Friday, September 30, 2016

Molecular Rationale for Improved Dynamic Nuclear Polarization of Biomembranes

Smith, A.N., et al., Molecular Rationale for Improved Dynamic Nuclear Polarization of Biomembranes. J Phys Chem B, 2016. 120(32): p. 7880-8.

Dynamic nuclear polarization (DNP) enhanced solid-state NMR can provide orders of magnitude in signal enhancement. One of the most important aspects of obtaining efficient DNP enhancements is the optimization of the paramagnetic polarization agents used. To date, the most utilized polarization agents are nitroxide biradicals. However, the efficiency of these polarization agents is diminished when used with samples other than small molecule model compounds. We recently demonstrated the effectiveness of nitroxide labeled lipids as polarization agents for lipids and a membrane embedded peptide. Here, we systematically characterize, via electron paramagnetic (EPR), the dynamics of and the dipolar couplings between nitroxide labeled lipids under conditions relevant to DNP applications. Complemented by DNP enhanced solid-state NMR measurements at 600 MHz/395 GHz, a molecular rationale for the efficiency of nitroxide labeled lipids as DNP polarization agents is developed. Specifically, optimal DNP enhancements are obtained when the nitroxide moiety is attached to the lipid choline headgroup and local nitroxide concentrations yield an average e(-)-e(-) dipolar coupling of 47 MHz. On the basis of these measurements, we propose a framework for development of DNP polarization agents optimal for membrane protein structure determination.

Thursday, September 29, 2016

Two Research Fellow positions and one PhD studentship at University of Southampton #DNPNMR

From the Ampere Magnetic Resonance List

Dear Colleagues,

I have two open Reserach Fellow Positions and a fully funded PhD studentship in my group ( at the University of Southampton.

* Post-Doctoral Research Fellowship in nuclear magnetic resonance in the research group of Dr Giuseppe Pileio, in collaboration with Prof Malcolm H Levitt. The project, funded by EPSRC(UK), concerns the development of NMR hardware and methodology that combines supercritical fluids with long-lived states NMR and dissolution-DNP to prolong the storage of hyperpolarised spin order and allow it to be transported remotely from the production site. The position is tenable from 1 December 2016 or as soon as possible thereafter with initial appointment for 2 years but with the possibility of a further extension of 1 more years, subject to project requirements. For further details and how to apply please follow this link:

* A 3 years PhD studentship is also available on the same project with application deadline 31 October 2016 and a salary of £14,296 per annum. For further details and how to apply please follow this link: . Please note that: due to funding restrictions this position is only open to UK/EU applicants

* Post-Doctoral Research Fellowship in nuclear magnetic resonance in the research group of Dr Giuseppe Pileio. The project, funded by EPSRC under the First Grant scheme, concerns the development of NMR methodology to probe translational dynamics in porous media by singlet-state NMR spectroscopy. The position is tenable from 1 November 2016 or as soon as possible thereafter with appointment for 1 year but with the possibility of a further extension of 1 more year, subject to funding and project requirements. For further details and how to apply please follow this link:

University of Southampton is a UK Russell Group university positioned in the top 1% of world universities according to QS World University Rankings. We have an international reputation for research, teaching and enterprise activities. Southampton is particularly well known for its magnetic resonance and computational chemistry research.

Many Thanks,
Dr. Giuseppe Pileio, PhD

Lecturer in Physical Chemistry,
Department of Chemistry,
Building 27 - Room 2059,
University of Southampton,
University Road, SO17 1BJ,
Internal Post Code: M16,
Southampton, Hampshire, UK.

Tel.: +44 (023) 80 59 4160
ORCID: 0000-0001-9223-3896

This is the AMPERE MAGNETIC RESONANCE mailing list:

NMR web database:

Wednesday, September 28, 2016

Filterable Agents for Hyperpolarization of Water, Metabolites, and Proteins

Vuichoud, B., et al., Filterable Agents for Hyperpolarization of Water, Metabolites, and Proteins. Chemistry, 2016: p. n/a-n/a.

Hyperpolarization is generated by dissolution dynamic nuclear polarization (d-DNP) using a polymer-based polarizing agent dubbed FLAP (filterable labeled agents for polarization). It consists of a thermo-responsive poly(N-isopropylacrylamide), also known as pNiPAM-COOH, labeled with nitroxide radicals. The polymer powder is impregnated with an arbitrary solution of interest and frozen as is. Dissolution is followed by a simple filtration, leading to hyperpolarized solutions free from any contaminants. We demonstrated the use of FLAP to hyperpolarize partially deuterated water up to P(1 H)=6 % with a long relaxation T1 >36 s characteristic of high purity. Water hyperpolarization can be transferred to drugs, metabolites, or proteins that are waiting in an NMR spectrometer, either by exchange of labile protons or through intermolecular Overhauser effects. We also show that FLAPs are suitable polarizing agents for 13 C-labeled metabolites such as pyruvate, acetate, and alanine.

Tuesday, September 27, 2016

IVAN (International Varian-Agilent NMR users group) Introduction

Introduction of IVAN

The International Varian-Agilent NMR users group sponsored by MR Resources.

MR Resources is pleased to announce the formation of a new international organization directed toward owners and users of NMR spectrometers from Varian Inc. and Agilent Technologies Inc.

As we all know, on October 14, 2014 Agilent Technologies Inc., owner of the former NMR division of Varian Inc., exited the NMR business. As a result, during the two years since, MR Resources has greatly increased its service and support commitment to Varian-Agilent NMR owners and users, welcoming many new customers in the process. MR Resources is fully dedicated to helping support the approximately 5,500 Varian-Agilent NMR spectrometers that remain in use worldwide. We hope that MR Resources will be the new home for all Varian-Agilent NMR spectrometer owners and users worldwide.

As such, to further increase our on-going commitment to Varian-Agilent NMR users, MR Resources will provide full and exclusive sponsorship for the IVAN Users Group. The purpose of the group will be to facilitate on-going technical support of the International Varian-Agilent NMR spectrometer user community by fostering interactive information exchange and face-to-face meetings of users. We wish to provide a much needed home base and platform for meetings, communications and other activities for owners and users of Varian-Agilent NMR spectrometers. MR Resources and IVAN are not affiliated with Agilent Technologies Inc. or Varian Inc. in any way.

The IVAN Users Group is now officially active, and to start things off MR Resources will sponsor a series of informative and interactive meetings for Varian-Agilent NMR users locally, regionally and in conjunction with NMR conferences. The IVAN meetings will take place in different locations around the world. Locations for meetings will be determined by the needs of users. Please indicate on the membership sign-up form if you would like to participate in an organization in your area. These meetings will be exclusive to IVAN User Group members and will be free of charge to attend. These meetings will bring together owners, customers and users, along with MR Resources personnel and many highly committed former Varian-Agilent experts. Indeed, the IVAN Executive Committee is comprised of a "Who's Who" from the Varian-Agilent NMR companies and the NMR community at large. Our first meeting will be in San Jose, California at the Fairmont Hotel on Friday October 28, 2016. We are also planning a subsequent full day meeting to accompany the Asilomar ENC in the spring of 2017 to be held the Saturday before the ENC opening.

If you are an owner of a Varian-Agilent NMR spectrometer or an interested user, you are invited to join IVAN and attend our meetings, as well as participate in other activities that will soon be developed. Select Join IVAN and fill out the membership form. We urge as many Varian-Agilent NMR spectrometer owners and users worldwide to join this very important group in order to ensure continuing operation and longevity of the Varian-Agilent NMR systems that we all have such a huge investment in.


Membership in IVAN is available to all Varian-Agilent NMR spectrometer owners and interested users, independent of your service plan or status as a MR Resources customer. There is no charge to become a member or to participate in meetings and activities. There are some restrictions on membership for those who do not identify as a direct Varian-Agilent NMR end-user site and for those that are NMR Vendors. MR Resources intends its own commercial involvement in the user group to be low key. The success of the IVAN user group depends upon the activities of its members. The role of MR Resources is to provide a home for meetings and communication. An email link is available on the membership form to contact us directly with questions about membership.

The on-going objectives for IVAN will be those of its users to enhance the usefulness of their NMR systems, extend the lifetime of the instruments, and to keep them running properly.

First IVAN Meeting, Fall 2016

We invite you to attend a kick-off meeting for IVAN in the San Francisco Bay Area on Friday October 28, 2016. The meeting will be one day – 10:00 AM to 3:30 PM at the Fairmont Hotel in San Jose, including lunch and followed by a "Happy Hour" at the Fairmont. Once you join IVAN you may select Our First Meeting in San Jose to register for the upcoming user meeting.

We have a large conference room and catering arranged for up to 100 individuals. Space is limited so sign up early! We hope to see many of you from the Bay Area and we make a special invitation to users from the US West Coast and further distances as well. We promise that you will not be disappointed and hope you can make it if possible! If not, a meeting the day before ENC in Monterey, California is in planning, and other local meetings are already under discussion.

Agenda for the Founding San Jose IVAN Meeting
  9:00 AM:  
Registration and Coffee at the Fairmont
10:00 AM:
Welcome and Introduction of Jon Webb (Dave Rice)
10:10 AM:
A Vision for the Future for Varian-Agilent NMR  (Jon Webb, MR Resources)
10:45 AM: 
Announcing OpenVnmrJ1 Software for the Varian-Agilent Community (Dan Iverson)
11:30 AM:
Discussion Topic:
Moving Forward Together with Service and Applications2 (chair: Michele Bodner)
12:00 PM:
Lunch will be served during the discussion.
1:15 PM 
Operation/Applications Sessions3 (organizers: Krish Krishnamurthy and Dave Russell)
3:00-3:30 PM
Conclusions and Planning for the Future
4:00 PM …. 
 “Happy Hour” (Soda, Wine and Beer Catered)

1OpenVnmrJ1.1A is an open-source successor to Agilent's VnmrJ4.2A, released by VOSSG, the VnmrJ Open-Source Steering Committee on 12-Sept-2016. VOSSG will continue development of OpenVnmrJ in association with the IVAN group.
2 A discussion of how we users can enhance the longevity and productivity of our Varian-Agilent consoles, probes and magnets. Bring your questions and issues.
3 We anticipate special topics chosen from the list below. Check the website for potential topics.

Meeting Special Topics

The topics below are under consideration for the afternoon sessions. Feel free to give your feedback about the choices with the following email link. We will select a subset, but at the very least, experts in these topics will be present at the San Jose meeting. Come with your questions!
  • New Veripulse Calibration with OpenVnmrJ (and VnmrJ4.2)
  • Software Administration and Automation with OpenVnmrJ (and VnmrJ4.2)
  • New 1D and 2D CRAFT from Chempacker
  • Using Chempack Tools
  • Biopack, NUS and NMRPipe with OpenVnmrJ (and VnmrJ4.2)
  • Managing Solids and Programming with SolidsPack Tools.
You can register for IVAN at the MRR webiste here. IVAN Registration
If you have more questions about IVAN you can send us an e-mail thru our website here. IVAN Questions

This email was sent to 
MR Resources · 160 Authority Drive · Fitchburg, MA 01420 · USA 

Monday, September 26, 2016

Milli-tesla NMR and spectrophotometry of liquids hyperpolarized by dissolution dynamic nuclear polarization

Zhu, Y., et al., Milli-tesla NMR and spectrophotometry of liquids hyperpolarized by dissolution dynamic nuclear polarization. J Magn Reson, 2016. 270: p. 71-6.

Hyperpolarization methods offer a unique means of improving low signal strength obtained in low-field NMR. Here, simultaneous measurements of NMR at a field of 0.7mT and laser optical absorption from samples hyperpolarized by dissolution dynamic nuclear polarization (D-DNP) are reported. The NMR measurement field closely corresponds to a typical field encountered during sample injection in a D-DNP experiment. The optical spectroscopy allows determination of the concentration of the free radical required for DNP. Correlation of radical concentration to NMR measurement of spin polarization and spin-lattice relaxation time allows determination of relaxivity and can be used for optimization of the D-DNP process. Further, the observation of the nuclear Overhauser effect originating from hyperpolarized spins is demonstrated. Signals from (1)H and (19)F in a mixture of trifluoroethanol and water are detected in a single spectrum, while different atoms of the same type are distinguished by J-coupling patterns. The resulting signal changes of individual peaks are indicative of molecular contact, suggesting a new application area of hyperpolarized low-field NMR for the determination of intermolecular interactions.

Friday, September 23, 2016

Hydration Dynamics of a Peripheral Membrane Protein #DNPNMR

Fisette, O., et al., Hydration Dynamics of a Peripheral Membrane Protein. J. Am. Chem. Soc., 2016. 138(36): p. 11526-11535.

Water dynamics in the hydration shell of the peripheral membrane protein annexin B12 were studied using MD simulations and Overhauser DNP-enhanced NMR. We show that retardation of water motions near phospholipid bilayers is extended by the presence of a membrane-bound protein, up to around 10 Å above that protein. Near the membrane surface, electrostatic interactions with the lipid head groups strongly slow down water dynamics, whereas protein-induced water retardation is weaker and dominates only at distances beyond 10 Å from the membrane surface. The results can be understood from a simple model based on additive contributions from the membrane and the protein to the activation free energy barriers of water diffusion next to the biomolecular surfaces. Furthermore, analysis of the intermolecular vibrations of the water network reveals that retarded water motions near the membrane shift the vibrational modes to higher frequencies, which we used to identify an entropy gradient from the membrane surface toward the bulk water. Our results have implications for processes that take place at lipid membrane surfaces, including molecular recognition, binding, and protein–protein interactions.

Wednesday, September 21, 2016

Impact of Ho3+-doping on 13C dynamic nuclear polarization using trityl OX063 free radical #DNPNMR

Kiswandhi, A., et al., Impact of Ho3+-doping on 13C dynamic nuclear polarization using trityl OX063 free radical. Phys. Chem. Chem. Phys., 2016. 18(31): p. 21351-21359.

We have investigated the effects of Ho-DOTA doping on the dynamic nuclear polarization (DNP) of [1-13C] sodium acetate using trityl OX063 free radical at 3.35 T and 1.2 K. Our results indicate that addition of 2 mM Ho-DOTA on 3 M [1-13C] sodium acetate sample in 1 : 1 v/v glycerol : water with 15 mM trityl OX063 improves the DNP-enhanced 13C solid-state nuclear polarization by a factor of around 2.7-fold. Similar to the Gd3+ doping effect on 13C DNP, the locations of the positive and negative 13C maximum polarization peaks in the 13C microwave DNP sweep are shifted towards each other with the addition of Ho-DOTA on the DNP sample. W-band electron spin resonance (ESR) studies have revealed that while the shape and linewidth of the trityl OX063 ESR spectrum was not affected by Ho3+-doping, the electron spin-lattice relaxation time T1 of trityl OX063 was prominently reduced at cryogenic temperatures. The reduction of trityl OX063 electron T1 by Ho-doping is linked to the 13C DNP improvement in light of the thermodynamic picture of DNP. Moreover, the presence of Ho-DOTA in the dissolution liquid at room temperature has negligible reduction effect on liquid-state 13C T1, in contrast to Gd3+-doping which drastically reduces the 13C T1. The results here suggest that Ho3+-doping is advantageous over Gd3+ in terms of preservation of hyperpolarized state-an important aspect to consider for in vitro and in vivo NMR or imaging (MRI) experiments where a considerable preparation time is needed to administer the hyperpolarized 13C liquid.