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H-F cross-polarization magic angle spinning dynamic nuclear polarization NMR investigation of advanced pharmaceutical formulations.
J Magn Reson
December 2024
Oral Product Development, Pharmaceutical Technology & Development, Operations, AstraZeneca, Gothenburg, Sweden.
A new 3.2 mm H-F-X magic angle spinning dynamic nuclear polarization NMR (MAS DNP-NMR) probe was developed with a unique coil design with separate radiofrequency channels for H excitation and C or F detection to enable acquisition of H-F cross-polarization (CP) MAS experiments, direct-detected F spectra with proton decoupling, and acquisition on C with simultaneous double decoupling on the H and 19F channels as well as H-F-C double-CP experiments under low temperature MAS DNP conditions. We use these sequences to study AZD2811, which is an active pharmaceutical ingredient (API), in its pure dry state as well as in its corresponding drug delivery formulation consisting of drug-loaded polymeric nanoparticles (PNPs).
View Article and Find Full Text PDFQuantitative LC-QToF-MS Analysis of Mycochemicals in Amanita muscaria, Psilocybe spp. (Agaricomycetes), and Consumer Products.
Int J Med Mushrooms
December 2024
National Center for Natural Products Research, Division of Pharmacognosy, Department of BioMolecular Sciences, School of Pharmacy, University of Mississippi, University, MS 38677, USA.
The psychedelic mushroom market has expanded rapidly due to changing regulations and increasing consumer demand. Product diversity now extends beyond traditional capsules and tablets to include gummies, powders, and confectionery items, complicating quality control efforts. To assess the quality and potential adulteration of Amanita musca-ria and Psilocybe cubensis-based products, a validated LC-QToF-MS method was developed.
View Article and Find Full Text PDFHyaluronic acid-based hydrogels as codelivery systems: The effect of intermolecular interactions investigated by HR-MAS and solid-state NMR Spectroscopy.
Carbohydr Polym
February 2025
Dipartimento di Chimica, Materiali e Ingegneria Chimica "G. Natta", Politecnico di Milano, via Mancinelli 7, I-20131 Milano, MI, Italy. Electronic address:
Article Synopsis
- - Hydrogels made from hyaluronic acid and agarose-carbomer are being studied for their potential to simultaneously deliver multiple drugs for different diseases, thanks to their biocompatibility and unique 3D structure.
- - The study focuses on how ethosuximide and sodium salicylate interact and diffuse within these hydrogels, using advanced techniques like NMR Spectroscopy to analyze their transport properties.
- - Findings suggest that when both drugs are loaded together, they behave similarly in their diffusion patterns, which may be influenced by drug-drug interactions, leading to a proposed trapping-release mechanism that affects how the drugs are released from the hydrogels.
Investigation of Protein Therapeutics in Frozen Conditions Using DNP MAS NMR: A Study on Pembrolizumab.
Mol Pharm
December 2024
Analytical Research and Development, Merck & Co., Inc., Rahway, New Jersey 07065, United States.
Article Synopsis
- * This study specifically investigates the high-concentration monoclonal antibody pembrolizumab (Keytruda) and its behavior in frozen solutions using advanced techniques like dynamic nuclear polarization (DNP) and solid-state NMR (ssNMR).
- * Findings reveal how these methods allow detailed analysis of the protein's structure, dynamics, and the behavior of its excipients at low temperatures, highlighting their potential for improving the stability assessment of biological drugs in frozen conditions.
An Efficient and Stable Polarizing Agent for In-Cell Magic-Angle Spinning Dynamic Nuclear Polarization NMR Spectroscopy.
J Phys Chem Lett
November 2024
Laboratory of Magnetic Resonance, Institut des Sciences et Ingénierie Chimiques, École Polytechnique Fédérale de Lausanne (EPFL), 1015 Lausanne, Switzerland.
Nuclear Magnetic Resonance (NMR) spectroscopy would be a method of choice to follow biochemical events in cells because it can analyze molecules in complex environments. However, the intrinsically low sensitivity of NMR makes in-cell measurements challenging. Dynamic Nuclear Polarization (DNP) has emerged as a method to circumvent this limitation, but most polarizing agents developed for DNP are unstable in reducing cellular environments.
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