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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http://dx.doi.org/10.1016/j.ssnmr.2022.101831 | DOI Listing |
Inorg Chem
January 2025
CNRS, University of Bordeaux, Bordeaux INP, ICMCB UMR CNRS 5026, F-33600 Pessac ,France.
The diaspore-type crystalline structure is historically well-known in mineralogy, but it has also been widely studied for various applications in the field of catalysis, electrocatalysis, and batteries. However, once two anions of similar ionic size but different electronegativity, such as F and O or more precisely OH, are combined, the knowledge of the location of these two anions is of paramount importance to understand the chemical properties in relation with the generation of hydrogen bonds. Coprecipitation and hydrothermal routes were used to prepare hydroxide-fluorides that crystallize all in an orthorhombic structure with four formula units per cell.
View Article and Find Full Text PDFAngew Chem Int Ed Engl
January 2025
KU Leuven, Materials engineering, Kasteelpark Arenberg 44 bus 2450, 3001 LEUVEN Belgium, LEUVEN, BELGIUM.
Traditional polymer solid electrolytes (PSEs) suffer from low Li conductivity, poor kinetics and safety concerns. Here, we present a novel porous MOF glass gelled polymer electrolyte (PMG-GPE) prepared via a top-down strategy, which features a unique three-dimensional interconnected graded-aperture structure for efficient ion transport. Comprehensive analyses, including time-of-flight secondary ion mass spectrometry (TOF-SIMS), Solid-state 7Li magic-angle-spinning nuclear magnetic resonance (MAS-NMR), Molecular Dynamics (MD) simulations, and electrochemical tests, quantify the pore structures, revealing their relationship with ion conductivity that increases and then decreases as macropore proportion rises.
View Article and Find Full Text PDFChem Asian J
January 2025
Qingdao University of Science and Technology, College of Polymer Science and Engineering, 53 ZHENGZHOU ROAD, 266000, Qingdao, CHINA.
Constructing highly conjugated three-dimensional covalent organic frameworks (3D COFs), particularly those with luminescent features, remains a significant challenge. In this work, we successfully synthesized a 3D COF, named 3D-Py-SP-COF, using a rigid and orthogonal spirobifluorene building block for the spatial 3D structure construction and planar pyrene as luminescent units. The incorporation of the pyrene and the unique rigid 3D network structure endow 3D-Py-SP-COF with fluorescent properties.
View Article and Find Full Text PDFMethods Mol Biol
January 2025
NMR Laboratory, Chemistry Department, University of Crete, Heraklion, Crete, Greece.
High Resolution-Magic Angle Spinning (HR-MAS) solid-state NMR spectroscopy is finding increasing application in the analysis of solid foods, bypassing the need for complicated solvent extraction procedures. In the present protocol, we report a simple analytical approach based on HR-MAS NMR spectroscopy for the phenolic profiling of olive fruits, flesh, or skin. This approach allows the facile characterization of phenolic compounds in olive fruits cultivated for extra-virgin olive oil production as a function of maturation and variety, in addition to processing technology for table olives.
View Article and Find Full Text PDFAnal Chem
January 2025
School of Petrochemical Engineering, Liaoning Petrochemical University, Fushun 113001, China.
Chiral discrimination is an indispensable tool that has pivotal importance in the assignment of absolute configuration and determination of enantiomeric excess in chiral compounds. A series of enantiomerically pure -1,2-diaminocyclohexane (-DACH)-derived benzamides were first synthesized by simple chemical steps, and 14 variated derivatives have been assessed as NMR chiral solvating agents (CSAs) for discrimination of the signals of mandelic acid (MA) in H NMR analysis. The highly efficient chiral recognition of CSA on different substrates, including MAs, carboxylic acids, amino acid derivatives, and phosphoric acids (32 examples), was expanded via H, F, and P NMR spectroscopy.
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