Publication date: Available online 11 April 2015 Source:Journal of Magnetic Resonance
Author(s): Aaron W. Kittell , James S. Hyde
Non-adiabatic rapid passage (NARS) electron paramagnetic resonance (EPR) spectroscopy was introduced by Kittell, A.W., Camenisch, T.G., Ratke, J.J. Sidabras, J.W., Hyde, J.S., 2011 as a general purpose technique to collect the pure absorption response. The technique has been used to improve sensitivity relative to sinusoidal magnetic field modulation, increase the range of inter-spin distances that can be measured under near physiological conditions [Kittell, A.W., Hustedt, E.J., Hyde, J.S., 2012], and enhance spectral resolution in copper (II) spectra [Hyde, J.S., Bennett, B., Kittell, A.W., Kowalski, J.M., Sidabras, J.W., 2013]. In the present work, the method is extended to CW microwave power saturation of spin-labeled T4 Lysozyme (T4L). As in the cited papers, rapid triangular sweep of the polarizing magnetic field was superimposed on slow sweep across the spectrum. Adiabatic rapid passage (ARP) effects were encountered in samples undergoing very slow rotational diffusion as the triangular magnetic field sweep rate was increased. The paper reports results of variation of experimental parameters at the interface of adiabatic and non-adiabatic rapid sweep conditions. Comparison of the forward (up) and reverse (down) triangular sweeps is shown to be a good indicator of the presence of rapid passage effects. Spectral turning points can be distinguished from spectral regions between turning points in two ways: differential microwave power saturation and differential passage effects. Oxygen accessibility data are shown under NARS conditions that appear similar to conventional field modulation data. However, the sensitivity is much higher, permitting, in principle, experiments at substantially lower protein concentrations. Spectral displays were obtained that appear sensitive to rotational diffusion in the range of rotational correlation times of 10-3 to 10-7 s in a manner that is analogous to saturation transfer spectroscopy. Graphical abstract
Journal Highlight: Rapid assessment of the illegal presence of 1,3-dimethylamylamine (DMAA) in sports nutrition and dietary supplements using 1H NMR spectroscopy
Journal Highlight: Rapid assessment of the illegal presence of 1,3-dimethylamylamine (DMAA) in sports nutrition and dietary supplements using 1H NMR spectroscopy
http://www.spectroscopynow.com/common/images/thumbnails/14898526bb5.jpgA proton NMR method was developed and validated for measuring 1,3-dimethylamylamine in sports nutrition and dietary supplements and is recommended for routine use in food testing, customs or doping control laboratories.
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http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja306813j/aop/images/medium/ja-2012-06813j_0004.gif
Journal of the American Chemical Society
DOI: 10.1021/ja306813j
http://feeds.feedburner.com/~ff/acs/jacsat?d=yIl2AUoC8zA
http://feeds.feedburner.com/~r/acs/jacsat/~4/eCGR552L3hw
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[Question from NMRWiki Q&A forum] adiabatic decoupling
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Hi NMRwikiers, for measuring scalar couplings we use some HSQC pulse sequences modified for obtaining the coupling in F1-dimension as a splitting of doublets for CH2 groups. As high resolution is needed we use high folding in the acqusition, but as a result we obtain a lot of coupling artifacts in phenyl signals. We think that the use of adiabatic decoupling schemes should give a reasonably good spectrum of phenyls but I have no experience in adiabatic decoupling. Anyone can give me a hand for Bruker spectrometers?
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Spin-Label CW Microwave Power Saturation and Rapid Passage with Triangular Non-Adiabatic Rapid Sweep (NARS) and Adiabatic Rapid Passage (ARP) EPR Spectroscopy
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