Freezing is essential for the stability of biological drug substances and products, particularly in frozen solution formulations and during the primary drying of lyophilized preparations. However, the unfrozen segment within the frozen matrix can alter solute concentration, ionic strength, and stabilizer crystallization, posing risks of increased biophysical instability and faster chemical degradation. While quantifying the unfrozen water content is important for designing stable...
Resolution in Cryogenic Solid State NMR: Challenges and Solutions
Resolution in Cryogenic Solid State NMR: Challenges and Solutions
Abstract
NMR at cryogenic temperatures has the potential to provide rich site-specific details regarding biopolymer structure, function, and mechanistic intermediates. Broad spectral lines compared with room temperature NMR can sometimes present practical challenges. A number of hypotheses regarding the origins of line broadening are explored. One frequently considered explanation is the presence of inhomogeneous conformational distributions. Possibly these arise when the facile characteristic motions that occur near room...
nmrlearner
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10-18-2023 06:17 AM
[NMR paper] Resolution in Cryogenic Solid State NMR: Challenges and Solutions
Resolution in Cryogenic Solid State NMR: Challenges and Solutions
NMR at cryogenic temperatures has the potential to provide rich site-specific details regarding biopolymer structure, function, and mechanistic intermediates. Broad spectral lines compared with room temperature NMR can sometimes present practical challenges. A number of hypotheses regarding the origins of line broadening are explored. One frequently considered explanation is the presence of inhomogeneous conformational distributions. Possibly these arise when the facile characteristic motions...
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nmrlearner
Journal club
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10-18-2023 06:17 AM
Solid State Properties of Pharmaceutical Materials
Solid State Properties of Pharmaceutical Materials
http://media.wiley.com/product_data/coverImage/05/11181453/1118145305.jpgPresents a detailed discussion of important solid-state properties, methods, and applications of solid-state analysisIllustrates the various phases or forms that solids can assume and discussesvarious issues related to the relative stability of solid forms and tendencies to undergo transformationCovers key methods of solid state analysis including X-ray powder diffraction, thermal analysis, microscopy, spectroscopy, and solid state NMRReviews critical physical...
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05-18-2017 03:23 PM
Amplifying dynamic nuclear polarization of frozen solutions by incorporating dielectric particles
From The DNP-NMR Blog:
Amplifying dynamic nuclear polarization of frozen solutions by incorporating dielectric particles
Kubicki, D.J., et al., Amplifying dynamic nuclear polarization of frozen solutions by incorporating dielectric particles. J Am Chem Soc, 2014. 136(44): p. 15711-8.
http://www.ncbi.nlm.nih.gov/pubmed/25285480
nmrlearner
News from NMR blogs
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11-10-2014 10:59 PM
Paramagnet induced signal quenching in MAS-DNP experiments in frozen homogeneous solutions
From The DNP-NMR Blog:
Paramagnet induced signal quenching in MAS-DNP experiments in frozen homogeneous solutions
Corzilius, B., et al., Paramagnet induced signal quenching in MAS-DNP experiments in frozen homogeneous solutions. J Magn Reson, 2014. 240(0): p. 113-23.
http://www.ncbi.nlm.nih.gov/pubmed/24394190
nmrlearner
News from NMR blogs
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05-07-2014 03:14 PM
[Question from NMRWiki Q&A forum] Relative quantification (residual solvents)
Relative quantification (residual solvents)
Hi All,
I've been trying to get a clear answer to this question for a while now, but can't seem to get a definitive answer. My approach is following the method described in "Practical NMR for organic chemists" by John Hollerton and Steve Richards. I don't take any issue with this method, by only problem is that it gives a WILDLY different answer to the one I obtain when I do NMR quantification in TopSpin... this is a big problem, since often we are interested in the % of unwanted molecules in our samples.
Let me give you a simplified...
nmrlearner
News from other NMR forums
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10-31-2013 12:05 AM
[NMR paper] Effects of a type I antifreeze protein (AFP) on the melting of frozen AFP and AFP+solute aqueous solutions studied by NMR microimaging experiment.
Effects of a type I antifreeze protein (AFP) on the melting of frozen AFP and AFP+solute aqueous solutions studied by NMR microimaging experiment.
Related Articles Effects of a type I antifreeze protein (AFP) on the melting of frozen AFP and AFP+solute aqueous solutions studied by NMR microimaging experiment.
J Biol Phys. 2013 Jan;39(1):131-44
Authors: Ba Y, Mao Y, Galdino L, Günsen Z
Abstract
The effects of a type I AFP on the bulk melting of frozen AFP solutions and frozen AFP+solute solutions were studied through an NMR...
nmrlearner
Journal club
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07-19-2013 09:20 PM
[NMR paper] Solid-state NMR studies of pharmaceutical solids in polymer matrices.
Solid-state NMR studies of pharmaceutical solids in polymer matrices.
Related Articles Solid-state NMR studies of pharmaceutical solids in polymer matrices.
Anal Bioanal Chem. 2004 Mar;378(6):1504-10
Authors: Lubach JW, Padden BE, Winslow SL, Salsbury JS, Masters DB, Topp EM, Munson EJ
Biodegradable drug-delivery systems can be formulated to release drug for hours to years and have been used for the controlled release of medications in animals and humans. An important consideration in developing a drug-delivery matrix is knowledge of the...
Quantification of Residual Water in Pharmaceutical Frozen Solutions via (1)H Solid-state NMR
Linear Mode
