final solution to this problem, keeping in mind that the resolution obtained in, e.g.…”

Section: Resultsmentioning

confidence: 99%

“…More important, the decoupling scheme induces a significant uptake of heat in the sample, in particular, if the sample contains high concentrations of ions (salt). For this reason, low-E probes have been developed to avoid problems associated with sample heating by partially excluding the electric field from the sample volume [24][25][26]. As a drawback, those probes commonly also have reduced B-fields, implying lower sensitivity.…”

Section: Introductionmentioning

confidence: 99%

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Sensitivity enhancement using paramagnetic relaxation in MAS solid-state NMR of perdeuterated proteins

Linser

Chevelkov

Diehl

et al. 2007

Journal of Magnetic Resonance

127

109

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Previously, Ishii et al., could show that chelated paramagnetic ions can be employed to significantly decrease the recycle delay of a MAS solid-state NMR experiment [N.P. Wickramasinghe, M. Kotecha, A. Samoson, J. Past, Y. Ishii, Sensitivity enhancement in C-13 solid-state NMR of protein microcrystals by use of paramagnetic metal ions for optimizing H-1 T-1 relaxation, J. Magn. Reson. 184 (2007) 350-356]. Application of the method is limited to very robust samples, for which sample stability is not compromised by RF induced heating. In addition, probe integrity might be perturbed in standard MAS PRE experiments due to the use of very short duty cycles. We show that these deleterious effects can be avoided if perdeuterated proteins are employed that have been re-crystallized from D 2 O:H 2 O = 9:1 containing buffer solutions. The experiments are demonstrated using the SH3 domain of chicken a-spectrin as a model system. The labeling scheme allows to record proton detected 1 H, 15 N correlation spectra with very high resolution in the absence of heteronuclear dipolar decoupling. Cu-edta as a doping reagent yields a reduction of the recycle delay by up to a factor of 15. In particular, we find that the 1 H T 1 for the bulk H N magnetization is reduced from 4.4 s to 0.3 s if the Cu-edta concentration is increased from 0 mM to 250 mM. Possible perturbations like chemical shift changes or line broadening due to the paramagnetic chelate complex are minimal. No degradation of our samples was observed in the course of the experiments.

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Sensitivity enhancement using paramagnetic relaxation in MAS solid-state NMR of perdeuterated proteins

Linser

Chevelkov

Diehl

et al. 2007

Journal of Magnetic Resonance

127

109

View full text Add to dashboard Cite

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“…30,41 Such high power RF irradiation is not desirable for heatsensitive samples like membrane proteins. [42][43][44] Therefore, in principle, it is easier to implement through-bond 13 C− 13 C correlation experiments under ultrafast-MAS for sequential resonance assignment purposes. In addition to the suppression of 1 H− 1 H dipolar couplings, ultrafast-MAS dramatically enhances spectral resolution of protons.…”

Section: Introductionmentioning

confidence: 99%

Constant-time 2D and 3D through-bond correlation NMR spectroscopy of solids under 60 kHz MAS

Zhang

Ramamoorthy

2016

The Journal of Chemical Physics

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Establishing connectivity and proximity of nuclei is an important step in elucidating the structure and dynamics of molecules in solids using magic angle spinning (MAS) NMR spectroscopy. Although recent studies have successfully demonstrated the feasibility of proton-detected multidimensional solid-state NMR experiments under ultrafast-MAS frequencies and obtaining high-resolution spectral lines of protons, assignment of proton resonances is a major challenge. In this study, we first re-visit and demonstrate the feasibility of 2D constant-time uniform-sign cross-peak correlation (CTUC-COSY) NMR experiment on rigid solids under ultrafast-MAS conditions, where the sensitivity of the experiment is enhanced by the reduced spin-spin relaxation rate and the use of low radio-frequency power for heteronuclear decoupling during the evolution intervals of the pulse sequence. In addition, we experimentally demonstrate the performance of a proton-detected pulse sequence to obtain a 3D 1 H/ 13 C/ 1 H chemical shift correlation spectrum by incorporating an additional cross-polarization period in the CTUC-COSY pulse sequence to enable proton chemical shift evolution and proton detection in the incrementable t 1 and t 3 periods, respectively. In addition to through-space and through-bond 13 C/ 1 H and 13 C/ 13 C chemical shift correlations, the 3D 1 H/ 13 C/ 1 H experiment also provides a COSY-type 1 H/ 1 H chemical shift correlation spectrum, where only the chemical shifts of those protons, which are bonded to two neighboring carbons, are correlated. By extracting 2D F1/F3 slices ( 1 H/ 1 H chemical shift correlation spectrum) at different 13 C chemical shift frequencies from the 3D 1 H/ 13 C/ 1 H spectrum, resonances of proton atoms located close to a specific carbon atom can be identified. Overall, the through-bond and through-space homonuclear/heteronuclear proximities determined from the 3D 1 H/ 13 C/ 1 H experiment would be useful to study the structure and dynamics of a variety of chemical and biological solids. C 2016 AIP Publishing LLC. [http://dx

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“…The analysis of RF-induced sample heating has led to the development of alternative coil geometries, e.g. scroll and other specialized coils, which reduce RF sample heating by lowering the inductance of the coil and minimizing the electric field generated in the sample (4,(6)(7)(8). Furthermore, many of these designs have the added benefit of high B 1 homogeneity.…”

Section: Introductionmentioning

confidence: 99%

An efficient 1H/31P double-resonance solid-state NMR probe that utilizes a scroll coil

Grant¹,

Sit²,

Angelis³

et al. 2007

Journal of Magnetic Resonance

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The construction and performance of a scroll coil double-resonance probe for solid-state NMR on stationary samples is described. The advantages of the scroll coil at the high resonance frequencies of 1 H and 31 P include: high efficiency, minimal perturbations of tuning by a wide range of samples, minimal RF sample heating of high dielectric samples of biopolymers in aqueous solution, and excellent RF homogeneity. The incorporation of a cable tie cinch for mechanical stability of the scroll coil is described. Experimental results obtained on a Hunter Killer Peptide 1 (HKP1) interacting with phospholipid bilayers of varying lipid composition demonstrate the capabilities of this probe on lossy aqueous samples.

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Using a cross-coil to reduce RF heating by an order of magnitude in triple-resonance multinuclear MAS at high fields

Cited by 69 publications

References 17 publications

Sensitivity enhancement using paramagnetic relaxation in MAS solid-state NMR of perdeuterated proteins

Sensitivity enhancement using paramagnetic relaxation in MAS solid-state NMR of perdeuterated proteins

Constant-time 2D and 3D through-bond correlation NMR spectroscopy of solids under 60 kHz MAS

An efficient 1H/31P double-resonance solid-state NMR probe that utilizes a scroll coil

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