We report pulse sequences for the sensitivity enhancement of magic-angle spinning and multiple-quantum magic-angle spinning spectra of spin-72 systems. Sensitivity enhancement is obtained with the use of fast amplitude-modulated (FAM) radiofrequency pulses. In one-dimensional magic-angle spinning experiments, signal enhancement of 3 is obtained by a FAM pulse followed by a soft 90 degrees pulse. In two-dimensional multiple-quantum magic-angle spinning experiments, FAM pulses are used for both the excitation of multiple-quantum coherences and for their conversion into observable single-quantum coherences. The observed signal enhancements are 2.2 in 3Q experiments, 3.1 in 5Q experiments, and 4.1 in 7Q experiments, compared to the conventional two-pulse scheme. The pulse schemes are demonstrated on the 45Sc NMR of Sc2(SO4)3 x 5H2O and the 139La NMR of LaAlO3. We also demonstrate the generation of FAM pulses by double-frequency irradiation.
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http://dx.doi.org/10.1016/s1090-7807(03)00159-9 | DOI Listing |
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).
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January 2025
Materials Science and Engineering Program, The Graduate School, Florida State University 2005 Levy Ave. Tallahassee FL 32310 USA
Solid electrolytes (SEs) are crucial for advancing next-generation rechargeable battery technologies, but their commercial viability is partially limited by expensive precursors, unscalable synthesis, or low ionic conductivity. Lithium tetrahaloaluminates offer an economical option but exhibit low Li conductivities with high activation energy barriers. This study reports the synthesis of lithium aluminum chalcohalide (LiAlClS) using inexpensive precursors one-step mechanochemical milling.
View Article and Find Full Text PDFACS Appl Mater Interfaces
January 2025
State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Science, Beijing 100085, China.
In solid-state nuclear magnetic resonance (ssNMR) spectroscopy, fast magic angle spinning (MAS) is a potent technique that efficiently reduces line broadening and makes it possible to probe structural details of biological systems in high resolution. However, its utilization in studying complex heterogeneous biomaterials such as bone in their native state has been limited. The present study has demonstrated the feasibility of acquiring two-dimensional (2D) H-H correlation spectra for native bone using multiple-quantum/single-quantum correlation experiments (MQ/SQ) at fast MAS (70 kHz).
View Article and Find Full Text PDFNat Commun
December 2024
Institut des Sciences et Ingénierie Chimiques, École Polytechnique Fédérale de Lausanne (EPFL), CH-1015, Lausanne, Switzerland.
While H-H J-couplings are the cornerstone of all spectral assignment methods in solution-state NMR, they are yet to be observed in solids. Here we observe H-H J-couplings in plastic crystals of (1S)-(-)-camphor in solid-state NMR at magic angle spinning (MAS) rates of 100 kHz and above. This is enabled in this special case because the intrinsic coherence lifetimes at fast MAS rates become longer than the inverse of the H-H J couplings.
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