35Cl dynamic nuclear polarization solid-state NMR of active pharmaceutical ingredients
Abstract
In this paper, we show how to obtain efficient dynamic nuclear polarization (DNP) enhanced 35Cl solid-state NMR (SSNMR) spectra at 9.4 T and demonstrate how they can be used to characterize the molecular-level structure of hydrochloride salts of active pharmaceutical ingredients (APIs) in both bulk and low wt% API dosage forms. 35Cl SSNMR central-transition powder patterns of chloride ions are typically tens to hundreds of kHz in breadth, and most cannot be excited uniformly with high-power rectangular pulses or acquired under conditions of magic-angle spinning (MAS). Herein, we demonstrate the combination of DNP and 1H–35Cl broadband adiabatic inversion cross polarization (BRAIN-CP) experiments for the acquisition of high quality wideline spectra of APIs under static sample conditions, and obtain signals up to 50 times greater than in spectra acquired without the use of DNP at 100 K. We report a new protocol, called spinning-on spinning-off (SOSO) acquisition, where MAS is applied during part of the polarization delay to increase the DNP enhancements and then the MAS rotation is stopped so that a wideline 35Cl NMR powder pattern free from the effects of spinning sidebands can be acquired under static conditions. This method provides an additional two-fold signal enhancement compared to DNP-enhancedmore »
- Authors:
-
- Univ. of Windsor, Windsor, ON (Canada)
- Iowa State Univ., Ames, IA (United States); Ames Lab., Ames, IA (United States)
- Ecole Polytechnique Federale Lausanne (Switzlerland)
- Publication Date:
- Research Org.:
- Ames Laboratory (AMES), Ames, IA (United States)
- Sponsoring Org.:
- USDOE
- OSTI Identifier:
- 1335033
- Report Number(s):
- IS-J-9134
Journal ID: ISSN 1463-9076; PPCPFQ
- Grant/Contract Number:
- AC02-07CH11358
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Physical Chemistry Chemical Physics. PCCP
- Additional Journal Information:
- Journal Volume: 18; Journal Issue: 37; Journal ID: ISSN 1463-9076
- Publisher:
- Royal Society of Chemistry
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEAR CHEMISTRY
Citation Formats
Hirsh, David A., Rossini, Aaron J., Emsley, Lyndon, and Schurko, Robert W. 35Cl dynamic nuclear polarization solid-state NMR of active pharmaceutical ingredients. United States: N. p., 2016.
Web. doi:10.1039/c6cp04353d.
Hirsh, David A., Rossini, Aaron J., Emsley, Lyndon, & Schurko, Robert W. 35Cl dynamic nuclear polarization solid-state NMR of active pharmaceutical ingredients. United States. https://doi.org/10.1039/c6cp04353d
Hirsh, David A., Rossini, Aaron J., Emsley, Lyndon, and Schurko, Robert W. Wed .
"35Cl dynamic nuclear polarization solid-state NMR of active pharmaceutical ingredients". United States. https://doi.org/10.1039/c6cp04353d. https://www.osti.gov/servlets/purl/1335033.
@article{osti_1335033,
title = {35Cl dynamic nuclear polarization solid-state NMR of active pharmaceutical ingredients},
author = {Hirsh, David A. and Rossini, Aaron J. and Emsley, Lyndon and Schurko, Robert W.},
abstractNote = {In this paper, we show how to obtain efficient dynamic nuclear polarization (DNP) enhanced 35Cl solid-state NMR (SSNMR) spectra at 9.4 T and demonstrate how they can be used to characterize the molecular-level structure of hydrochloride salts of active pharmaceutical ingredients (APIs) in both bulk and low wt% API dosage forms. 35Cl SSNMR central-transition powder patterns of chloride ions are typically tens to hundreds of kHz in breadth, and most cannot be excited uniformly with high-power rectangular pulses or acquired under conditions of magic-angle spinning (MAS). Herein, we demonstrate the combination of DNP and 1H–35Cl broadband adiabatic inversion cross polarization (BRAIN-CP) experiments for the acquisition of high quality wideline spectra of APIs under static sample conditions, and obtain signals up to 50 times greater than in spectra acquired without the use of DNP at 100 K. We report a new protocol, called spinning-on spinning-off (SOSO) acquisition, where MAS is applied during part of the polarization delay to increase the DNP enhancements and then the MAS rotation is stopped so that a wideline 35Cl NMR powder pattern free from the effects of spinning sidebands can be acquired under static conditions. This method provides an additional two-fold signal enhancement compared to DNP-enhanced SSNMR spectra acquired under purely static conditions. DNP-enhanced 35Cl experiments are used to characterize APIs in bulk and dosage forms with Cl contents as low as 0.45 wt%. These results are compared to DNP-enhanced 1H–13C CP/MAS spectra of APIs in dosage forms, which are often hindered by interfering signals arising from the binders, fillers and other excipient materials.},
doi = {10.1039/c6cp04353d},
journal = {Physical Chemistry Chemical Physics. PCCP},
number = 37,
volume = 18,
place = {United States},
year = {Wed Aug 24 00:00:00 EDT 2016},
month = {Wed Aug 24 00:00:00 EDT 2016}
}
Web of Science
Works referenced in this record:
Nanosizing — Oral formulation development and biopharmaceutical evaluation
journal, July 2007
- Kesisoglou, Filippos; Panmai, Santipharp; Wu, Yunhui
- Advanced Drug Delivery Reviews, Vol. 59, Issue 7
Solid form screening – A review
journal, January 2009
- Aaltonen, J.; Alleso, M.; Mirza, S.
- European Journal of Pharmaceutics and Biopharmaceutics, Vol. 71, Issue 1
Assessing the performance of amorphous solid dispersions
journal, April 2012
- Newman, Ann; Knipp, Gregory; Zografi, George
- Journal of Pharmaceutical Sciences, Vol. 101, Issue 4
An Overview of Pharmaceutical Cocrystals as Intellectual Property
journal, May 2007
- Trask, Andrew V.
- Molecular Pharmaceutics, Vol. 4, Issue 3
Dealing with the Impact of Ritonavir Polymorphs on the Late Stages of Bulk Drug Process Development
journal, September 2000
- Chemburkar, Sanjay R.; Bauer, John; Deming, Kris
- Organic Process Research & Development, Vol. 4, Issue 5
Crystalline Polymorphism of Organic Compounds
book, January 1998
- Caira, Mino R.
- Design of Organic Solids. Topics in Current Chemistry
Identification, Preparation, and Characterization of Several Polymorphs and Solvates of Terazosin Hydrochloride
journal, April 2006
- Bauer, J.; Morley, J.; Spanton, S.
- Journal of Pharmaceutical Sciences, Vol. 95, Issue 4
Influence of physicochemical properties on dissolution of drugs in the gastrointestinal tract
journal, April 1997
- Hörter, D.; Dressman, J. B.
- Advanced Drug Delivery Reviews, Vol. 25, Issue 1
Mechanistic Insights into the Dissolution of Spray-Dried Amorphous Solid Dispersions
journal, August 2012
- Langham, Zoe A.; Booth, Jonathan; Hughes, Les P.
- Journal of Pharmaceutical Sciences, Vol. 101, Issue 8
Impact of solid state properties on developability assessment of drug candidates
journal, February 2004
- Huang, L.
- Advanced Drug Delivery Reviews, Vol. 56, Issue 3
Characterization of the solid-state: spectroscopic techniques
journal, May 2001
- Bugay, David E.
- Advanced Drug Delivery Reviews, Vol. 48, Issue 1
Crystal structures of drugs: advances in determination, prediction and engineering
journal, January 2004
- Datta, Sharmistha; Grant, David J. W.
- Nature Reviews Drug Discovery, Vol. 3, Issue 1
NMR studies of organic polymorphs & solvates
journal, January 2006
- Harris, Robin K.
- The Analyst, Vol. 131, Issue 3
Applications of solid-state NMR to pharmaceutical polymorphism and related matters*
journal, February 2007
- Harris, Robin K.
- Journal of Pharmacy and Pharmacology, Vol. 59, Issue 2
Characterization of Pharmaceutical Compounds by Solid-state NMR
book, January 2015
- Vogt, Frederick G.
- eMagRes
35 Cl solid-state NMR of HCl salts of active pharmaceutical ingredients: structural prediction, spectral fingerprinting and polymorph recognition
journal, January 2014
- Hildebrand, Marcel; Hamaed, Hiyam; Namespetra, Andrew M.
- CrystEngComm, Vol. 16, Issue 31
Application of Solid-State 35 Cl NMR to the Structural Characterization of Hydrochloride Pharmaceuticals and their Polymorphs
journal, August 2008
- Hamaed, Hiyam; Pawlowski, Jenna M.; Cooper, Benjamin F. T.
- Journal of the American Chemical Society, Vol. 130, Issue 33
35 Cl solid-state NMR spectroscopy of HCl pharmaceuticals and their polymorphs in bulk and dosage forms
journal, January 2016
- Namespetra, Andrew M.; Hirsh, David A.; Hildebrand, Marcel P.
- CrystEngComm, Vol. 18, Issue 33
Two-dimensional proton-detected 35 Cl/ 1 H correlation solid-state NMR experiment under fast magic angle sample spinning: application to pharmaceutical compounds
journal, January 2016
- Pandey, Manoj Kumar; Kato, Hiroshi; Ishii, Yuji
- Physical Chemistry Chemical Physics, Vol. 18, Issue 8
Solid-State NMR Analysis of a Complex Crystalline Phase of Ronacaleret Hydrochloride
journal, August 2014
- Vogt, Frederick G.; Williams, Glenn R.; Strohmeier, Mark
- The Journal of Physical Chemistry B, Vol. 118, Issue 34
Chlorine-35/37 NMR Spectroscopy of Solid Amino Acid Hydrochlorides: Refinement of Hydrogen-Bonded Proton Positions Using Experiment and Theory
journal, December 2006
- Bryce, David L.; Sward, Gregory D.
- The Journal of Physical Chemistry B, Vol. 110, Issue 51
Alkaline Earth Chloride Hydrates: Chlorine Quadrupolar and Chemical Shift Tensors by Solid-State NMR Spectroscopy and Plane Wave Pseudopotential Calculations
journal, June 2007
- Bryce, David L.; Bultz, Elijah B.
- Chemistry - A European Journal, Vol. 13, Issue 17
Magnetic resonance spectral reconstruction using frequency‐shifted and summed Fourier transform processing
journal, March 1995
- Clark, W. G.; Hanson, M. E.; Lefloch, F.
- Review of Scientific Instruments, Vol. 66, Issue 3
71Ga and 69Ga nuclear magnetic resonance study of β-Ga2O3: resolution of four- and six-fold coordinated Ga sites in static conditions
journal, May 1995
- Massiot, Dominique; Farnan, Ian; Gautier, Nathalie
- Solid State Nuclear Magnetic Resonance, Vol. 4, Issue 4
Ultra-Wideline Solid-State NMR Spectroscopy
journal, June 2013
- Schurko, Robert W.
- Accounts of Chemical Research, Vol. 46, Issue 9
Adiabatic Pulses for Wideband Inversion and Broadband Decoupling
journal, August 1995
- Kupce, E.; Freeman, R.
- Journal of Magnetic Resonance, Series A, Vol. 115, Issue 2
Quadrupolar nuclear magnetic resonance spectroscopy in solids using frequency-swept echoing pulses
journal, November 2007
- Bhattacharyya, Rangeet; Frydman, Lucio
- The Journal of Chemical Physics, Vol. 127, Issue 19
Acquisition of ultra-wideline NMR spectra from quadrupolar nuclei by frequency stepped WURST–QCPMG
journal, January 2009
- O’Dell, Luke A.; Rossini, Aaron J.; Schurko, Robert W.
- Chemical Physics Letters, Vol. 468, Issue 4-6
QCPMG using adiabatic pulses for faster acquisition of ultra-wideline NMR spectra
journal, October 2008
- O’Dell, Luke A.; Schurko, Robert W.
- Chemical Physics Letters, Vol. 464, Issue 1-3
Broadband adiabatic inversion pulses for cross polarization in wideline solid-state NMR spectroscopy
journal, November 2012
- Harris, Kristopher J.; Lupulescu, Adonis; Lucier, Bryan E. G.
- Journal of Magnetic Resonance, Vol. 224
Polarization-Enhanced NMR Spectroscopy of Biomolecules in Frozen Solution
journal, May 1997
- Hall, Dennis A.; Maus, Douglas C.; Gerfen, Gary J.
- Science, Vol. 276, Issue 5314
High field dynamic nuclear polarization—the renaissance
journal, January 2010
- Griffin, R. G.; Prisner, T. F.
- Physical Chemistry Chemical Physics, Vol. 12, Issue 22
Dynamic nuclear polarization at high magnetic fields
journal, February 2008
- Maly, Thorsten; Debelouchina, Galia T.; Bajaj, Vikram S.
- The Journal of Chemical Physics, Vol. 128, Issue 5
Dynamic nuclear polarization with a cyclotron resonance maser at 5 T
journal, November 1993
- Becerra, Lino R.; Gerfen, Gary J.; Temkin, Richard J.
- Physical Review Letters, Vol. 71, Issue 21
A Spectrometer for Dynamic Nuclear Polarization and Electron Paramagnetic Resonance at High Frequencies
journal, November 1995
- Becerra, L. R.; Gerfen, G. J.; Bellew, B. F.
- Journal of Magnetic Resonance, Series A, Vol. 117, Issue 1
Operational characteristics of a 14-W 140-GHz gyrotron for dynamic nuclear polarization
journal, June 2006
- Joye, C. D.; Griffin, R. G.; Hornstein, M. K.
- IEEE Transactions on Plasma Science, Vol. 34, Issue 3
Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization
journal, June 2009
- Barnes, Alexander B.; Mak-Jurkauskas, Melody L.; Matsuki, Yoh
- Journal of Magnetic Resonance, Vol. 198, Issue 2
High-Frequency Dynamic Nuclear Polarization in MAS Spectra of Membrane and Soluble Proteins
journal, November 2003
- Rosay, Melanie; Lansing, Jonathan C.; Haddad, Kristin C.
- Journal of the American Chemical Society, Vol. 125, Issue 45
TOTAPOL: A Biradical Polarizing Agent for Dynamic Nuclear Polarization Experiments in Aqueous Media
journal, September 2006
- Song, Changsik; Hu, Kan-Nian; Joo, Chan-Gyu
- Journal of the American Chemical Society, Vol. 128, Issue 35
Highly Efficient, Water-Soluble Polarizing Agents for Dynamic Nuclear Polarization at High Frequency
journal, August 2013
- Sauvée, Claire; Rosay, Melanie; Casano, Gilles
- Angewandte Chemie International Edition, Vol. 52, Issue 41
Dynamic Nuclear Polarization with Biradicals
journal, September 2004
- Hu, Kan-Nian; Yu, Hsiao-hua; Swager, Timothy M.
- Journal of the American Chemical Society, Vol. 126, Issue 35
Large Molecular Weight Nitroxide Biradicals Providing Efficient Dynamic Nuclear Polarization at Temperatures up to 200 K
journal, August 2013
- Zagdoun, Alexandre; Casano, Gilles; Ouari, Olivier
- Journal of the American Chemical Society, Vol. 135, Issue 34
Rational design of dinitroxide biradicals for efficient cross-effect dynamic nuclear polarization
journal, January 2016
- Kubicki, Dominik J.; Casano, Gilles; Schwarzwälder, Martin
- Chemical Science, Vol. 7, Issue 1
Instrumentation for solid-state dynamic nuclear polarization with magic angle spinning NMR
journal, March 2016
- Rosay, Melanie; Blank, Monica; Engelke, Frank
- Journal of Magnetic Resonance, Vol. 264
Solid-state dynamic nuclear polarization at 263 GHz: spectrometer design and experimental results
journal, January 2010
- Rosay, Melanie; Tometich, Leo; Pawsey, Shane
- Physical Chemistry Chemical Physics, Vol. 12, Issue 22
Dynamic Nuclear Polarization Solid-State NMR in Heterogeneous Catalysis Research
journal, October 2015
- Kobayashi, Takeshi; Perras, Frédéric A.; Slowing, Igor I.
- ACS Catalysis, Vol. 5, Issue 12
Dynamic Nuclear Polarization Surface Enhanced NMR Spectroscopy
journal, March 2013
- Rossini, Aaron J.; Zagdoun, Alexandre; Lelli, Moreno
- Accounts of Chemical Research, Vol. 46, Issue 9
Mesoporous Silica Nanoparticles Loaded with Surfactant: Low Temperature Magic Angle Spinning 13 C and 29 Si NMR Enhanced by Dynamic Nuclear Polarization
journal, January 2013
- Lafon, Olivier; Thankamony, Aany S. Lilly; Kobayashi, Takeshi
- The Journal of Physical Chemistry C, Vol. 117, Issue 3
Dynamic Nuclear Polarization NMR Enables the Analysis of Sn-Beta Zeolite Prepared with Natural Abundance 119 Sn Precursors
journal, April 2014
- Gunther, William R.; Michaelis, Vladimir K.; Caporini, Marc A.
- Journal of the American Chemical Society, Vol. 136, Issue 17
Natural Abundance 17 O DNP Two-Dimensional and Surface-Enhanced NMR Spectroscopy
journal, June 2015
- Perras, Frédéric A.; Kobayashi, Takeshi; Pruski, Marek
- Journal of the American Chemical Society, Vol. 137, Issue 26
Dynamic Nuclear Polarization Enhanced Natural Abundance 17 O Spectroscopy
journal, February 2013
- Blanc, Frédéric; Sperrin, Luke; Jefferson, David A.
- Journal of the American Chemical Society, Vol. 135, Issue 8
Direct dynamic nuclear polarization targeting catalytically active 27 Al sites
journal, January 2015
- Lund, Alicia; Hsieh, Ming-Feng; Siaw, Ting-Ann
- Physical Chemistry Chemical Physics, Vol. 17, Issue 38
Rapid Natural-Abundance 2D 13 C- 13 C Correlation Spectroscopy Using Dynamic Nuclear Polarization Enhanced Solid-State NMR and Matrix-Free Sample Preparation
journal, October 2012
- Takahashi, Hiroki; Lee, Daniel; Dubois, Lionel
- Angewandte Chemie International Edition, Vol. 51, Issue 47
Untangling the Condensation Network of Organosiloxanes on Nanoparticles using 2D 29 Si– 29 Si Solid-State NMR Enhanced by Dynamic Nuclear Polarization
journal, September 2014
- Lee, Daniel; Monin, Guillaume; Duong, Nghia Tuan
- Journal of the American Chemical Society, Vol. 136, Issue 39
Selective Host-Guest Interaction between Metal Ions and Metal-Organic Frameworks Using Dynamic Nuclear Polarization Enhanced Solid-State NMR Spectroscopy
journal, October 2014
- Guo, Zhiyong; Kobayashi, Takeshi; Wang, Lin-Lin
- Chemistry - A European Journal, Vol. 20, Issue 49
Surface Enhanced NMR Spectroscopy by Dynamic Nuclear Polarization
journal, November 2010
- Lesage, Anne; Lelli, Moreno; Gajan, David
- Journal of the American Chemical Society, Vol. 132, Issue 44
Dynamic Nuclear Polarization of Amyloidogenic Peptide Nanocrystals: GNNQQNY, a Core Segment of the Yeast Prion Protein Sup35p
journal, August 2006
- van der Wel, Patrick C. A.; Hu, Kan-Nian; Lewandowski, Józef
- Journal of the American Chemical Society, Vol. 128, Issue 33
Dynamic Nuclear Polarization NMR Spectroscopy of Microcrystalline Solids
journal, September 2012
- Rossini, Aaron J.; Zagdoun, Alexandre; Hegner, Franziska
- Journal of the American Chemical Society, Vol. 134, Issue 40
Dynamic nuclear polarisation enhanced 14 N overtone MAS NMR spectroscopy
journal, January 2014
- Rossini, Aaron J.; Emsley, Lyndon; O'Dell, Luke A.
- Phys. Chem. Chem. Phys., Vol. 16, Issue 25
A New Tool for NMR Crystallography: Complete 13 C/ 15 N Assignment of Organic Molecules at Natural Isotopic Abundance Using DNP-Enhanced Solid-State NMR
journal, October 2015
- Märker, Katharina; Pingret, Morgane; Mouesca, Jean-Marie
- Journal of the American Chemical Society, Vol. 137, Issue 43
High-resolution NMR of hydrogen in organic solids by DNP enhanced natural abundance deuterium spectroscopy
journal, October 2015
- Rossini, Aaron J.; Schlagnitweit, Judith; Lesage, Anne
- Journal of Magnetic Resonance, Vol. 259
Quantitative Structural Constraints for Organic Powders at Natural Isotopic Abundance Using Dynamic Nuclear Polarization Solid-State NMR Spectroscopy
journal, March 2015
- Mollica, Giulia; Dekhil, Myriam; Ziarelli, Fabio
- Angewandte Chemie International Edition, Vol. 54, Issue 20
Polymorphs of Theophylline Characterized by DNP Enhanced Solid-State NMR
journal, October 2015
- Pinon, Arthur C.; Rossini, Aaron J.; Widdifield, Cory M.
- Molecular Pharmaceutics, Vol. 12, Issue 11
Dynamic Nuclear Polarization Enhanced NMR Spectroscopy for Pharmaceutical Formulations
journal, January 2014
- Rossini, Aaron J.; Widdifield, Cory M.; Zagdoun, Alexandre
- Journal of the American Chemical Society, Vol. 136, Issue 6
2H-DNP-enhanced 2H–13C solid-state NMR correlation spectroscopy
journal, January 2010
- Maly, Thorsten; Andreas, Loren B.; Smith, Albert A.
- Physical Chemistry Chemical Physics, Vol. 12, Issue 22
Dynamic Nuclear Polarization of Oxygen-17
journal, July 2012
- Michaelis, Vladimir K.; Markhasin, Evgeny; Daviso, Eugenio
- The Journal of Physical Chemistry Letters, Vol. 3, Issue 15
Dynamic nuclear polarization enhancement of protons and vanadium-51 in the presence of pH-dependent vanadyl radicals: Dynamic nuclear polarization enhancement of protons and vanadium-51
journal, September 2014
- Perez Linde, Angel J.; Carnevale, Diego; Miéville, Pascal
- Magnetic Resonance in Chemistry, Vol. 53, Issue 2
Enhanced Solid-State NMR Correlation Spectroscopy of Quadrupolar Nuclei Using Dynamic Nuclear Polarization
journal, October 2012
- Lee, Daniel; Takahashi, Hiroki; Thankamony, Aany S. L.
- Journal of the American Chemical Society, Vol. 134, Issue 45
Atomic Description of the Interface between Silica and Alumina in Aluminosilicates through Dynamic Nuclear Polarization Surface-Enhanced NMR Spectroscopy and First-Principles Calculations
journal, August 2015
- Valla, Maxence; Rossini, Aaron J.; Caillot, Maxime
- Journal of the American Chemical Society, Vol. 137, Issue 33
Dynamic nuclear polarization of quadrupolar nuclei using cross polarization from protons: surface-enhanced aluminium-27 NMR
journal, January 2012
- Vitzthum, Veronika; Miéville, Pascal; Carnevale, Diego
- Chemical Communications, Vol. 48, Issue 14
DNP-Enhanced Ultrawideline Solid-State NMR Spectroscopy: Studies of Platinum in Metal–Organic Frameworks
journal, June 2016
- Kobayashi, Takeshi; Perras, Frédéric A.; Goh, Tian Wei
- The Journal of Physical Chemistry Letters, Vol. 7, Issue 13
Theory for cross effect dynamic nuclear polarization under magic-angle spinning in solid state nuclear magnetic resonance: The importance of level crossings
journal, August 2012
- Thurber, Kent R.; Tycko, Robert
- The Journal of Chemical Physics, Vol. 137, Issue 8
Fast passage dynamic nuclear polarization on rotating solids
journal, November 2012
- Mentink-Vigier, Frederic; Akbey, Ümit; Hovav, Yonatan
- Journal of Magnetic Resonance, Vol. 224
Dynamic nuclear polarization at 40 kHz magic angle spinning
journal, January 2016
- Chaudhari, Sachin R.; Berruyer, Pierrick; Gajan, David
- Physical Chemistry Chemical Physics, Vol. 18, Issue 15
From nuclear structure to the quadrupolar NMR interaction and high-resolution spectroscopy
journal, March 2005
- Jerschow, Alexej
- Progress in Nuclear Magnetic Resonance Spectroscopy, Vol. 46, Issue 1
Neutron diffraction study of L-histidine hydrochloride monohydrate
journal, March 1977
- Fuess, H.; Hohlwein, D.; Mason, S. A.
- Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry, Vol. 33, Issue 3
CCDC 189162: Experimental Crystal Structure Determination
dataset, January 2003
- Schollmeyer, D.; Henk, M.
- Cambridge Crystallographic Data Centre
A monoclinic polymorph of isoxsuprine hydrochloride
journal, November 2004
- Yathirajan, Hemmige S.; Nagaraj, Basavegowda; Narasegowda, Rajenahally S.
- Acta Crystallographica Section E Structure Reports Online, Vol. 60, Issue 12
X-Ray crystallography studies and CP-MAS 13C NMR spectroscopy on the solid-state stereochemistry of diphenhydramine hydrochloride, an antihistaminic drug
journal, January 1990
- Glaser, Robert; Maartmann-Moe, Knut
- Journal of the Chemical Society, Perkin Transactions 2, Issue 7
NMR nomenclature. Nuclear spin properties and conventions for chemical shifts(IUPAC Recommendations 2001)
journal, January 2001
- Harris, Robin K.; Becker, Edwin D.; Cabral de Menezes, Sonia M.
- Pure and Applied Chemistry, Vol. 73, Issue 11
Enhancement of CP-MAS Signals by Variable-Amplitude Cross Polarization. Compensation for Inhomogeneous B1 Fields
journal, January 1994
- Peersen, O. B.; Wu, X. L.; Smith, S. O.
- Journal of Magnetic Resonance, Series A, Vol. 106, Issue 1
Variable-Amplitude Cross-Polarization MAS NMR
journal, October 1993
- Peersen, O. B.; Wu, X. L.; Kustanovich, I.
- Journal of Magnetic Resonance, Series A, Vol. 104, Issue 3
Ramped-Amplitude Cross Polarization in Magic-Angle-Spinning NMR
journal, October 1994
- Metz, G.; Wu, X. L.; Smith, S. O.
- Journal of Magnetic Resonance, Series A, Vol. 110, Issue 2
An Improved Broadband Decoupling Sequence for Liquid Crystals and Solids
journal, January 2000
- Fung, B. M.; Khitrin, A. K.; Ermolaev, Konstantin
- Journal of Magnetic Resonance, Vol. 142, Issue 1
Ultra-wideline27Al NMR Investigation of Three- and Five-Coordinate Aluminum Environments
journal, January 2006
- Tang, Joel A.; Masuda, Jason D.; Boyle, Timothy J.
- ChemPhysChem, Vol. 7, Issue 1
Proton-detected 14N MAS NMR using homonuclear decoupled rotary resonance
journal, February 2007
- Gan, Zhehong; Amoureux, Jean Paul; Trébosc, Julien
- Chemical Physics Letters, Vol. 435, Issue 1-3
Through-space MP-CPMAS experiments between spin-1/2 and half-integer quadrupolar nuclei in solid-state NMR
journal, May 2008
- Hu, B.; Amoureux, J. P.; Trébosc, J.
- Journal of Magnetic Resonance, Vol. 192, Issue 1
SIMPSON: A General Simulation Program for Solid-State NMR Spectroscopy
journal, December 2000
- Bak, Mads; Rasmussen, Jimmy T.; Nielsen, Niels Chr
- Journal of Magnetic Resonance, Vol. 147, Issue 2
Computer-intensive simulation of solid-state NMR experiments using SIMPSON
journal, September 2014
- Tošner, Zdeněk; Andersen, Rasmus; Stevensson, Baltzar
- Journal of Magnetic Resonance, Vol. 246
13C solid-state NMR analysis of the most common pharmaceutical excipients used in solid drug formulations, Part I: Chemical shifts assignment
journal, April 2016
- Pisklak, Dariusz Maciej; Zielińska- Pisklak, Monika Agnieszka; Szeleszczuk, Łukasz
- Journal of Pharmaceutical and Biomedical Analysis, Vol. 122
Analysis of Structural Variability in Pharmaceutical Excipients Using Solid-State NMR Spectroscopy
journal, June 2011
- Sperger, Diana M.; Munson, Eric Jon
- AAPS PharmSciTech, Vol. 12, Issue 3
Solid-state NMR spectroscopy of the quadrupolar halogens: chlorine-35/37, bromine-79/81, and iodine-127
journal, January 2006
- Bryce, David L.; Sward, Gregory D.
- Magnetic Resonance in Chemistry, Vol. 44, Issue 4
A Study of Transition-Metal Organometallic Complexes Combining 35 Cl Solid-State NMR Spectroscopy and 35 Cl NQR Spectroscopy and First-Principles DFT Calculations
journal, August 2013
- Johnston, Karen E.; O'Keefe, Christopher A.; Gauvin, Régis M.
- Chemistry - A European Journal, Vol. 19, Issue 37
An Investigation of Chlorine Ligands in Transition-Metal Complexes via 35 Cl Solid-State NMR and Density Functional Theory Calculations
journal, August 2014
- O’Keefe, Christopher A.; Johnston, Karen E.; Sutter, Kiplangat
- Inorganic Chemistry, Vol. 53, Issue 18
Non-aqueous solvents for DNP surface enhanced NMR spectroscopy
journal, January 2012
- Zagdoun, Alexandre; Rossini, Aaron J.; Gajan, David
- Chem. Commun., Vol. 48, Issue 5
Solid‐State NMR Studies of Pharmaceutical Systems
journal, March 2008
- Geppi, Marco; Mollica, Giulia; Borsacchi, Silvia
- Applied Spectroscopy Reviews, Vol. 43, Issue 3
Solid-state NMR spectroscopy in pharmaceutical research and analysis
journal, November 2006
- Berendt, Robert T.; Sperger, Diana M.; Munson, Eric J.
- TrAC Trends in Analytical Chemistry, Vol. 25, Issue 10
Amplifying Dynamic Nuclear Polarization of Frozen Solutions by Incorporating Dielectric Particles
journal, October 2014
- Kubicki, Dominik J.; Rossini, Aaron J.; Purea, Armin
- Journal of the American Chemical Society, Vol. 136, Issue 44
Highly Efficient, Water-Soluble Polarizing Agents for Dynamic Nuclear Polarization at High Frequency
journal, August 2013
- Sauvée, Claire; Rosay, Melanie; Casano, Gilles
- Angewandte Chemie, Vol. 125, Issue 41
Quantitative Structural Constraints for Organic Powders at Natural Isotopic Abundance Using Dynamic Nuclear Polarization Solid-State NMR Spectroscopy
journal, March 2015
- Mollica, Giulia; Dekhil, Myriam; Ziarelli, Fabio
- Angewandte Chemie, Vol. 127, Issue 20
Solid-State NMR Spectroscopy of the Quadrupolar Halogens: Chlorine-35/37, Bromine-79/81, and Iodine-127
journal, August 2006
- Bryce, David L.; Sward, Gregory D.
- ChemInform, Vol. 37, Issue 35
Applications of Solid-State NMR to Pharmaceutical Polymorphism and Related Matters
journal, July 2007
- Harris, Robin K.
- ChemInform, Vol. 38, Issue 27
Rapid Natural-Abundance 2D 13 C- 13 C Correlation Spectroscopy Using Dynamic Nuclear Polarization Enhanced Solid-State NMR and Matrix-Free Sample Preparation
journal, October 2012
- Takahashi, Hiroki; Lee, Daniel; Dubois, Lionel
- Angewandte Chemie, Vol. 124, Issue 47
From Nuclear Structure to the Quadrupolar NMR Interaction and High-Resolution Spectroscopy
journal, August 2005
- Jerschow, Alexej
- ChemInform, Vol. 36, Issue 31
Rational design of dinitroxide biradicals for efficient cross-effect dynamic nuclear polarization
text, January 2016
- J., Kubicki, Dominik; Gilles, Casano,; Martin, Schwarzwälder,
- ETH Zurich
SIMPSON: A general simulation program for solid-state NMR spectroscopy
journal, December 2011
- Bak, Mads; Rasmussen, Jimmy T.; Nielsen, Niels Chr.
- Journal of Magnetic Resonance, Vol. 213, Issue 2
Works referencing / citing this record:
19 F Magic Angle Spinning Dynamic Nuclear Polarization Enhanced NMR Spectroscopy
journal, April 2019
- Viger‐Gravel, Jasmine; Avalos, Claudia E.; Kubicki, Dominik J.
- Angewandte Chemie, Vol. 131, Issue 22
Mechanochemistry vs. solution growth: striking differences in bench stability of a cimetidine salt based on a synthetic method
journal, January 2018
- Ayoub, Ghada; Štrukil, Vjekoslav; Fábián, László
- CrystEngComm, Vol. 20, Issue 45
19 F Magic Angle Spinning Dynamic Nuclear Polarization Enhanced NMR Spectroscopy
journal, May 2019
- Viger‐Gravel, Jasmine; Avalos, Claudia E.; Kubicki, Dominik J.
- Angewandte Chemie International Edition, Vol. 58, Issue 22