Article
Chemistry, Multidisciplinary
Diego Gauto, Ons Dakhlaoui, Ildefonso Marin-Montesinos, Sabine Hediger, Gael De Paepe
Summary: High-field dynamic nuclear polarization is expanding the applications of solid-state NMR in surface chemistry, materials science, and structural biology. Targeted DNP approaches, where paramagnets are specifically located on biomolecular systems, show potential for improving NMR sensitivity without the need for glass-forming DNP matrices. This technique is particularly useful for studying diluted biomolecular systems like membrane proteins in their lipidic environment and extracting structural information through paramagnetic relaxation enhancement.
Article
Chemistry, Physical
Yu Wang, Kazuyuki Takeda
Summary: In this study, we explore the transfer of magnetization between different nuclear spin species in solid-state nuclear magnetic resonance using a technique called cross-polarization (CP). This technique involves applying radiofrequency irradiation that simultaneously induces nutations around orthogonal axes. We introduce the concept of DOuble NUTation (DONUT), which represents the nutation frame and facilitates polarization transfer through the development of the zero-quantum or double-quantum secular component of the heteronuclear dipolar interaction.
PHYSICAL CHEMISTRY CHEMICAL PHYSICS
(2023)
Article
Chemistry, Multidisciplinary
Lixin Liang, Yi Ji, Zhenchao Zhao, Caitlin M. Quinn, Xiuwen Han, Xinhe Bao, Tatyana Polenova, Guangjin Hou
Summary: The phase modulated rotary resonance (PMRR) technique allows for the reintroduction of heteronuclear dipolar couplings while suppressing other interactions under a wide range of MAS conditions, with robust performance.
Article
Chemistry, Physical
Pravin P. Taware, Mukul G. Jain, Sreejith Raran-Kurussi, Vipin Agarwal, P. K. Madhu, Kaustubh R. Mote
Summary: Proteins rely on conformational changes to carry out function, and measuring these changes can provide insight into their function. In this study, the researchers combined different strategies to measure dipole-dipole couplings in nondeuterated systems at a high MAS frequency of 100 kHz. These strategies allow for the access of dipolar order parameters in a variety of systems at increasingly fast MAS frequencies.
JOURNAL OF PHYSICAL CHEMISTRY LETTERS
(2023)
Article
Biochemistry & Molecular Biology
Marta Bonaccorsi, Tanguy Le Marchand, Guido Pintacuda
Summary: Magic-Angle Spinning Nuclear Magnetic Resonance (MAS NMR) is a rapidly developing technique that complements solution NMR, X-ray crystallography, and electron microscopy for the biophysical characterization of microcrystalline, poorly crystalline or disordered protein samples. MAS NMR is ideal for investigating both structures and dynamics, and has been increasingly applied in structural biology research in recent years to describe conformational dynamics in various systems.
CURRENT OPINION IN STRUCTURAL BIOLOGY
(2021)
Review
Chemistry, Physical
Bianca Chandler, Lauren Todd, Steven O. Smith
Summary: G protein-coupled receptors (GPCRs) are a class of transmembrane proteins with a simple structure that can recognize diverse chemical signals. There are over 800 GPCRs encoded in the human genome, serving as receptors for vision, smell, taste, and other physiological processes. While protein crystallography and electron cryo-microscopy have provided high-resolution structures of GPCRs, the structural changes induced by ligand or drug binding to stabilize active or inactive conformations are often subtle. NMR spectroscopy can provide insights into the local structure, dynamics, and activation pathways of GPCRs, capturing intermediate states and low-population conformations. Solid-state magic angle spinning NMR has been used to study the structure and activation mechanisms of GPCRs, particularly in the diverse class A family. This review highlights the application of solid-state and solution-state NMR spectroscopy in understanding the activation of different GPCR classes and subfamilies by their ligands and the modulation of GPCR activation by small molecule drugs. (c) 2021 Elsevier B.V. All rights reserved.
PROGRESS IN NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY
(2022)
Article
Biochemical Research Methods
Andrea Bertarello, Pierrick Berruyer, Urban Skantze, Samiksha Sardana, Malvika Sardana, Charles S. Elmore, Markus Schade, Elisabetta Chiarparin, Staffan Schantz, Lyndon Emsley
Summary: Dynamic nuclear polarization (DNP) significantly enhances the sensitivity of MAS NMR, but cross polarization (CP) is usually not quantitative. Research shows that absolute quantification in MAS DNP NMR is possible under DNP conditions, with errors below 10%.
JOURNAL OF MAGNETIC RESONANCE
(2021)
Article
Chemistry, Physical
Zhengfeng Zhang, Yongchao Su, Hang Xiao, Jun Yang
Summary: Long-range heteronuclear correlation poses a challenge in solid-state NMR, but a selective method called hetSPR has been proposed to enhance desired correlations and suppress unwanted ones. This user-friendly method has been shown to effectively enhance the long-range correlation in a pharmaceutical drug.
JOURNAL OF PHYSICAL CHEMISTRY LETTERS
(2022)
Article
Biochemical Research Methods
Daniel Banks, Brian Michael, Natalie Golota, Robert G. Griffin
Summary: This paper discusses the use of 3D printing and rapid prototyping methods to fabricate 3.2 mm stators and drive caps for NMR experiments. With the assistance of CAD software, these components can be produced at a fraction of the cost of commercial parts, while demonstrating comparable performance to commercially available systems.
JOURNAL OF MAGNETIC RESONANCE
(2022)
Article
Biochemical Research Methods
Evgeny Nimerovsky, Stefan Becker, Loren B. Andreas
Summary: In this study, we investigate the windowed sequence for cross polarization (wCP) and find that it has additional matching conditions compared to traditional cross polarization. By considering the flip angle of the pulse, we observe a striking similarity between wCP and CP transfer conditions. Using spin-1/2 formalism and average Hamiltonian theory, we derive an analytical approximation that matches these observed transfer conditions. Data recorded at spectrometers with different external magnetic fields show that these transfers and the selectivity of CP are related to flip angle (average nutation).
JOURNAL OF MAGNETIC RESONANCE
(2023)
Article
Chemistry, Analytical
Alan Wong
Summary: High-Resolution Magic-Angle Spinning (HRMAS) NMR spectroscopy is considered an essential technique in metabolomics for assessing the biochemical composition of tissue samples. HRMAS localized profiling shows promise for spatial resolution of metabolic profiles within the sampling tissues.
ANALYTICAL METHODS
(2023)
Review
Chemistry, Physical
Kai Xue, Riddhiman Sarkar, Zdenek Tosner, Bernd Reif
Summary: Proton detection in solid state NMR is continuously advancing, and current achievements include the necessity of deuteration for optimal spectral quality, the superiority of 13CH3 isotopomers for methyl groups at high MAS frequencies, and the sensitivity enhancement with increased static magnetic field.
PROGRESS IN NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY
(2022)
Article
Chemistry, Physical
Debashis Majhi, Boris B. Kharkov, Sergey Dvinskikh
Summary: Dipolar NMR spectroscopy is a powerful analytical tool for studying structural and dynamic properties of solids at the molecular level. An approach to determine the signs of dipolar couplings in liquid crystals is presented, where sign information can be directly obtained from one-dimensional NMR spectra in samples spinning slightly off the magic angle. This method can be used to develop an experimental strategy for sign-sensitive measurements of heteronuclear dipolar couplings in anisotropic soft materials.
CHEMICAL PHYSICS LETTERS
(2021)
Article
Chemistry, Multidisciplinary
Suochang Xu, Nicholas R. Jaegers, Wenda Hu, Ja Hun Kwak, Xinhe Bao, Junming Sun, Yong Wang, Jian Zhi Hu
Summary: In this study, detailed analysis of three aluminum oxide phases was conducted using high-field NMR, revealing structural information of different aluminum sites and providing a method to quantify complex mixtures of aluminum sites in transition alumina samples. The results showcase the potential of high-field NMR in characterizing materials and identifying distinct phases within a sample.
Review
Chemistry, Multidisciplinary
Amir Goldbourt
Summary: This article introduces the application of solid-state nuclear magnetic resonance techniques in the study of molecular structure, particularly focusing on the measurement of internuclear distances between spin-1/2 and quadrupolar nuclei with spins larger than one half. Analytical expressions for recoupling curves from different techniques are provided, suggesting a coherent nomenclature for these techniques, along with discussions on handling special cases.
MAGNETIC RESONANCE IN CHEMISTRY
(2021)
