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

Chou, Ching Yu; Chu, M. L.; Chang, Chi‐Fon; Huang, Tai Huang

doi:10.1016/j.jmr.2011.12.001

Cited by 32 publications

(70 citation statements)

References 34 publications

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“…A high speed sample shuttling instrument, named field-cycler, based on the design of Chou et al 23. was installed to a 500 MHz wide-bore superconducting magnet equipped with a 5-mm broadband homebuilt radio-frequency probe-head.…”

Section: Methodsmentioning

confidence: 99%

“…Here we use our rapid mechanical sample-shuttling device for performing T 1 relaxation measurements covering an ultra-wide range of magnetic fields in a virtually continuous fashion2327. We demonstrate the high reliability of the measurements by observing the equilibrium magnetization of newly designed mixed Gd-Eu vanadate nanoparticles at different magnetic fields and perform a field-dependent study of T 1 relaxation on three different nanoparticle compositions and sizes.…”

mentioning

confidence: 99%

“…An alternative approach to the use of pulsed magnetic fields for NMRD studies, is the use of rapid sample translation between positions in the stray magnetic field produced by the NMR magnet20212223. This approach offers the possibility to reach a wider range of magnetic fields, which can cover the entire span between the field values at the center of the magnet and virtually a null magnetic field.…”

mentioning

confidence: 99%

“…The major disadvantage lies however in the significantly longer time that the sample requires in order to travel between the locations of pre-polarization, relaxation and detection which can be of the order of several hundreds of milliseconds. Rapid sample shuttling is achieved using pneumatic212425, or mechanic technologies202223. Mechanical technologies are much more versatile and precise and can be easily used with standard NMR hardware as we recently demonstrated in the area of bio-molecular high-resolution fast field cycling relaxometry222326.…”

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confidence: 99%

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Ultra-wide range field-dependent measurements of the relaxivity of Gd1−xEuxVO4 nanoparticle contrast agents using a mechanical sample-shuttling relaxometer

Chou

Abdesselem

Bouzigues

et al. 2017

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The current trend for Magnetic Resonance Imaging points towards higher magnetic fields. Even though sensitivity and resolution are increased in stronger fields, T1 contrast is often reduced, and this represents a challenge for contrast agent design. Field-dependent measurements of relaxivity are thus important to characterize contrast agents. At present, the field-dependent curves of relaxivity are usually carried out in the field range of 0 T to 2 T, using fast field cycling relaxometers. Here, we employ a high-speed sample shuttling device to switch the magnetic fields experienced by the nuclei between virtually zero field, and the center of any commercial spectrometer. We apply this approach on rare-earth (mixed Gadolinium-Europium) vanadate nanoparticles, and obtain the dispersion curves from very low magnetic field up to 11.7 T. In contrast to the relaxivity profiles of Gd chelates, commonly used for clinical applications, which display a plateau and then a decrease for increasing magnetic fields, these nanoparticles provide maximum contrast enhancement for magnetic fields around 1–1.5 T. These field-dependent curves are fitted using the so-called Magnetic Particle (MP) model and the extracted parameters discussed as a function of particle size and composition. We finally comment on the new possibilities offered by this approach.

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Section: Methodsmentioning

confidence: 99%

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confidence: 99%

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confidence: 99%

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confidence: 99%

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Ultra-wide range field-dependent measurements of the relaxivity of Gd1−xEuxVO4 nanoparticle contrast agents using a mechanical sample-shuttling relaxometer

Chou

Abdesselem

Bouzigues

et al. 2017

Sci Rep

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“…10,11 Relaxometry can be reconciled with high-resolution high-field NMR by rapidly “shuttling” the sample from high to low field and back. 12−14 Slower shuttling has allowed fruitful studies of slowly relaxing phosphorus-31 and carbon-13 nuclei in lipids, 15 but relaxation of nitrogen-15 in proteins is so fast at low fields that the shuttling must be carried out very rapidly. To the best of our knowledge, there is only one pioneering study, 16 albeit shuttling was limited to a fairly narrow range of magnetic fields (down to 4 T).…”

Section: Introductionmentioning

confidence: 99%

Nanosecond Time Scale Motions in Proteins Revealed by High-Resolution NMR Relaxometry

et al. 2013

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Understanding the molecular determinants underlying protein function requires the characterization of both structure and dynamics at atomic resolution. Nuclear relaxation rates allow a precise characterization of protein dynamics at the Larmor frequencies of spins. This usually limits the sampling of motions to a narrow range of frequencies corresponding to high magnetic fields. At lower fields one cannot achieve sufficient sensitivity and resolution in NMR. Here, we use a fast shuttle device where the polarization builds up and the signals are detected at high field, while longitudinal relaxation takes place at low fields 0.5 < B0 < 14.1 T. The sample is propelled over a distance up to 50 cm by a blowgun-like system in about 50 ms. The analysis of nitrogen-15 relaxation in the protein ubiquitin over such a wide range of magnetic fields offers unprecedented insights into molecular dynamics. Some key regions of the protein feature structural fluctuations on nanosecond time scales, which have so far been overlooked in high-field relaxation studies. Nanosecond motions in proteins may have been underestimated by traditional high-field approaches, and slower supra-τc motions that have no effect on relaxation may have been overestimated. High-resolution relaxometry thus opens the way to a quantitative characterization of nanosecond motions in proteins.

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Recovering Invisible Signals by Two‐Field NMR Spectroscopy

et al. 2016

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Nuclear magnetic resonance (NMR) studies have benefited tremendously from the steady increase in the strength of magnetic fields.Spectacular improvements in both sensitivity and resolution have enabled the investigation of molecular systems of rising complexity.A tv ery high fields,t his progress may be jeopardized by line broadening, whichi sd ue to chemical exchange or relaxation by chemical shift anisotropy. In this work, we introduce at wo-field NMR spectrometer designed for both excitation and observation of nuclear spins in two distinct magnetic fields in as ingle experiment. NMR spectra of several small molecules as well as ap rotein were obtained, with two dimensions acquired at vastly different magnetic fields.R esonances of exchanging groups that are broadened beyond recognition at high field can be sharpened to narrow peaks in the low-field dimension. Tw o-field NMR spectroscopye nables the measurement of chemical shifts at optimal fields and the study of molecular systems that suffer from internal dynamics,a nd opens new avenues for NMR spectroscopya tv ery high magnetic fields.

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

Cited by 32 publications

References 34 publications

Ultra-wide range field-dependent measurements of the relaxivity of Gd1−xEuxVO4 nanoparticle contrast agents using a mechanical sample-shuttling relaxometer

Ultra-wide range field-dependent measurements of the relaxivity of Gd1−xEuxVO4 nanoparticle contrast agents using a mechanical sample-shuttling relaxometer

Nanosecond Time Scale Motions in Proteins Revealed by High-Resolution NMR Relaxometry

Recovering Invisible Signals by Two‐Field NMR Spectroscopy

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