A compact high-speed mechanical sample shuttle for field-dependent high-resolution solution NMR.
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-(15)N-HSQC spectra of (u-(13)C, (15)N)-ubiquitin with relaxation at low fields (3.77 T) and detection at 14.1T were obtained to illustrate its utility in R(1) measurements of macromolecules at low fields. Field-dependent (13)C-R(1) data of (3,3,3-d)-alanine at various field strengths were determined and analyzed to assess CSA and (1)H-(13)C dipolar contributions to the carboxyl (13)C-R(1).
Department of Physics, National Taiwan Normal University, Taipei 116, Taiwan, ROC.
Ching-Yu
CY
Chou
Minglee
M
Chu
Chi-Fon
CF
Chang
Tai-Huang
TH
Huang
D004867:Equipment Design; D019544:Equipment Failure Analysis; D009682:Magnetic Resonance Spectroscopy / Q000295:instrumentation*; D055617:Micro-Electrical-Mechanical Systems / Q000295:instrumentation*; D008846:Micromanipulation / Q000295:instrumentation*; D008904:Miniaturization; D012680:Sensitivity and Specificity; D013048:Specimen Handling / Q000295:instrumentation*