A compact high-speed mechanical sample shuttle for field-dependent high-resolution solution NMR

Ching Yu Chou, Minglee Chu, Chi Fon Chang, Tai Huang Huang

Research output: Contribution to journalArticle

16 Citations (Scopus)

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 languageEnglish
Pages (from-to)302-308
Number of pages7
JournalJournal of Magnetic Resonance
Volume214
DOIs
Publication statusPublished - 2012 Jan 1

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

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