Abstract
Field-dependent NMR studies of bio-molecular systems using a sample shuttling hardware operating on a high-field NMR apparatus have provided valuable structural and dynamic information. We have recently published a design of a compact sample transportation device, called “field-cycler”, which was installed in a commercial spectrometer and which provided highly precise positioning and stability during high speed shuttling. In this communication, we demonstrate the first use of a sample shuttling device on a commercial high field standard bore NMR spectrometer, equipped with a commercial triple resonance cryogenically cooled NMR probe. The performance and robustness of the hardware operating in 1D and 2D field cycling experiments, as well as the impact of the sample shuttling time on the signal intensity are discussed.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
References
Akasaka K, Ishima R, Shibata S (1990) Proton spin relaxation in biopolymers at high magnetic fields. Phys B Condens Matter 164:163–179
Akke M, Skelton NJ, Kordel J, Palmer AG, Chazin WJ (1993) Effects of ion binding on the backbone dynamics of calbindin D9 k determined by nitrogen-15 NMR relaxation. Biochemistry 32:9832–9844
Arthur G, Palmer WJF III, Cavanagh John, Sketon Nicholas J, Rance Mark (2006) Protein NMR spectroscopy: principles and practice, 2nd edn. Academic Press Inc, Cambridge
Black RD, Early TA, Roemer PB, Mueller OM, Mogrocampero A, Turner LG, Johnson GA (1993) A high-temperature superconducting receiver for nuclear-magnetic-resonance microscopy. Science 259:793–795
Charlier C et al (2013) Nanosecond time scale motions in proteins revealed by high-resolution NMR relaxometry. J Am Chem Soc 135:18665–18672
Chou CY, Chu M, Chang CF, Huang TH (2012) A compact high-speed mechanical sample shuttle for field-dependent high-resolution solution NMR. J Magn Reson 214:302–308
Chou C-Y, Ferrage F, Aubert G, Sakellariou D (2015) Simple method for the generation of multiple homogeneous field volumes inside the bore of superconducting magnets. Sci Rep 5:12200
Clarkson MW, Lei M, Eisenmesser EZ, Labeikovsky W, Redfield A, Kern D (2009) Mesodynamics in the SARS nucleocapsid measured by NMR field cycling. J Biomol NMR 45:217–225
Farrow NA et al (1994) Backbone dynamics of a free and a phosphopeptide-complexed Src homology 2 domain studied by 15 N NMR relaxation. Biochemistry 33:5984–6003
Grosse S, Gubaydullin F, Scheelken H, Vieth HM, Yurkovskaya AV (1999) Field cycling by fast NMR probe transfer: design and application in field-dependent CIDNP experiments. Appl Magn Reson 17:211–225
Kimmich R, Anoardo E (2004) Field-cycling NMR relaxometry. Prog Nucl Magn Reson Spectrosc 44:257–320
Kovacs H, Moskau D, Spraul M (2005) Cryogenically cooled probes—a leap in NMR technology. Prog Nucl Magn Reson Spectrosc 46:131–155
Krahn A et al (2010) Shuttle DNP spectrometer with a two-center magnet. Phys Chem Chem Phys 12:5830–5840
Noack F (1986) NMR field-cycling spectroscopy—Principles and applications. Prog Nucl Magn Reson Spectrosc 18:171–276
Nusser W, Kimmich R (1990) Protein backbone fluctuations and NMR field-cycling relaxation spectroscopy. J Phys Chem-Us 94:5637–5639
Redfield AG (2003) Shuttling device for high-resolution measurements of relaxation and related phenomena in solution at low field, using a shared commercial 500 MHz NMR instrument. Magn Reson Chem 41:753–768
Redfield A (2012) High-resolution NMR field-cycling device for full-range relaxation and structural studies of biopolymers on a shared commercial instrument. J Biomol NMR 52:159–177
Reese M et al (2008) Construction of a liquid-state NMR DNP shuttle spectrometer: first experimental results and evaluation of optimal performance characteristics. Appl Magn Reson 34:301–311
Roberts MF, Redfield AG (2004a) High-resolution P-31 field cycling NMR as a probe of phospholipid dynamics. J Am Chem Soc 126:13765–13777
Roberts MF, Redfield AG (2004b) Phospholipid bilayer surface configuration probed quantitatively by P-31 field-cycling NMR. Proc Natl Acad Sci USA 101:17066–17071
Roberts MF, Cui Q, Turner CJ, Case DA, Redfield AG (2004) High-resolution field-cycling NMR studies of a DNA octamer as a probe of phosphodiester dynamics and comparison with computer simulation. Biochemistry 43:3637–3650
Styles P, Soffe NF, Scott CA, Crag DA, Row F, White DJ, and White PCJ (1984) A high-resolution NMR probe in which the coil and preamplifier are cooled with liquid helium. J Magn Reson 60:397–404
Swanson SD, Kennedy SD (1993) A sample-shuttle nuclear-magnetic-relaxation-dispersion spectrometer. J Magn Reson Ser A 102:375–377
Thakur CS, Luo Y, Chen B, Eldho NV, Dayie TK (2012) Biomass production of site selective 13C/15 N nucleotides using wild type and a transketolase E. coli mutant for labeling RNA for high resolution NMR. J Biomol NMR 52:103–114
Wagner S, Dinesen TR, Rayner T, Bryant RG (1999) High-resolution magnetic relaxation dispersion measurements of solute spin probes using a dual-magnet system. J Magn Reson 140:172–178
Yanagisawa Y et al (2008) Towards beyond-1 GHz solution NMR: internal 2H lock operation in an external current mode. J Magn Reson 192:329–337
Acknowledgments
We greatly acknowledge Dr. Sophie Zinn-Justin (CEA) for stimulating discussions and for allowing us access to the 700 MHz spectrometer, Dr. Nikolas Birlirakis (ENS) for useful comments on the manuscript and Dr. F. Ferrage (ENS) for comments and suggestions. We would like to give the special acknowledgement to Dr. Jan Marchant and the labs of Prof. Michael F. Summers and Prof. Kwaku T. Dayie in Maryland University, USA, for the UUCG tetra-loop RNA sample preparation. We also thank Mr. Angelo Guiga and the staffs in the Academia Sinica Machine Shop, Taiwan, especially Mr. Cherng-Yin Lin, for the production of the high-precision hardware. This work is supported by ERC grants 2F4BIODYN and R-EVOLUTION-M-R (StG 205119), ANR DYN-IDP in France, and NSC 102-2113-M-001-010 from The National Science Council, The Republic of China.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Chou, CY., Chu, M., Chang, CF. et al. High sensitivity high-resolution full range relaxometry using a fast mechanical sample shuttling device and a cryo-probe. J Biomol NMR 66, 187–194 (2016). https://doi.org/10.1007/s10858-016-0066-5
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10858-016-0066-5