Journal of magnetic resonance最新文献

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17O quadrupolar chemical exchange saturation transfer (Q-CEST) NMR for investigations of molecular dynamics in solids 17O四极性化学交换饱和转移(Q-CEST)核磁共振用于固体分子动力学的研究。
IF 1.9 3区 化学
Journal of magnetic resonance Pub Date : 2026-04-01 Epub Date: 2026-02-26 DOI: 10.1016/j.jmr.2026.108045
Liliya Vugmeyster , Karen Basaves , Riqiang Fu , Sean T. Holmes , Dmitry Ostrovsky
{"title":"17O quadrupolar chemical exchange saturation transfer (Q-CEST) NMR for investigations of molecular dynamics in solids","authors":"Liliya Vugmeyster ,&nbsp;Karen Basaves ,&nbsp;Riqiang Fu ,&nbsp;Sean T. Holmes ,&nbsp;Dmitry Ostrovsky","doi":"10.1016/j.jmr.2026.108045","DOIUrl":"10.1016/j.jmr.2026.108045","url":null,"abstract":"<div><div>We introduce quadrupolar chemical exchange saturation transfer (Q-CEST) for half-integer quadrupolar nuclei such as oxygen-17 as a complementary NMR tool for studies of molecular dynamics in solids. Experiments on the model compounds NaNO<sub>3</sub> and hydration water in fibrils formed by pyro-glutamate E3 Amyloid-β protein are combined with simulations and theoretical approaches to obtain parameters of molecular motions. We determine the rate constants for 3-site jumps of oxygen atoms in NaNO<sub>3</sub> and rate constants and populations of tetrahedral jumps of hydration water in the proximity to protein surface below the bulk freezing point. The detection is focused on the central transition (CT). However, during the saturation the transmitter is swept across a wide range of frequencies reaching the first satellite transitions. A detailed analysis is provided for CT Q-CEST profiles in the presence of molecular dynamics covering two dynamical transitions occurring approximately in the microsecond and nanosecond time scale ranges and paying special attention to correct inclusion of the dynamics averaging of the second order quadrupolar interaction.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"385 ","pages":"Article 108045"},"PeriodicalIF":1.9,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147367648","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Spectral-band-selective multidimensional nuclear magnetic resonance spectroscopy using broadband dipolar recoupling schemes 使用宽带偶极重耦合方案的光谱带选择性多维核磁共振波谱学。
IF 1.9 3区 化学
Journal of magnetic resonance Pub Date : 2026-03-01 Epub Date: 2026-02-04 DOI: 10.1016/j.jmr.2026.108022
Edward P. Saliba , Sarah A. Overall , Alexander B. Barnes
{"title":"Spectral-band-selective multidimensional nuclear magnetic resonance spectroscopy using broadband dipolar recoupling schemes","authors":"Edward P. Saliba ,&nbsp;Sarah A. Overall ,&nbsp;Alexander B. Barnes","doi":"10.1016/j.jmr.2026.108022","DOIUrl":"10.1016/j.jmr.2026.108022","url":null,"abstract":"<div><div>Nuclear magnetic resonance (NMR) spectroscopy is an important analytical tool for probing molecular structures and interactions. For high complexity samples, multidimensional spectroscopy is essential for improving the resolution of NMR data. However, multidimensional experiments cost significant experimental time which scales with the number of indirect points. This is particularly challenging when dealing with highly dispersed nuclei, such as <sup>13</sup>C, due to the large chemical shift range, with large regions that are spectrally empty. Herein, we describe a method for limiting the spectral width of dipolar based multidimensional NMR experiments in the indirect dimension in a manner that can be easily integrated into relaxation and distance measuring schemes. We demonstrate the acquisition of narrow strips of broadband homonuclear recoupling <sup>13</sup>C-<sup>13</sup>C correlation spectra on a range of biomolecular and cellular samples, allowing targeted acquisition of high-resolution spectra of the region of interest with a significant reduction in the acquisition time. We also demonstrate the use of the spectral-band-selective method for allowing fast acquisition of RFDR build-up experiments. The band-selective method is easy to implement in any dipolar-based multidimensional pulse sequence by an addition of one pulse per band-selected indirect dimension and a slight modification of the phase cycle.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"384 ","pages":"Article 108022"},"PeriodicalIF":1.9,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146145366","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Heisenberg spin exchange and relaxation dynamics in EPR oximetry: A photoinduced transition from non-adiabatic rapid-sweeps to the rapid-scan regime EPR血氧测定中的海森堡自旋交换和弛豫动力学:从非绝热快速扫描到快速扫描的光诱导转变
IF 1.9 3区 化学
Journal of magnetic resonance Pub Date : 2026-03-01 Epub Date: 2026-01-27 DOI: 10.1016/j.jmr.2026.108021
Florian Johannsen, Malte Drescher
{"title":"Heisenberg spin exchange and relaxation dynamics in EPR oximetry: A photoinduced transition from non-adiabatic rapid-sweeps to the rapid-scan regime","authors":"Florian Johannsen,&nbsp;Malte Drescher","doi":"10.1016/j.jmr.2026.108021","DOIUrl":"10.1016/j.jmr.2026.108021","url":null,"abstract":"<div><div>Rapid-scan electron paramagnetic resonance spectroscopy (RS EPR) has emerged as a powerful tool to monitor light-induced processes accompanied by changes of the EPR lineshape and is frequently used for measuring local oxygen concentrations. Here we use LiPc (lithium phthalocyanine) and CTPO (3-Carbamoyl-2,2,5,5-tetramethyl-3-pyrrolin-1-oxyl) as spin probes and demonstrate control over the oxygen partial pressure through a photochemical reaction. The resulting changes in <span><math><msub><mrow><mtext>pO</mtext></mrow><mrow><mn>2</mn></mrow></msub></math></span> manifest as characteristic distortions of the EPR lineshape and reveal how Heisenberg spin exchange influences relaxation dynamics. As a proof-of-concept, we investigate photopolymerization at reduced oxygen levels. These results highlight the potential of RS for studying oxidation processes in biochemical systems.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"384 ","pages":"Article 108021"},"PeriodicalIF":1.9,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146102407","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Automated frequency tuning for broadband NMR spectroscopy: A LabVIEW-based solution 宽带核磁共振光谱的自动频率调谐:基于labview的解决方案
IF 1.9 3区 化学
Journal of magnetic resonance Pub Date : 2026-03-01 Epub Date: 2026-02-03 DOI: 10.1016/j.jmr.2026.108020
Yanan Li , Hadrien Mayaffre , Florian Bärtl , Steffen Krämer , Mladen Horvatić
{"title":"Automated frequency tuning for broadband NMR spectroscopy: A LabVIEW-based solution","authors":"Yanan Li ,&nbsp;Hadrien Mayaffre ,&nbsp;Florian Bärtl ,&nbsp;Steffen Krämer ,&nbsp;Mladen Horvatić","doi":"10.1016/j.jmr.2026.108020","DOIUrl":"10.1016/j.jmr.2026.108020","url":null,"abstract":"<div><div>This work introduces an automated frequency-tuning system for Nuclear Magnetic Resonance (NMR) spectroscopy. Developed using LabVIEW software, the system is designed for the top-tuning configurations of NMR probes commonly used in solid-state physics for broad-frequency-sweep spectra at very low temperatures and/or high magnetic fields. The system integrates a stepper motor, driver, phase shifter, and network analyzer to enable rapid, precise, and efficient probe tuning. Traditional manual tuning for broadband NMR is labor-intensive and time-consuming, often hindering timely data acquisition. Our automated solution significantly reduces tuning time and minimizes user intervention, thereby enhancing the efficiency and accuracy of NMR measurements. The system’s effectiveness is demonstrated with experimental <sup>63</sup>Cu and <sup>65</sup>Cu NMR results from an SrCu<sub>2</sub>(BO<sub>3</sub>)<sub>2</sub> sample in a high magnetic field. This automation is particularly valuable for streamlining research in ultra-high magnetic fields, which are exceptionally expensive to produce.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"384 ","pages":"Article 108020"},"PeriodicalIF":1.9,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146102388","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Solvent PRE and effective near surface electrostatics: theory, methods, and biological insights 溶剂PRE和有效的近表面静电:理论、方法和生物学见解。
IF 1.9 3区 化学
Journal of magnetic resonance Pub Date : 2026-03-01 Epub Date: 2025-12-04 DOI: 10.1016/j.jmr.2025.108007
Sydney Griggs, Yusuke Okuno
{"title":"Solvent PRE and effective near surface electrostatics: theory, methods, and biological insights","authors":"Sydney Griggs,&nbsp;Yusuke Okuno","doi":"10.1016/j.jmr.2025.108007","DOIUrl":"10.1016/j.jmr.2025.108007","url":null,"abstract":"<div><div>Electrostatic interactions are central to biomolecular structure, dynamics, and function, yet experimentally probing local electrostatic potentials with residue-level resolution remains challenging. Solvent paramagnetic relaxation enhancement (sPRE) offers a powerful nuclear magnetic resonance (NMR) approach to directly quantify near-surface electrostatic environments without requiring structural information. In this review, we outline the theoretical framework underlying sPRE, emphasizing recent advances in spectral density analysis, spatial decomposition, and the influence of intermolecular potentials. We discuss the effective near-surface electrostatic potential (ENS), a derived quantity that captures local electrostatic fields by comparing transverse relaxation rates induced by paramagnetic cosolutes of differing charge. Applications to proteins, nucleic acids, and intrinsically disordered systems highlight the ability of sPRE and ENS to reveal electrostatic modulation in complex biological contexts, including phase separation, ion atmosphere structure, and protein–nucleic acid interactions. We also examine current limitations and provide a theoretical basis for interpreting ENS, offering perspectives for future methodological developments in electrostatics mapping by NMR.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"384 ","pages":"Article 108007"},"PeriodicalIF":1.9,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145800915","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A high-performance ceramic volume coil for preclinical MRI 一种用于临床前MRI的高性能陶瓷体积线圈
IF 1.9 3区 化学
Journal of magnetic resonance Pub Date : 2026-02-01 Epub Date: 2026-01-23 DOI: 10.1016/j.jmr.2026.108019
Conner S. Ubert , Sergey V. Petryakov , Maciej M. Kmiec , Ryan C. O'Connell , Victor B. Kassey , Periannan Kuppusamy
{"title":"A high-performance ceramic volume coil for preclinical MRI","authors":"Conner S. Ubert ,&nbsp;Sergey V. Petryakov ,&nbsp;Maciej M. Kmiec ,&nbsp;Ryan C. O'Connell ,&nbsp;Victor B. Kassey ,&nbsp;Periannan Kuppusamy","doi":"10.1016/j.jmr.2026.108019","DOIUrl":"10.1016/j.jmr.2026.108019","url":null,"abstract":"<div><div>A novel volume radio-frequency (RF) coil built around a cylindrical ceramic dielectric (relative permittivity ε<sub>r</sub> = 270) was developed for high-field small-animal magnetic resonance imaging (MRI). Finite element simulations were used to optimize the resonator geometry, resulting in an inner diameter of 30 mm, an outer diameter of 47 mm and a length of 43 mm, which is tuned to approximately 400 MHz resonance frequency. The coil is tuned and matched solely by two inductively coupled loops, eliminating the need for lumped-element tuning and matching capacitors. In the loaded state the coil exhibits a quality factor of 105 and very uniform transmit fields, with a B<sub>1</sub> homogeneity of 98.2% in the unloaded condition. Phantom experiments show 97% signal uniformity across 0.7 mm slices and a signal-to-noise ratio (SNR) ranging from 55 to 220 along the coil axis. B<sub>1</sub> mapping confirms accurate excitation (mean actual-to-nominal flip-angle ratio = 1.05) with a coefficient of variation of 1.9%. High-resolution mouse images demonstrate that the ceramic resonator provides excellent anatomical detail, confirming its utility for preclinical MRI. This dielectric-resonator design delivers B<sub>1</sub> homogeneity comparable to or better than conventional coils while simplifying hardware, improving tuning stability and reducing RF losses, establishing it as a cost-effective and robust solution for quantitative high-field preclinical MRI.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"383 ","pages":"Article 108019"},"PeriodicalIF":1.9,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146022783","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Simple setup for in situ electrochemical electron paramagnetic resonance spectroscopy to study organic energy-storage materials 用于原位电化学电子顺磁共振波谱研究有机储能材料的简易装置
IF 1.9 3区 化学
Journal of magnetic resonance Pub Date : 2026-02-01 Epub Date: 2025-12-18 DOI: 10.1016/j.jmr.2025.108010
Anatoliy A. Vereshchagin , Maryam Seif-Eddine , Kaltum Abdiaziz , Maxie M. Roessler , Oleg V. Levin , Jan Behrends
{"title":"Simple setup for in situ electrochemical electron paramagnetic resonance spectroscopy to study organic energy-storage materials","authors":"Anatoliy A. Vereshchagin ,&nbsp;Maryam Seif-Eddine ,&nbsp;Kaltum Abdiaziz ,&nbsp;Maxie M. Roessler ,&nbsp;Oleg V. Levin ,&nbsp;Jan Behrends","doi":"10.1016/j.jmr.2025.108010","DOIUrl":"10.1016/j.jmr.2025.108010","url":null,"abstract":"<div><div>The design and application of a cost-effective, customisable electrochemical cell suitable for <em>in situ</em> X-band (9–10 GHz) Electron Paramagnetic Resonance (EPR) experiments is demonstrated. The cell is optimized for investigating electrochemical parameters of redox-active polymer films at room temperature using polar organic electrolytes. The polymer film to be studied is directly deposited onto the surface of a platinum wire acting as the working electrode. The three-electrode cylindrical cell design with mutual arrangement of the electrodes, inspired by the “ultramicroelectrode concept”, provides enhanced electrochemical response by minimizing ohmic drop while maintaining flexibility for a wide range of experimental setups. The cell performance is demonstrated using a redox conducting polymeric cathode material for organic radical batteries, namely poly[N,N″-bis(3-(4-oxy(2,2,6,6-tetramethylpiperidin-1-oxyl)butoxy)salicylidene)ethylenediiminato nickel(II)], as a test material. Continuous-wave EPR experiments using a portable benchtop spectrometer at a fixed magnetic field allow detecting the material's state of charge, initialisation of oxidation and reduction processes, as well as estimating electrochemical properties. The cell design presented here enables potentiostatic, galvanostatic, and potentiodynamic measurement modes, while offering the possibility of customisation through 3D printing and the use of various electrode materials.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"383 ","pages":"Article 108010"},"PeriodicalIF":1.9,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145789972","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Transfer of magnetization from 1H to half-integer quadrupolar nuclei in solids: comparison of different through-space INEPT variants 固体中从1H到半整数四极核的磁化转移:不同通过空间的INEPT变体的比较。
IF 1.9 3区 化学
Journal of magnetic resonance Pub Date : 2026-02-01 Epub Date: 2025-12-16 DOI: 10.1016/j.jmr.2025.108009
Lixin Liang , Yury G. Kolyagin , Julien Trébosc , Guangjin Hou , Olivier Lafon , Hiroki Nagashima , Jean-Paul Amoureux
{"title":"Transfer of magnetization from 1H to half-integer quadrupolar nuclei in solids: comparison of different through-space INEPT variants","authors":"Lixin Liang ,&nbsp;Yury G. Kolyagin ,&nbsp;Julien Trébosc ,&nbsp;Guangjin Hou ,&nbsp;Olivier Lafon ,&nbsp;Hiroki Nagashima ,&nbsp;Jean-Paul Amoureux","doi":"10.1016/j.jmr.2025.108009","DOIUrl":"10.1016/j.jmr.2025.108009","url":null,"abstract":"&lt;div&gt;&lt;div&gt;The majority of chemical elements can be observed by NMR only through half-integer quadrupolar nuclei with spin &lt;em&gt;S&lt;/em&gt; = 3/2, 5/2, 7/2 or 9/2. As a result, probing the proximities between these isotopes and protons is crucial for investigating the structure of numerous hydrogen-containing materials, including heterogeneous catalysts, pharmaceuticals, nanostructured materials, etc. These experiments must be conducted under magic-angle spinning (MAS) conditions to resolve the different chemical environments. In particular, different variants of the &lt;sup&gt;1&lt;/sup&gt;H → &lt;em&gt;S&lt;/em&gt; through-space refocused INEPT (&lt;em&gt;D&lt;/em&gt;-RINEPT) sequence have been proposed to probe long-range proximities between protons and half-integer quadrupolar nuclei. These pulse sequences differ by the employed heteronuclear dipolar recoupling scheme as well as the method used to refocus the chemical shift anisotropy of protons during the defocusing and refocusing periods. Some of the most efficient &lt;em&gt;D&lt;/em&gt;-RINEPT variants that have been reported so far, include (i) that employing the symmetry-based supercycled &lt;span&gt;&lt;math&gt;&lt;mi&gt;SR&lt;/mi&gt;&lt;msubsup&gt;&lt;mn&gt;4&lt;/mn&gt;&lt;mn&gt;1&lt;/mn&gt;&lt;mn&gt;2&lt;/mn&gt;&lt;/msubsup&gt;&lt;/math&gt;&lt;/span&gt; recoupling built from adiabatic inversion pulses incorporated into two spin-echoes and (ii) that using wPMRR (windowed Phase-Modulated Rotary Resonance) recoupling combined with two dipolar-echoes. In particular, the former has been used to enhance the sensitivity of NMR detection of quadrupolar isotopes via indirect DNP (Dynamic Nuclear Polarization) via protons. Nevertheless, there is a lack of comparative studies of these &lt;em&gt;D&lt;/em&gt;-RINEPT variants in the literature. In the present study, we introduce new variants of this general scheme, exploring the incorporation of windowed basic elements into the &lt;span&gt;&lt;math&gt;&lt;mi&gt;R&lt;/mi&gt;&lt;msubsup&gt;&lt;mn&gt;4&lt;/mn&gt;&lt;mn&gt;1&lt;/mn&gt;&lt;mn&gt;2&lt;/mn&gt;&lt;/msubsup&gt;&lt;/math&gt;&lt;/span&gt; recoupling, and the application of these novel recoupling sequences into dipolar-echo instead of spin-echo refocusing. The efficiencies of these novel &lt;em&gt;D&lt;/em&gt;-RINEPT sequences are compared with the existing ones as well as to that of CPMAS (Cross-Polarization under MAS). This experimental comparison is performed at 18.8 T with different MAS frequencies, ν&lt;sub&gt;R&lt;/sub&gt; = 10, 20, and 50 kHz, for &lt;sup&gt;1&lt;/sup&gt;H → &lt;sup&gt;27&lt;/sup&gt;Al and &lt;sup&gt;1&lt;/sup&gt;H → &lt;sup&gt;35&lt;/sup&gt;Cl polarization transfers in γ-Al&lt;sub&gt;2&lt;/sub&gt;O&lt;sub&gt;3&lt;/sub&gt; and &lt;span&gt;l&lt;/span&gt;-histidine·HCl·H&lt;sub&gt;2&lt;/sub&gt;O, respectively. The first sample features moderate &lt;sup&gt;1&lt;/sup&gt;H–&lt;sup&gt;1&lt;/sup&gt;H dipolar interactions, whereas large &lt;sup&gt;1&lt;/sup&gt;H–&lt;sup&gt;1&lt;/sup&gt;H couplings are present in the second. We demonstrate that at ν&lt;sub&gt;R&lt;/sub&gt; ≤ 20–25 kHz, the most efficient &lt;em&gt;D&lt;/em&gt;-RINEPT variant is that employing on &lt;sup&gt;1&lt;/sup&gt;H channel two spin-echoes incorporating (i) the &lt;span&gt;&lt;math&gt;&lt;mi&gt;SR&lt;/mi&gt;&lt;msubsup&gt;&lt;mn&gt;4&lt;/mn&gt;&lt;mn&gt;1&lt;/mn&gt;&lt;mn&gt;2&lt;/mn&gt;&lt;/msubsup&gt;&lt;/math&gt;&lt;/span&gt; recoupling built from adiabatic pulses, (ii) two composite pulses and (iii) continuous-wave ","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"383 ","pages":"Article 108009"},"PeriodicalIF":1.9,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145835849","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
DNP enhanced solid-state NMR of lattice-like microcrystalline protein assemblies facilitated by co-assembly with dinitroxide-tagged proteins DNP增强了晶格状微晶蛋白组装的固态核磁共振,促进了与二氮氧化合物标记的蛋白质的共组装。
IF 1.9 3区 化学
Journal of magnetic resonance Pub Date : 2026-02-01 Epub Date: 2025-12-23 DOI: 10.1016/j.jmr.2025.108011
Christian M. O'Neil, Lakshmi Bhai, Daniel W. Conroy, Christopher P. Jaroniec
{"title":"DNP enhanced solid-state NMR of lattice-like microcrystalline protein assemblies facilitated by co-assembly with dinitroxide-tagged proteins","authors":"Christian M. O'Neil,&nbsp;Lakshmi Bhai,&nbsp;Daniel W. Conroy,&nbsp;Christopher P. Jaroniec","doi":"10.1016/j.jmr.2025.108011","DOIUrl":"10.1016/j.jmr.2025.108011","url":null,"abstract":"<div><div>Dynamic nuclear polarization (DNP) enables dramatic sensitivity enhancements of solid-state nuclear magnetic resonance (NMR) spectra for biological systems to be realized via polarization transfer from unpaired electrons of a polarizing agent, typically a nitroxide biradical, to nuclear spins of the system of interest. Here, we systematically investigate the prospect of recording DNP enhanced solid-state NMR spectra of hydrated lattice-like protein assemblies within sample formulations that are free of the commonly employed glycerol-based glassy solvent matrix containing exogenous polarizing agent molecules and instead consist of isotope-enriched protein of interest co-assembled with its dinitroxide-tagged structural analog incorporated as a dopant at low concentration. As a model system we use microcrystals of <sup>13</sup>C,<sup>15</sup>N-labeled immunoglobulin-binding domain of protein G (GB1) doped with different amounts in the ∼1–16 % regime of a GB1 variant, 28R1/32R1, containing nitroxide spin labels at residues 28 and 32. For 28R1/32R1 dopant concentration of 4 %, equivalent to ca. 5 mM polarizing agent in the microcrystals, the DNP signal enhancement for <sup>13</sup>C,<sup>15</sup>N-GB1 was found to be comparable to that obtained for model amino acid <sup>13</sup>C,<sup>15</sup>N-proline in the usual glycerol/D<sub>2</sub>O/H<sub>2</sub>O matrix containing 5 mM 28R1/32R1 as the polarizing agent; further sensitivity increases were observed for 28R1/32R1 concentrations on the order of 10 %. Moreover, the spectral resolution for hydrated <sup>13</sup>C,<sup>15</sup>N-GB1 microcrystals doped with 28R1/32R1 at ∼100 K was similar to that for a microcrystal suspension in glycerol/D<sub>2</sub>O/H<sub>2</sub>O with AMUPol biradical. This sample formulation approach based on doping with dinitroxide-tagged proteins is expected to be applicable to not only protein microcrystals but also to other lattice-like or filamentous assemblies composed of small to medium-size protein subunits, and further major improvements in sensitivity can be anticipated for this approach with continued development of optimal covalent nitroxide biradical DNP polarizing agent tags.</div></div>","PeriodicalId":16267,"journal":{"name":"Journal of magnetic resonance","volume":"383 ","pages":"Article 108011"},"PeriodicalIF":1.9,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145835814","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Revisiting fluorine relaxation: a perspective on fluorine NMR in structural and dynamic studies of biomolecules 重新审视氟弛豫:氟核磁共振在生物分子结构和动力学研究中的应用。
IF 1.9 3区 化学
Journal of magnetic resonance Pub Date : 2026-02-01 Epub Date: 2025-12-07 DOI: 10.1016/j.jmr.2025.108006
Yuki Toyama , Koh Takeuchi , Ichio Shimada
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