Wednesday, January 16, 2019

Determining Cholesterol Binding to Membrane Proteins by Cholesterol 13C Labeling in Yeast and Dynamic Nuclear Polarization NMR #DNPNMR

Elkins, Matthew R, Ivan V Sergeyev, and Mei Hong. “Determining Cholesterol Binding to Membrane Proteins by Cholesterol 13C Labeling in Yeast and Dynamic Nuclear Polarization NMR.” Journal of the American Chemical Society, 2018, 15437–15449. 

We present a general strategy for determining the cholesterol-binding site of eukaryotic membrane proteins in native-like lipid membranes by NMR spectroscopy. The strategy combines yeast biosynthetic 13C enrichment of cholesterol with detection of protein-cholesterol 13C-13C cross peaks in 2D correlation NMR spectra under the dynamic nuclear polarization (DNP) condition. Low-temperature DNP not only allows high-sensitivity detection of weak protein cholesterol cross peaks in 2D spectra but also immobilizes cholesterol and protein to enable intermolecular distance measurements. We demonstrate this approach on the influenza M2 protein, which utilizes cholesterol to conduct membrane scission in the last step of virus budding and release from the host cell plasma membrane. A 13C-13C double-quantum filter was employed to significantly simplify the 2D 13C-13C correlation spectra and facilitate the identification of protein-cholesterol cross peaks. A number of cross peaks between the M2 transmembrane residues’ sidechains and the cholesterol sterol group were detected, which complement recently measured protein contacts to the isooctyl tail of cholesterol to define an extended binding interface. These results provide atomic-level evidence of M2-cholesterol interaction to cause membrane curvature and scission, and the approach is generally applicable to other eukaryotic membrane proteins for understanding the influence of cholesterol on membrane protein function.

Monday, January 14, 2019

Efficient Hyperpolarization of U- 13C-Glucose Using Narrow-Line UV-Generated Labile Free Radicals #DNPNMR

DNP requires a paramagnetic polarizing agent. This is great for DNP but not so great for the NMR experiment, since the paramagnetic species often causes line broadening due to increase nuclear relaxation. To decrease the unwanted relaxation enhancement some researchers suggested to remove (e.g. filter out) the paramagnetic species after the dissolution step.

The article describes an elegant method, using UV generated radicals for polarization at low temperatures, which recombine once the sample is heated up during the dissolution process, effectively removing the paramagnetic enhanced relaxation process.

Capozzi, Andrea, Saket Patel, Christine Pepke Gunnarsson, Irene Marco-Rius, Arnaud Comment, Magnus Karlsson, Mathilde H. Lerche, Olivier Ouari, and Jan Henrik Ardenkjaer-Larsen. “Efficient Hyperpolarization of U- 13C-Glucose Using Narrow-Line UV-Generated Labile Free Radicals.” Angewandte Chemie, December 20, 2018.

Free radicals generated via irradiation with UV-light of a frozen solution containing a fraction of pyruvic acid (PA), have demonstrated their dissolution Dynamic Nuclear Polarization (dDNP) potential providing up to 30% [1-13C]PA liquid-state polarization. Moreover, their labile nature has proven to pave a way to nuclear polarization storage and transport. Herein, differently from the case of PA, we tackled the issue of providing dDNP UV-radical precursors, trimethylpyruvic acid (TriPA) and its methyl-deuterated form d9-TriPA, not involved in any metabolic pathway. The 13C dDNP performance was evaluated for hyperpolarization of [U-13C6,1,2,3,4,5,6,6-d7]-Dglucose. The generated UV-radical proved to be a versatile and highly efficient polarizing agent providing, after dissolution and transfer (10 s), a 13C liquid-state polarization up to 32%.

Friday, January 11, 2019

Recent advances in solid-state nuclear magnetic resonance spectroscopy of exotic nuclei #DNPNMR

Leroy, César, and David L. Bryce. “Recent Advances in Solid-State Nuclear Magnetic Resonance Spectroscopy of Exotic Nuclei.” Progress in Nuclear Magnetic Resonance Spectroscopy 109 (December 2018): 160–99.

We present a review of recent advances in solid-state nuclei nuclear magnetic resonance (SSNMR) studies of exotic nuclei. Exotic nuclei may be spin-1/2 or quadrupolar, and typically have low gyromagnetic ratios, low natural abundances, large quadrupole moments (when I > 1/2) , or some combination of these properties, generally resulting in low receptivities and/or prohibitively broad line widths. Some nuclides are little studied for other reasons, also rendering them somewhat exotic. We first discuss some of the recent progress in pulse sequences and hardware development which continues to enable researchers to study new kind of materials as well as previously unfeasible nuclei. This is followed by a survey of applications to a wide range of exotic nuclei (including e.g., 9Be, 25Mg, 33S, 39K, 43Ca, 47/49Ti, 53Cr, 59Co, 61Ni, 67Zn, 73Ge, 75As, 87Sr, 115In, 119Sn, 121/123Sb, 135/137Ba, 185/187Re, 209Bi) , most of them quadrupolar. The scope of the review is the past ten years, i.e., 2007 – 2017

Thursday, January 10, 2019

[NMR] PhD position in NMR crystallography #DNPNMR

A PhD position is available to join the Emsley group at EPFL, Lausanne

We are looking for highly motivated candidates to take up a PhD position developing new methods in NMR spectroscopy to address the challenging problem of atomic-level structure determination in chemistry and materials science. In particular we will be working on dynamic nuclear polarization enhanced NMR methods for materials. Examples of our recent work and the application areas that we work on can be found on our website:

We are looking for highly motivated candidates with strong scientific background, independence, and who enjoy teamwork. You should hold a relevant qualification in chemistry, physics or related disciplines. Skills in developing experimental multi-dimensional nuclear magnetic resonance are a plus.

Our laboratory at EPFL is part of one the world’s leading chemistry departments, and is located Lausanne on the north shore of Lake Geneva. The laboratory is equipped with unique state of the art NMR spectrometers (including gyrotron DNP accessories at 400 and 900 MHz, a dissolution-DNP machine, and 100 kHz magic angle spinning probes).

Motivated candidates should contact Lyndon Emsley with a CV by email at Applications will be reviewed from 1st February onwards, until the position is filled. 
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[NMR] parahydrogen-hyperpolarization: PhD student position available at MOIN CC in Kiel, Germany.

Dear colleagues!

the molecular imaging north competence center (MOIN CC) in Kiel, Germany, is looking for a PhD student in the area of parahydrogen hyperpolarization for MRI and NMR.

The PhD position is part of the DFG-funded research training circle 2154 "materials for brain" and more information (will be) available on

Candidates with a physics and engineering background are particularly encouraged to apply. The salary is quite competitive (and the research is excellent!).

Please inquire and apply via email at

Merry Christmas!

Prof. Dr. Jan-Bernd Hövener

Head, Section Biomedical Imaging and MOIN CC
Head, Emmy Noether Group Molecular and Metabolic MRI - M3

Section Biomedical Imaging, MOIN CC
Am Botanischen Garten 14
D-24118 Kiel

phone: +49 (0) 431 880-5832
fax: +49 (0) 431 880-5852

Office UKSH
Building 522, Room 107
phone: +49 (0) 431 500 16 600

Office Freiburg
Breisacher Straße 60a,
D-79106 Freiburg
phone: +49 (0) 761 270-93910



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[NMR] Postdoc and PhD positions in MAS-DNP / Solid State NMR at the Weizmann Institute of Science #DNPNMR

Several positions are available for postdoctoral researchers and PhD candidates in the group of Michal Leskes at the Department of Materials and Interfaces, Weizmann Institute of science.

The projects, funded by the ERC, include the development of paramagnetic metal ion dopants as endogenous polarization agents for MAS-DNP and application of this approach in the study of energy storage and conversion materials. 

Our lab is equipped with a Bruker 400MHz MAS-DNP spectrometer with LT-DNP MAS probes, as well as a wide range of MAS and static solids NMR probes. In addition to our lab dedicated equipment, extensive NMR and EPR systems are available on campus as part of our research support facilities – these include 400, 500 and 800MHz NMR spectrometers equipped with MAS systems and X and Q band pulse and CW EPR systems. 

Required background for postdoctoral positions: PhD in Chemistry/Physics with extensive hands-on experience in solid state NMR/DNP/EPR. Experience in spin dynamics simulations and/or DFT calculations is an advantage as well experience in materials science.

For PhD applications: BSc and MSc (or equivalent) in Chemistry/Physics/Materials science and engineering are required.

Candidates should have excellent communication skills in English.

Further details on PhD studies and the postdoctoral fellowships can be found here:

The Weizmann Institute is located in a small, affordable and friendly town, 25 minutes from Tel Aviv and 45 minutes from Jerusalem, and is one of Israel's premier scientific institutions. It is a research centre where the official language is English, and which offers numerous facilities to international visitors, including furnished apartments for postdocs.

For additional information and application please contact Michal Leskes by email at

Applications should include CV, list of publications and contact details of two references.

Further details and relevant publications can be found on our website:

Dr. Michal Leskes
Department of Materials and Interfaces
Weizmann Institute of Science
Rehovot 7610001
Office: +972-8-934-2588
NMR Lab: +972-8-934-2424
Mobile: +972-544224001

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Wednesday, January 9, 2019

Oxygen-induced leakage of spin polarization in Overhauser-enhanced magnetic resonance imaging: Application for oximetry in tumors #DNPNMR

Gorodetskii, Artem A., Timothy D. Eubank, Benoit Driesschaert, Martin Poncelet, Emily Ellis, Valery V. Khramtsov, and Andrey A. Bobko. “Oxygen-Induced Leakage of Spin Polarization in Overhauser-Enhanced Magnetic Resonance Imaging: Application for Oximetry in Tumors.” Journal of Magnetic Resonance 297 (December 2018): 42–50.

Overhauser-enhanced Magnetic Resonance Imaging (OMRI) is a double resonance technique applied for oxygen imaging in aqueous samples and biological tissues. In this report, we present an improved OMRI approach of oxygen measurement using the single line ‘‘Finland” trityl spin probe. Compared to a traditional approach, we introduced an additional mechanism of leakage of spin polarization due to an interaction of a spin system with oxygen. The experimental comparison of the new approach with an oxygendependent leakage factor to a traditional approach performed in phantom samples in vitro, and mouse tumor model in vivo, shows improved accuracy of determination of oxygen and contrast agent concentrations.

Monday, January 7, 2019

Influence of 13C Isotopic Labeling Location on Dynamic Nuclear Polarization of Acetate #DNPNMR

Niedbalski, Peter, Christopher Parish, Andhika Kiswandhi, Zoltan Kovacs, and Lloyd Lumata. “Influence of 13C Isotopic Labeling Location on Dynamic Nuclear Polarization of Acetate.” The Journal of Physical Chemistry A 121, no. 17 (May 4, 2017): 3227–33.

Dynamic nuclear polarization (DNP) via the dissolution method has alleviated the insensitivity problem in liquid-state nuclear magnetic resonance (NMR) spectroscopy by amplifying the signals by several thousand-fold. This NMR signal amplification process emanates from the microwavemediated transfer of high electron spin alignment to the nuclear spins at high magnetic field and cryogenic temperature. Since the interplay between the electrons and nuclei is crucial, the chemical composition of a DNP sample such as the type of free radical used, glassing solvents, or the nature of the target nuclei can significantly affect the NMR signal enhancement levels that can be attained with DNP. Herein, we have investigated the influence of 13C isotopic labeling location on the DNP of a model 13C compound, sodium acetate, at 3.35 T and 1.4 K using the narrow electron spin resonance (ESR) line width free radical trityl OX063. Our results show that the carboxyl 13C spins yielded about twice the polarization produced in methyl 13C spins. Deuteration of the methyl 13C group, while proven beneficial in the liquid-state, did not produce an improvement in the 13C polarization level at cryogenic conditions. In fact, a slight reduction of the solid-state 13C polarization was observed when 2H spins are present in the methyl group. Furthermore, our data reveal that there is a close correlation between the solid-state 13C T1 relaxation times of these samples and the relative 13C polarization levels. The overall results suggest the achievable solid-state polarization of 13C acetate is directly affected by the location of the 13C isotopic labeling via the possible interplay of nuclear relaxation leakage factor and cross-talks between nuclear Zeeman reservoirs in DNP.

Wednesday, January 2, 2019

Dynamic Nuclear Polarization of Metal–Organic Frameworks Using Photoexcited Triplet Electrons #DNPNMR

Fujiwara, Saiya, Masanori Hosoyamada, Kenichiro Tateishi, Tomohiro Uesaka, Keiko Ideta, Nobuo Kimizuka, and Nobuhiro Yanai. “Dynamic Nuclear Polarization of Metal–Organic Frameworks Using Photoexcited Triplet Electrons.” Journal of the American Chemical Society 140, no. 46 (November 21, 2018): 15606–10.

While dynamic nuclear polarization based on photoexcited triplet electrons (triplet-DNP) has the potential to hyperpolarize nuclear spins of target substrates in the low magnetic field at room temperature, there has been no triplet-DNP system offering structural rigidity and substrate accessibility. Here, we report the first example of triplet-DNP of nanoporous metal−organic frameworks. Accommodation of a carboxylate-modified pentacene derivative in a partially deuterated ZIF-8 (DZIF-8) results in a clear 1H NMR signal enhancement over thermal equilibrium.