Abstract
Analysis of NMR relaxation data has provided significant insight on molecular dynamic, leading to a more comprehensive understanding of macromolecular functions. However, traditional methodology allows relaxation measurements performed only at a few fixed high fields, thus severely restricting their potential for extracting more complete dynamic information. Here we report the design and performance of a compact high-speed servo-mechanical shuttle assembly adapted to a commercial 600 MHz high-field superconducting magnet. The assembly is capable of shuttling the sample in a regular NMR tube from the center of the magnet to the top (fringe field ∼0.01 T) in 100 ms with no loss of sensitivity other than that due to intrinsic relaxation. The shuttle device can be installed by a single experienced user in 30 min. Excellent 2D- 15N-HSQC spectra of (u- 13C, 15N)-ubiquitin with relaxation at low fields (3.77 T) and detection at 14.1 T were obtained to illustrate its utility in R 1 measurements of macromolecules at low fields. Field-dependent 13C-R 1 data of (3,3,3-d)-alanine at various field strengths were determined and analyzed to assess CSA and 1H- 13C dipolar contributions to the carboxyl 13C-R 1.
| Original language | English |
|---|---|
| Pages (from-to) | 302-308 |
| Number of pages | 7 |
| Journal | Journal of Magnetic Resonance |
| Volume | 214 |
| DOIs | |
| Publication status | Published - 2012 Jan 1 |
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Keywords
- Field cycling
- Field-dependent NMR relaxation
- High-speed sample shuttler
- Molecular dynamics
- Nuclear magnetic relaxation dispersion (NMRD)
- Servo-mechanical shuttler
ASJC Scopus subject areas
- Biophysics
- Biochemistry
- Nuclear and High Energy Physics
- Condensed Matter Physics
Cite this
A compact high-speed mechanical sample shuttle for field-dependent high-resolution solution NMR. / Chou, Ching Yu; Chu, Minglee; Chang, Chi Fon; Huang, Tai-huang.
In: Journal of Magnetic Resonance, Vol. 214, 01.01.2012, p. 302-308.Research output: Contribution to journal › Article
}
TY - JOUR
T1 - A compact high-speed mechanical sample shuttle for field-dependent high-resolution solution NMR
AU - Chou, Ching Yu
AU - Chu, Minglee
AU - Chang, Chi Fon
AU - Huang, Tai-huang
PY - 2012/1/1
Y1 - 2012/1/1
N2 - Analysis of NMR relaxation data has provided significant insight on molecular dynamic, leading to a more comprehensive understanding of macromolecular functions. However, traditional methodology allows relaxation measurements performed only at a few fixed high fields, thus severely restricting their potential for extracting more complete dynamic information. Here we report the design and performance of a compact high-speed servo-mechanical shuttle assembly adapted to a commercial 600 MHz high-field superconducting magnet. The assembly is capable of shuttling the sample in a regular NMR tube from the center of the magnet to the top (fringe field ∼0.01 T) in 100 ms with no loss of sensitivity other than that due to intrinsic relaxation. The shuttle device can be installed by a single experienced user in 30 min. Excellent 2D- 15N-HSQC spectra of (u- 13C, 15N)-ubiquitin with relaxation at low fields (3.77 T) and detection at 14.1 T were obtained to illustrate its utility in R 1 measurements of macromolecules at low fields. Field-dependent 13C-R 1 data of (3,3,3-d)-alanine at various field strengths were determined and analyzed to assess CSA and 1H- 13C dipolar contributions to the carboxyl 13C-R 1.
AB - Analysis of NMR relaxation data has provided significant insight on molecular dynamic, leading to a more comprehensive understanding of macromolecular functions. However, traditional methodology allows relaxation measurements performed only at a few fixed high fields, thus severely restricting their potential for extracting more complete dynamic information. Here we report the design and performance of a compact high-speed servo-mechanical shuttle assembly adapted to a commercial 600 MHz high-field superconducting magnet. The assembly is capable of shuttling the sample in a regular NMR tube from the center of the magnet to the top (fringe field ∼0.01 T) in 100 ms with no loss of sensitivity other than that due to intrinsic relaxation. The shuttle device can be installed by a single experienced user in 30 min. Excellent 2D- 15N-HSQC spectra of (u- 13C, 15N)-ubiquitin with relaxation at low fields (3.77 T) and detection at 14.1 T were obtained to illustrate its utility in R 1 measurements of macromolecules at low fields. Field-dependent 13C-R 1 data of (3,3,3-d)-alanine at various field strengths were determined and analyzed to assess CSA and 1H- 13C dipolar contributions to the carboxyl 13C-R 1.
KW - Field cycling
KW - Field-dependent NMR relaxation
KW - High-speed sample shuttler
KW - Molecular dynamics
KW - Nuclear magnetic relaxation dispersion (NMRD)
KW - Servo-mechanical shuttler
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UR - http://www.scopus.com/inward/citedby.url?scp=84855644575&partnerID=8YFLogxK
U2 - 10.1016/j.jmr.2011.12.001
DO - 10.1016/j.jmr.2011.12.001
M3 - Article
C2 - 22200566
AN - SCOPUS:84855644575
VL - 214
SP - 302
EP - 308
JO - Journal of Magnetic Resonance
JF - Journal of Magnetic Resonance
SN - 1090-7807
ER -