|Poster: PA - Solution and In vivo/Ex vivo |
Poster number: 137, All Week, 2:00 - 3:45, Fred Farr Pavilion
Ex-vivo Comprehensive Multiphase NMR of Intact Daphnia magna
Rajshree Ghosh Biswas1; Blythe Fortier-Mcgill1; Ronald Soong1; Daniel Schmidig2; Peter De Castro2; Stephan Graf2; Sebastian Wegner3; Falko Busse3; Jochem Struppe4; Michael Fey4; Myrna J. Simpson1; Andre J. Simpson1
1Environmental NMR Centre, University of Toronto, Toronto, Canada; 2Bruker Biospin AG, Fällanden, Switzerland; 3Bruker BioSpin GmbH, Rheinstetten, Germany; 4Bruker Corporation, Billerica, USA
Comprehensive Multiphase NMR (CMP-NMR) is a novel technique used to study different phases (solids, solutions and semisolids) in intact samples. This study illustrates multi-phase spectral editing techniques to follow ex vivo samples of Daphnia magna over various life stages and over different generations. The research demonstrates how spectral editing approaches in combination with multiphase NMR help uncover novel information on biological processes. In summary ex vivo NMR proves to be a very powerful approach to study whole organisms in a comprehensive manner and should provide very complimentary information to in vivo based research.
|Poster: PA - Solution and * omics / natural products |
Poster number: 162, All Week, 2:00pm - 3:45pm, Fred Farr Pavilion
Comprehensive Multiphase NMR: A Powerful Tool in Optimizing Biofuel Production
Paris Ning1; Daniel Lane1; Ronald Soong1; Daniel Schmidig2; Thomas Frei2; Peter De Castro2; Ivan Kovacevic2; Stephan Graf2; Sebastian Wegner3; Falko Busse3; Jochem Struppe4; Michael Fey4; Henry J. Stronks5; Martine Monette5; Hermann Heumann6; Myrna J. Simpson1; Andre J Simpson1
1University of Toronto, Toronto, Canada; 2Bruker Biospin AG (Switzerland), Fällanden, Switzerland; 3Bruker BioSpin, Rheinstetten, Germany; 4Bruker BioSpin, Billerica, MA; 5Bruker Ltd., Milton, Canada; 6Silantes GmbH, München, Germany
Algae is seen as one of the most important sources of biofuel. Comprehensive Multiphase (CMP) NMR combines all electronics and hardware required to give an overview of all phases. Applying CMP-NMR to algae, post extraction, provides a unique insight into what has been extracted (solution phase), what has been swollen (i.e. potential to be extracted with optimization) and what is inaccessible to subcritical water (i.e. that in the true solid-phase). In turn when applied to different algal strains and extraction procedures, CMP-NMR provides a quick overview as to how effective the approach is as-well as identifying the material that remains and could be extracted with further method optimization.
|Poster: PA - Solution and Instrumentation |
Poster number: 176, All Week, 2:00pm - 3:45pm, Fred Farr Pavilion
Improving HTS NMR Coil Pulse Shapes and Receive Bandwidth
Ghoncheh Amouzandeh1; Omid Sanati2; Vijaykumar Ramaswamy3; Nicolas Freytag3; Lawrence Hornak2; Arthur Edison2; William W. Brey1
1National High Magnetic Field Labratory / FSU, Tallahassee, FL; 2University of Georgia, Athens, GA; 3Bruker Biospin AG, Fällanden, Switzerland
Replacing normal metal NMR coils with high-temperature superconducting (HTS) coils can significantly improve the SNR due to the high Q factor of superconducting resonators. However, the high Q factor will reduce the system bandwidth for both reception and excitation which can be problematic for 13C with a wide chemical shift range. Exciting the whole chemical shift dispersion spectrum requires both strong and short RF pulses. Detecting the FID also requires a short dead-time before losing the NMR signal. The RF properties and the ability of the HTS resonators to accurately generate short pulses for excitation are studied in the time domain. The results show adding a shorted stub into the transmit path will shorten the coil rise and fall times.
|Poster: PA - Solution and New or unusual science |
Poster number: 181, All Week, 2:00pm - 3:45pm, Fred Farr Pavilion
Learning from the Jewellery Industry: CNC Micro-milling for Rapid, Cheap and Background Free NMR Micro-coils
Vincent Moxley-Paquette1; Daniel Lane1; Ronald Soong1; Paris Ning1; Monica Bastawrous1; Maysam Pedram2; Md Aminul Haque Talukder2; Ebrahim Ghafar Zadeh2; Dimitri Zverev3; Richard Martin4; Bob Macpherson5; Mike Vargas5; Falko Busse6; Wolfgang Bermel6; Till Kuehn7; Rainer Kuemmerle7; Danijela Al Adwan-Stojilkovic7; Daniel Schmidig7; Michael Fey8; Henry Stronks9; André Simpson1
1University of Toronto, Toronto, ON; 2York University, North York, ON; 3NSCNC Manufacturing LTD, Port Coquitlam, BC; 4IMicrosolder, Meaford, ON; 5Apogee Steel Fabrication Inc., Mississauga, ON; 6Bruker Biospin GmbH, Rheinstetten, Germany; 7Bruker BioSpin AG, Fällanden, Switzerland; 8Bruker Corporation, Billerica, MA; 9Bruker Canada Ltd, Milton, ON
There is great interest in miniaturizing NMR detection with the ultimate goal of studying metabolism in individual cells, eggs and tiny organisms. Here we explore the potential of micro-milling directly on Teflon electroplated with copper. Multi-turn spiral coils (40 µm wide copper) and a microstrip are fabricated as examples. Furthermore, micro-milling allows sample holders to be easily constructed at the same time as the coil is made. The microstrip was designed, milled, matched/tuned, and tested on the NMR spectrometer within 24 hrs, demonstrating the considerable potential of micro-machining for rapid prototyping of NMR micro sensors.
|Poster: PB - Solids and Small Molecules |
Poster number: 188, All Week, 2:00pm - 3:45pm, Fred Farr Pavilion
Ultrafast Magic Angle Spinning NMR Investigation of Natural Abundance Pharmaceuticals
Xingyu Lu1; Chengbin Huang1, 2; Karen C. Thompson1; Yu Tsutsumi4; Jean-Paul Amoureux4; Daniel Skomski1; Haichen Nie1; Wei Xu1; Yongchao Su1, 3
1Pharmaceutical Sciences, Merck & Co., Inc., Kenilworth, NJ; 2School of Pharmacy, University of Wisconsin-Madiso, Madison, WI; 3College of Pharmacy, University of Texas at Austin, Austin, TX; 4Bruker BioSpin, Yokohama, Japan
Solid-state NMR plays an indispensable role in characterizing solid pharmaceutical dosages for the noninvasive, quantitative and high resolution capabilities. The molecular investigation in multicomponent and natural abundance drug products offers both technical challenges and opportunities for this advanced technique. We aim at advancing proton detected spectroscopy under ultrafast magic angle spinning (MAS) of 60-111 kHz in pharmaceutical sciences. Development of novel multidimensional and heteronuclear correlation methods and their applications in the investigation of quantification of pharmaceutical formulation, drug-polymer interaction, and molecular packing of crystalline and amorphous drug molecules will be presented.
|Poster: PB - Solids and Biomolecular |
Poster number: 233, All Week, 2:00pm - 3:45pm, Fred Farr Pavilion
DNP-MAS NMR for the Structural Characterization of Spider Silk Fibers
Dillan Stengel1; David Onofrei1; Roshan Guia1; Parmida Saadipour1; Shane Pawsey2; Melanie Rosay2; Bennett Addison1; Gregory Holland1
1San Diego State University, San Diego, CA; 2Bruker Biospin Corporation, Billerica, MA
Spider dragline silk is an impressive biological polymer with mechanical properties that rival steel and Kevlar. Dragline silk, the strongest silk spiders make, is spun from silk proteins within the major ampullate gland. These silk proteins are comprised of a repetitive core rich in poly(Ala) runs and glycine-rich regions of Gly-Gly-X, or Gly-Pro-Gly-X-X. Unfortunately, the fibers are produced in low yield and take weeks, sometimes months, to isotope label and collect for solid-state NMR studies. In addition, the solid-state NMR spectra exhibit extremely broad 13C and 15N dimensions further hindering S/N. We therefore examined the potential of DNP-MAS NMR for investigating spider silk, improve S/N and enable more advanced three-dimensional (3D) experiments for structural characterization.
|Poster: PB - Solids and New or unusual science |
Poster number: 283, All Week, 2:00pm - 3:45pm, Fred Farr Pavilion
Protein NMR resonance assignment without spectral analysis: 5D SOlid-state Automated Projection SpectroscopY (SO-APSY)
Henry Orton1; Jan Stanek2, 3; Tobias Schubeis2; Dylan Foucaudeau2; Claire Ollier2; Adrian Draney2; Tanguy Le Marchand2; Diane Cala-De Paepe2; Isabella Felli4; Roberta Pierattelli4; Sebastian Hiller5; Wolfgang Bermel6; Guido Pintacuda2
1Australian National University, Canberra, Australia; 2CRMN Lyon, Lyon, France; 3University of Warsaw, Warsaw, Poland; 4CERM - University of Florence, Florence, Italy; 5Biozentrum, Basel, Switzerland; 6Bruker Biospin, Rheinstetten, Germany
Narrow proton signals, high sensitivity, and efficient coherence transfersprovided by fast magic-angle spinning at high magnetic fields make automated projection spectroscopy feasible in protein solid-state NMR. We present the first ultra-high dimensional implementation of this approach where 5D peak lists are reconstructed from a number of 2D projections for protein samples of different molecular size and aggregation state, featuring limited dispersion of chemical shifts or inhomogeneous broadenings. The resulting datasets are particularly suitable to automated analysis, yielding rapid and unbiased backbone resonance assignments.
|Poster: PE - Hyperpolarization and Small Molecules |
Poster number: 344, All Week, 2:00pm - 3:45pm, Fred Farr Pavilion
Cyclic Coherent Hyperpolarization of Water with p-H2
Eric Breynaert1; Ewoud Vaneeckhaute1; Jean-Max Tyburn2; James Kempf3; Francis Taulelle1; Johan Martens1
1COK-KAT, KU Leuven, Leuven, BELGIUM; 2Bruker Biospin, Rheinstetten, Germany; 3Bruker Biospin, Billerica, MA, US
|Poster: PE - Hyperpolarization and Biomolecular |
Poster number: 358, All Week, 2:00pm- 3:45pm, Fred Farr Pavilion
Biradical-tagged Phospholipid for Matrix-free DNP MAS NMR of Membrane Proteins
Daryl Good2; Maxim Voinov1; David Bolton2; Meaghan Ward2; Ivan Sergeev3; Marc Caporini3; Peter Scheffer2; Andy Lo2; Melanie Rosay3; Antonin Marek1; Leonid Brown2; Vladimir Ladizhansky2; Alex I. Smirnov1
1North Carolina State University, Raleigh, NC; 2University of Guelph, Guelph, ON; 3Bruker Biospin Ltd., Billerica, MA
A novel DNP polarizing agent ToSMTSL-PTE representing a phospholipid bearing a biradical – a TOTAPOL derivative – tethered to the polar head group by a flexible linker was synthesized, characterized, and employed to enhance solid-state NMR signal of a lipid-reconstituted integral membrane protein proteorhodopsin . The results were compared with DNP enhancements obtained with a conventional sample protocol based on dispersing TOTAPOL in a glassy water-glycerol matrix. Complementary variable temperature EPR and differential scanning calorimetry experiments indicated possible conformational changes and an inhomogeneous distribution of the lipid-based biradicals in lipid bilayers when mixed at high (20 mol%) concentration for maximum DNP enhancement. Thus, the latter two factors should be also considered for further development of matrix-free DNP of membrane proteins.
|Poster: PE - Hyperpolarization and Materials |
Poster number: 370, All Week, 2:00pm - 3:45pm, Fred Farr Pavilion
Narrow line and Hybrid BDPA-Nitroxide Polarizing Agents for High-Field and Fast-MAS DNP
Dorothea Wisser1; Ganesan Karthikeyan3; Alicia Lund1; Gilles Casano3; Hakim Karoui3; Maxim Yulikov4; Georges Menzildjian1; Arthur Pinon2; Armin Purea5; Frank Engelke5; Sachin Chaudhari1; Dominik Kubicki2; Aaron Rossini2; Ilia Moroz4; David Gajan1; Christophe Copéret4; Gunnar Jeschke4; Lyndon Emsley2; Anne Lesage1; Olivier Ouari3; Moreno Lelli6
1ENS Lyon, Lyon, France; 2EPFL, Lausanne, Switzerland; 3AixMarseille Université, CNRS, ICR,, Marseille, France; 4ETH Zürich, Zürich, Switzerland; 5Bruker BioSpin GmbH, Rheinstetten, Germany; 6University of Florence, Sesto Fiorentino (Florence), Italy
DNP can boost sensitivity of MAS NMR by around 2 orders of magnitude at 9.4T. Nevertheless, dinitroxide biradicals suffer for a significant drop in performance at high field and fast MAS. Here we show how these limits can be overcome with new polarizing agents, based on the narrow EPR line BDPA radical. Overhauser DNP of BDPA radical in OTP yields enhancements over 100 at 18.8 T and 40 kHz MAS that increase with MAS and with no depolarization or quenching effects. Hybrid BDPA-nitroxide biradicals on the other hand show the highest enhancements and overall sensitivity gains observed up to now at high field. The potential of these polarizing agents for the characterization of pharmaceutical and functionalized material surfaces is illustrated.
| Poster: PE - Hyperpolarization and Instrumentation |
Poster number: 391, All Week, 2:00pm - 3:45pm, Fred Farr Pavilion
Microwave field simulations at 263GHz–527GHz for small-diameter MAS-DNP probes focusing the incident microwave beam by means of a waveguide coupler
Armin Purea1; Christian Reiter1; Fabien Aussenac2; Frank Engelke1
1Bruker BioSpin, Rheinstetten, Germany; 2Bruker Biospin, Wissembourg, France