Solid state nuclear magnetic resonance最新文献

{"title":"1H/13C/15N triple-resonance experiments for structure determinaton of membrane proteins by oriented-sample NMR","authors":"Joel Lapin,&nbsp;Emmanuel O. Awosanya,&nbsp;Richard J.A. Esteves,&nbsp;Alexander A. Nevzorov","doi":"10.1016/j.ssnmr.2020.101701","DOIUrl":"10.1016/j.ssnmr.2020.101701","url":null,"abstract":"<div><p>The benefits of triple-resonance experiments for structure determination of macroscopically oriented membrane proteins by solid-state NMR are discussed. While double-resonance ¹H/¹⁵<span>N experiments are effective for structure elucidation of alpha-helical domains, extension of the method of oriented samples to more complex topologies and assessing side-chain conformations necessitates further development of triple-resonance (</span>¹H/¹³C/¹⁵N) NMR pulse sequences. Incorporating additional spectroscopic dimensions involving ¹³C spin-bearing nuclei, however, introduces essential complications arising from the wide frequency range of the ¹H-¹³<span>C dipolar couplings and </span>¹³<span>C CSA (&gt;20 ​kHz), and the presence of the </span>¹³C-¹³C homonuclear dipole-dipole interactions. The recently reported ROULETTE–CAHA pulse sequence, in combination with the selective z-filtering, can be used to evolve the structurally informative ¹H-¹³<span>C dipolar coupling arising from the aliphatic carbons while suppressing the signals from the carbonyl and methyl regions. Proton-mediated magnetization transfer under mismatched Hartman-Hahn conditions (MMHH) can be used to correlate </span>¹³C and ¹⁵N nuclei in such triple-resonance experiments for the subsequent ¹⁵<span>N detection. The recently developed pulse sequences are illustrated for n-acetyl Leucine<span> (NAL) single crystal and doubly labeled Pf1 coat protein reconstituted in magnetically aligned bicelles. An interesting observation is that in the case of </span></span>¹⁵N-labeled NAL measured at ¹³C natural abundance, the triple (¹H/¹³C/¹⁵N) MMHH scheme predominantly gives rise to long-range intermolecular magnetization transfers from ¹³C to ¹⁵N spins; whereas direct Hartmann-Hahn ¹³C/¹⁵N transfer is entirely intramolecular. The presented developments advance NMR of oriented samples for structure determination of membrane proteins and liquid crystals.</p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":null,"pages":null},"PeriodicalIF":3.2,"publicationDate":"2021-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ssnmr.2020.101701","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"38661792","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}

{"title":"Hyperpolarisation techniques","authors":"Ryan E. Mewis","doi":"10.1039/9781839164965-00151","DOIUrl":"https://doi.org/10.1039/9781839164965-00151","url":null,"abstract":"","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":null,"pages":null},"PeriodicalIF":3.2,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86793160","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}

{"title":"Applications of solid-state NMR spectroscopy in environmental science","authors":"Qian Wang,&nbsp;Ulla Gro Nielsen","doi":"10.1016/j.ssnmr.2020.101698","DOIUrl":"10.1016/j.ssnmr.2020.101698","url":null,"abstract":"<div><p><span><span>Environmental science is an interdisciplinary field, which integrates chemical, physical, and biological sciences to study environmental problems and human impact on the environment. This article highlights the use of solid-state NMR spectroscopy (SSNMR) in studies of environmental processes and remediation with examples from both laboratory studies and samples collected in the field. The contemporary topics presented include soil </span>chemistry, environmental remediation (e.g., heavy metals and </span>radionuclides removal, carbon dioxide mineralization), and phosphorus recovery. SSNMR is a powerful technique, which provides atomic-level information about speciation in complex environmental samples as well as the interactions between pollutants and minerals/organic matter on different environmental interfaces. The challenges in the application of SSNMR in environmental science (e.g., measurement of paramagnetic nuclei and low-gamma nuclei) are also discussed, and perspectives are provided for the future research efforts.</p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":null,"pages":null},"PeriodicalIF":3.2,"publicationDate":"2020-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ssnmr.2020.101698","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"38558086","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}

{"title":"Structural and functional synthesis of the continuous wave NQR temperature sensor with increased conversion linearity","authors":"A. Samila ,&nbsp;I. Safronov ,&nbsp;O. Hotra","doi":"10.1016/j.ssnmr.2020.101700","DOIUrl":"10.1016/j.ssnmr.2020.101700","url":null,"abstract":"<div><p><span><span><span>The paper describes development of the detailed structure and circuit diagrams of the continuous wave NQR </span>temperature sensor with increased conversion linearity. It is experimentally established that at amplitude modulation of 40% and change of input voltage in the range of 20–1000 ​mV, the circuit of a symmetric marginal </span>oscillator<span> with a linear active demodulator provides better linearity of transfer characteristic than the circuits of asymmetric marginal oscillators with JFET<span> or diode detectors. As a thermometric substance of the proposed NQR sensor, copper oxide Cu</span></span></span>₂O was used, which is characterized by a strong temperature dependence of the resonance frequency of ⁶³Cu NQR. In contrast to ³⁵Cl NQR in KClO₃<span>, for cuprous oxide the temperature dependence of </span>⁶³<span>Сu NQR frequency in the frequency range 26.621–25.658 ​MHz is linear in the temperature range 100–390 ​K. It is experimentally confirmed that the use of a low mass sample (less than 200 ​mg) as a thermometric substance of the proposed NQR sensor is quite sufficient for successfully observation of the resonance line at the SNR equal to 9.1 ​dB.</span></p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":null,"pages":null},"PeriodicalIF":3.2,"publicationDate":"2020-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ssnmr.2020.101700","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"38620538","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}

{"title":"The 1H T1 dispersion curve of fentanyl citrate to identify NQR parameters","authors":"Michael W. Malone ,&nbsp;Michelle A. Espy ,&nbsp;Sun He ,&nbsp;Michael T. Janicke ,&nbsp;Robert F. Williams","doi":"10.1016/j.ssnmr.2020.101697","DOIUrl":"10.1016/j.ssnmr.2020.101697","url":null,"abstract":"<div><p>We report the ¹H <span><math><mrow><msub><mi>T</mi><mn>1</mn></msub></mrow></math></span> dispersion curve between 0 and 5 ​MHz for the synthetic opioid fentanyl citrate (C₂₈H₃₆N₂O₈). The structures in the curve can be used to estimate the ¹⁴<span>N nuclear quadrupole resonance (NQR) frequencies of the material. Density functional theory predictions of the NQR parameters of several fentanyl citrate compounds are also reported. The predictions for the aniline nitrogen are consistent with structures in the observed </span><span><math><mrow><msub><mi>T</mi><mn>1</mn></msub></mrow></math></span> data. To help interpret the fentanyl citrate results the <span><math><mrow><msub><mi>T</mi><mn>1</mn></msub></mrow></math></span><span> dispersion curve for the explosive ammonium nitrate is also presented.</span></p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":null,"pages":null},"PeriodicalIF":3.2,"publicationDate":"2020-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ssnmr.2020.101697","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"38504569","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}

{"title":"Iterative baseline correction algorithm for dead time truncated one-dimensional solid-state MAS NMR spectra","authors":"Maxime Yon,&nbsp;Franck Fayon,&nbsp;Dominique Massiot,&nbsp;Vincent Sarou-Kanian","doi":"10.1016/j.ssnmr.2020.101699","DOIUrl":"10.1016/j.ssnmr.2020.101699","url":null,"abstract":"<div><p><span><span>We present an algorithm suitable for automatically correcting rolling baseline coming from time-domain truncation induced by the dead time in pulse-acquire one-dimensional MAS </span>NMR spectra<span>. It relies on an iterative estimation of the baseline restricted in the time-domain by the dead time duration combined with a histogram filter allowing adaptive selection of the baseline points. This method does not make any assumption regarding the NMR resonances line shapes or widths and does not modify the acquired free induction decay points. This makes it suitable for accurate deconvolution and quantification of single-pulse MAS NMR spectra. The baseline correction accuracy is evaluated on synthetic solid-state spectra of </span></span>¹⁹F, ⁷¹Ga, and ²³Na by comparing the fitted baseline to the theoretical one. The versatility of the algorithm is also exemplified on three additional solid-state spectra of ²³Na and ⁷¹Ga. The algorithm is made available to the community through a user-friendly standalone Matlab® application.</p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":null,"pages":null},"PeriodicalIF":3.2,"publicationDate":"2020-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ssnmr.2020.101699","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"38601561","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}

{"title":"A method for fast field settling in cryogen-free superconducting magnets for NMR","authors":"Eugeny Kryukov,&nbsp;Yury Bugoslavsky,&nbsp;Angel Joaquin Perez Linde,&nbsp;Thomas Holubar,&nbsp;Stephen Burgess,&nbsp;David Marlow,&nbsp;Jeremy Good","doi":"10.1016/j.ssnmr.2020.101684","DOIUrl":"10.1016/j.ssnmr.2020.101684","url":null,"abstract":"<div><p>We propose a fast algorithm to energise a cryogen free magnet to a highly persistent state. A decay rate as low as 0.021 ​ppm/h can be achieved in less than an hour after reaching the target field. The decay rate drops further to 0.0004 ​ppm/h in the following 48 ​h. This procedure can be applied at different values of target field, which makes it feasible to use a single magnet for study of various NMR lines at different fields. The mechanism of establishing a highly stable magnetic field can be understood on the basis of the magnetic properties<span><span> of the superconducting wire, which were studied using a vibrating sample </span>magnetometer. The results confirm the high quality of the superconducting wire and joints.</span></p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":null,"pages":null},"PeriodicalIF":3.2,"publicationDate":"2020-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ssnmr.2020.101684","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"38427607","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}

{"title":"In-situ reaction monitoring of a mechanochemical ball mill reaction with solid state NMR","authors":"Jan Gerrit Schiffmann ,&nbsp;Franziska Emmerling ,&nbsp;Inês C.B. Martins ,&nbsp;Leo Van Wüllen","doi":"10.1016/j.ssnmr.2020.101687","DOIUrl":"10.1016/j.ssnmr.2020.101687","url":null,"abstract":"<div><p>We present an approach towards the <em>in situ</em><span> solid state NMR<span><span> monitoring of mechanochemical reactions in a ball mill. A miniaturized vibration ball mill is integrated into the measuring coil of a home-built solid state NMR probe, allowing for static solid state NMR measurements during the mechanochemical reaction within the vessel. The setup allows to quantitatively follow the product evolution of a prototypical mechanochemical reaction, the formation of zinc phenylphosphonate from zinc acetate and phenylphosphonic acid. </span>MAS<span> NMR investigations on the final reaction mixture confirmed a reaction yield of 89% in a typical example. Thus, NMR spectroscopy may in the future provide complementary information about reaction mechanisms of mechanochemical reactions and team up with other analytical methods which have been employed to follow reactions </span></span></span><em>in situ</em><span>, such as Raman spectroscopy or X-ray diffraction.</span></p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":null,"pages":null},"PeriodicalIF":3.2,"publicationDate":"2020-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ssnmr.2020.101687","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"38360232","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}

{"title":"Combining fast magic angle spinning dynamic nuclear polarization with indirect detection to further enhance the sensitivity of solid-state NMR spectroscopy","authors":"Zhuoran Wang ,&nbsp;Michael P. Hanrahan ,&nbsp;Takeshi Kobayashi ,&nbsp;Frédéric A. Perras ,&nbsp;Yunhua Chen ,&nbsp;Frank Engelke ,&nbsp;Christian Reiter ,&nbsp;Armin Purea ,&nbsp;Aaron J. Rossini ,&nbsp;Marek Pruski","doi":"10.1016/j.ssnmr.2020.101685","DOIUrl":"10.1016/j.ssnmr.2020.101685","url":null,"abstract":"<div><p><span><span><span>Dynamic nuclear polarization (DNP) and indirect detection are two commonly applied approaches for enhancing the sensitivity of solid-state NMR spectroscopy. However, their use in tandem has not yet been investigated. With the advent of low-temperature fast </span>magic angle spinning (MAS) probes with 1.3-mm diameter rotors capable of MAS at 40 ​kHz it becomes feasible to combine these two techniques. In this study, we performed DNP-enhanced 2D indirectly detected </span>heteronuclear correlation (idHETCOR) experiments on </span>¹³C, ¹⁵N, ¹¹³Cd and ⁸⁹<span>Y nuclei in functionalized mesoporous silica<span>, CdS nanoparticles, and Y</span></span>₂O₃<span><span><span> nanoparticles. The sensitivity of the 2D idHETCOR experiments was compared with those of DNP-enhanced directly-detected 1D cross polarization (CP) and 2D </span>HETCOR experiments performed with a standard 3.2-mm rotor. Due to low CP </span>polarization transfer<span> efficiencies and large proton linewidth, the sensitivity gains achieved by indirect detection alone were lower than in conventional (non-DNP) experiments. Nevertheless, despite the smaller sample volume the 2D idHETCOR experiments showed better absolute sensitivities than 2D HETCOR experiments for nuclei with the lowest gyromagnetic ratios. For </span></span>⁸⁹Y, 2D idHETCOR provided 8.2 times better sensitivity than the 1 D⁸⁹Y-detected CP experiment performed with a 3.2-mm rotor.</p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":null,"pages":null},"PeriodicalIF":3.2,"publicationDate":"2020-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ssnmr.2020.101685","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"38381848","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}

{"title":"Tailoring NMR experiments for structural characterization of amorphous biological solids: A practical guide","authors":"John E. Kelly ,&nbsp;Christine Chrissian ,&nbsp;Ruth E. Stark","doi":"10.1016/j.ssnmr.2020.101686","DOIUrl":"10.1016/j.ssnmr.2020.101686","url":null,"abstract":"<div><p><span>Many interesting solid-state targets for biological research do not form crystalline structures; these materials include intrinsically disordered proteins, plant biopolymer<span> composites, cell-wall polysaccharides, and </span></span>soil organic matter<span><span>. The absence of aligned repeating structural elements and atomic-level rigidity presents hurdles to achieving structural elucidation and obtaining functional insights. We describe strategies for adapting several solid-state NMR methods to determine the molecular structures and compositions of these </span>amorphous biosolids.</span></p><p>The main spectroscopic problems in studying amorphous structures by NMR are over/under-sampling of the spin signals and spectral complexity. These problems arise in part because amorphous biosolids typically contain a mix of rigid and mobile domains, making it difficult to select a single experiment or set of acquisition conditions that fairly represents all nuclear spins in a carbon-based organic sample. These issues can be addressed by running hybrid experiments, such as using direct excitation alongside cross polarization-based methods, to develop a more holistic picture of the macromolecular system. In situations of spectral crowding or overlap, the structural elucidation strategy can be further assisted by coupling ¹³C spins to nuclei such as ¹⁵N, filtering out portions of the spectrum, highlighting individual moieties of interest, and adding a second or third spectral dimension to an NMR experiment in order to spread out the resonances and link them pairwise through space or through bonds. We discuss practical aspects and illustrations from the recent literature for 1D experiments that use cross or direct polarization and both homo- and heteronuclear 2D and 3D solid-state NMR experiments.</p></div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":null,"pages":null},"PeriodicalIF":3.2,"publicationDate":"2020-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ssnmr.2020.101686","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"38353990","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}