F fast MAS (60-111 kHz) dipolar and scalar based correlation spectroscopy of organic molecules and pharmaceutical formulations.

Solid State Nucl Magn Reson

Department of Chemistry and Biochemistry, University of Delaware, Newark, DE, 19716, United States; Department of Structural Biology, University of Pittsburgh, School of Medicine, 3501 Fifth Ave., Pittsburgh, PA, 15261, United States; Pittsburgh Center for HIV Protein Interactions, University of Pittsburgh, School of Medicine, 1051 Biomedical Science Tower 3, 3501 Fifth Avenue, Pittsburgh, PA, 15261, United States. Electronic address:

Published: December 2022

AI Article Synopsis

  • F magic angle spinning (MAS) NMR spectroscopy is an advanced technique for studying fluorinated solids, and new probes enabling spinning frequencies up to 111 kHz have greatly improved its analytical capabilities.
  • The study focuses on two pharmaceuticals, mefloquine and atorvastatin calcium, highlighting how higher MAS frequencies enhance the quality of 1D and 2D experiments, making detailed analysis possible.
  • Results indicate that techniques like H decoupling and heteronuclear correlation experiments are not only feasible but also much more efficient at 100 kHz, paving the way for broader applications in chemistry and biology.

Article Abstract

F magic angle spinning (MAS) NMR spectroscopy is a powerful tool for characterization of fluorinated solids. The recent development of F MAS NMR probes, operating at spinning frequencies of 60-111 kHz, enabled analysis of systems spanning from organic molecules to pharmaceutical formulations to biological assemblies, with unprecedented resolution. Herein, we systematically evaluate the benefits of high MAS frequencies (60-111 kHz) for 1D and 2D F-detected experiments in two pharmaceuticals, the antimalarial drug mefloquine and a formulation of the cholesterol-lowering drug atorvastatin calcium. We demonstrate that H decoupling is essential and that scalar-based, heteronuclear single quantum coherence (HSQC) and heteronuclear multiple quantum coherence (HMQC) correlation experiments become feasible and efficient at the MAS frequency of 100 kHz. This study opens doors for the applications of high frequency F MAS NMR to a wide range of problems in chemistry and biology.

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Source
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC10280467PMC
http://dx.doi.org/10.1016/j.ssnmr.2022.101831DOI Listing

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