Solid state nuclear magnetic resonance最新文献_第10页

Iterative baseline correction algorithm for dead time truncated one-dimensional solid-state MAS NMR spectra 死时间截断一维固态MAS核磁共振谱的迭代基线校正算法

IF 3.2 3区化学

Solid state nuclear magnetic resonance Pub Date : 2020-12-01 DOI: 10.1016/j.ssnmr.2020.101699

Maxime Yon, Franck Fayon, Dominique Massiot, Vincent Sarou-Kanian

{"title":"Iterative baseline correction algorithm for dead time truncated one-dimensional solid-state MAS NMR spectra","authors":"Maxime Yon, Franck Fayon, Dominique Massiot, Vincent Sarou-Kanian","doi":"10.1016/j.ssnmr.2020.101699","DOIUrl":"10.1016/j.ssnmr.2020.101699","url":null,"abstract":"<div>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 NMR spectra. 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 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.</div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"110 ","pages":"Article 101699"},"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}

引用次数: 4

The 1H T1 dispersion curve of fentanyl citrate to identify NQR parameters 利用枸橼酸芬太尼的1H T1弥散曲线识别NQR参数

IF 3.2 3区化学

Solid state nuclear magnetic resonance Pub Date : 2020-12-01 DOI: 10.1016/j.ssnmr.2020.101697

Michael W. Malone , Michelle A. Espy , Sun He , Michael T. Janicke , Robert F. Williams

引用次数: 1

Combining fast magic angle spinning dynamic nuclear polarization with indirect detection to further enhance the sensitivity of solid-state NMR spectroscopy 将快速魔角自旋动态核极化与间接探测相结合，进一步提高固态核磁共振光谱的灵敏度

IF 3.2 3区化学

Solid state nuclear magnetic resonance Pub Date : 2020-10-01 DOI: 10.1016/j.ssnmr.2020.101685

Zhuoran Wang , Michael P. Hanrahan , Takeshi Kobayashi , Frédéric A. Perras , Yunhua Chen , Frank Engelke , Christian Reiter , Armin Purea , Aaron J. Rossini , Marek Pruski

{"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 , Michael P. Hanrahan , Takeshi Kobayashi , Frédéric A. Perras , Yunhua Chen , Frank Engelke , Christian Reiter , Armin Purea , Aaron J. Rossini , Marek Pruski","doi":"10.1016/j.ssnmr.2020.101685","DOIUrl":"10.1016/j.ssnmr.2020.101685","url":null,"abstract":"<div>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 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 heteronuclear correlation (idHETCOR) experiments on 13C, 15N, 113Cd and 89Y nuclei in functionalized mesoporous silica, CdS nanoparticles, and Y2O3 nanoparticles. The sensitivity of the 2D idHETCOR experiments was compared with those of DNP-enhanced directly-detected 1D cross polarization (CP) and 2D HETCOR experiments performed with a standard 3.2-mm rotor. Due to low CP polarization transfer 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 89Y, 2D idHETCOR provided 8.2 times better sensitivity than the 1 D89Y-detected CP experiment performed with a 3.2-mm rotor.</div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"109 ","pages":"Article 101685"},"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}

引用次数: 17

Tailoring NMR experiments for structural characterization of amorphous biological solids: A practical guide 裁剪核磁共振实验的结构表征无定形生物固体:实用指南

IF 3.2 3区化学

Solid state nuclear magnetic resonance Pub Date : 2020-10-01 DOI: 10.1016/j.ssnmr.2020.101686

John E. Kelly , Christine Chrissian , Ruth E. Stark

{"title":"Tailoring NMR experiments for structural characterization of amorphous biological solids: A practical guide","authors":"John E. Kelly , Christine Chrissian , Ruth E. Stark","doi":"10.1016/j.ssnmr.2020.101686","DOIUrl":"10.1016/j.ssnmr.2020.101686","url":null,"abstract":"<div>Many interesting solid-state targets for biological research do not form crystalline structures; these materials include intrinsically disordered proteins, plant biopolymer composites, cell-wall polysaccharides, and soil organic matter. 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 amorphous biosolids.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.</div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"109 ","pages":"Article 101686"},"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}

引用次数: 17

Field-stepwise-swept QCPMG solid-state 115In NMR of indium oxide 场逐步扫描的QCPMG固态115In氧化铟核磁共振

IF 3.2 3区化学

Solid state nuclear magnetic resonance Pub Date : 2020-10-01 DOI: 10.1016/j.ssnmr.2020.101688

Kazuhiko Yamada , Takumi Yamaguchi , Ryutaro Ohashi , Shinobu Ohki , Kenzo Deguchi , Kenjiro Hashi , Atsushi Goto , Tadashi Shimizu

引用次数: 2

Recent advances in solid-state relaxation dispersion techniques 固态弛豫色散技术的最新进展

IF 3.2 3区化学

Solid state nuclear magnetic resonance Pub Date : 2020-08-01 DOI: 10.1016/j.ssnmr.2020.101665

Petra Rovó

{"title":"Recent advances in solid-state relaxation dispersion techniques","authors":"Petra Rovó","doi":"10.1016/j.ssnmr.2020.101665","DOIUrl":"10.1016/j.ssnmr.2020.101665","url":null,"abstract":"<div>This review describes two rotating-frame (<math><mrow><msub><mi>R</mi><mrow><mn>1</mn><mi>ρ</mi></mrow></msub></mrow></math>) relaxation dispersion methods, namely the Bloch-McConnell Relaxation Dispersion and the Near-rotary Resonance Relaxation Dispersion, which enable the study of microsecond time-scale conformational fluctuations in the solid state using magic-angle-spinning nuclear magnetic resonance spectroscopy. The goal is to provide the reader with key ideas, experimental descriptions, and practical considerations associated with <math><mrow><msub><mi>R</mi><mrow><mn>1</mn><mi>ρ</mi></mrow></msub></mrow></math> measurements that are needed for analyzing relaxation dispersion and quantifying conformational exchange. While the focus is on protein motion, many presented concepts can be equally well adapted to study the microsecond time-scale dynamics of other bio- (e.g. lipids, polysaccharides, nucleic acids), organic (e.g. pharmaceutical compounds), or inorganic molecules (e.g., metal organic frameworks). This article summarizes the essential contributions made by recent theoretical and experimental solid-state NMR studies to our understanding of protein motion. Here we discuss recent advances in fast MAS applications that enable the observation and atomic level characterization of sparsely populated conformational states which are otherwise inaccessible for other experimental methods. Such high-energy states are often associated with protein functions such as molecular recognition, ligand binding, or enzymatic catalysis, as well as with disease-related properties such as misfolding and amyloid formation.</div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"108 ","pages":"Article 101665"},"PeriodicalIF":3.2,"publicationDate":"2020-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ssnmr.2020.101665","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"38081014","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: 23

Corrigendum to “Solid-state NMR of plant and fungal cell walls: A critical reviewˮ [Solid State Nucl. Magn. Reson. 107 (2020) 101660] “植物和真菌细胞壁的固态核磁共振:一个重要的回顾”[固态核]的勘误。粉剂。报章。107 (2020)101660]

IF 3.2 3区化学

Solid state nuclear magnetic resonance Pub Date : 2020-08-01 DOI: 10.1016/j.ssnmr.2020.101675

Wancheng Zhao, Liyanage D. Fernando, Alex Kirui, Fabien Deligey, Tuo Wang

引用次数: 0

Accelerating high-resolution NMR of half-integer quadrupolar nuclei in solids: SPAM-MQMAS and SPAM-STMAS 固体中半整数四极核的加速高分辨率核磁共振:SPAM-MQMAS和SPAM-STMAS

IF 3.2 3区化学

Solid state nuclear magnetic resonance Pub Date : 2020-08-01 DOI: 10.1016/j.ssnmr.2020.101668

Akiko Sasaki , Yu Tsutsumi , Jean-Paul Amoureux

{"title":"Accelerating high-resolution NMR of half-integer quadrupolar nuclei in solids: SPAM-MQMAS and SPAM-STMAS","authors":"Akiko Sasaki , Yu Tsutsumi , Jean-Paul Amoureux","doi":"10.1016/j.ssnmr.2020.101668","DOIUrl":"10.1016/j.ssnmr.2020.101668","url":null,"abstract":"<div>In solid-state NMR, multiple-quantum MAS (MQMAS) and satellite-transition MAS (STMAS) experiments are well-established techniques to obtain high-resolution spectra of half-integer quadrupolar nuclei. In 2004 and 2005, a soft-pulse-added-mixing (SPAM) concept was introduced by Gan and Amoureux to enhance the S/N ratio of MQMAS and STMAS experiments. Despite their robustness and simplicity, SPAM approaches have not yet been widely applied. Here, we further exploit SPAM concepts for sensitivity enhancement upon acquisition of two-dimensional MQMAS and STMAS spectra and also establish a general procedure upon implementation of SPAM-MQMAS and SPAM-STMAS NMR. Its effectiveness and ease in experimental setup are demonstrated using simulations and experiments performed on I = 3/2 (23Na, 87Rb), 5/2 (27Al, 85Rb) and 9/2 (93Nb) nuclei with a variety of quadrupolar coupling constants (CQ). Compared to the conventional z-filter methods, sensitivity enhancements in between 2 and 4 are achievable with SPAM. We recommend to use SPAM with a ratio of 4:1 for the number of echoes and antiechoes to safely maximize the sensitivity and resolution simultaneously. In addition, a comparison of the experimental approaches is made in the context of SPAM-MQMAS and SPAM-STMAS NMR with respect to repetition delay and spinning frequency, aiming to discuss the precautions upon making a judicious choice of high-resolution NMR methods of half-integer quadrupolar nuclei.</div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"108 ","pages":"Article 101668"},"PeriodicalIF":3.2,"publicationDate":"2020-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ssnmr.2020.101668","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"38135834","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: 3

NMR and NQR study of polymorphism in carbamazepine 卡马西平基因多态性的NMR和NQR研究

IF 3.2 3区化学

Solid state nuclear magnetic resonance Pub Date : 2020-06-01 DOI: 10.1016/j.ssnmr.2020.101653

Tomaž Apih , Veselko Žagar , Janez Seliger

{"title":"NMR and NQR study of polymorphism in carbamazepine","authors":"Tomaž Apih , Veselko Žagar , Janez Seliger","doi":"10.1016/j.ssnmr.2020.101653","DOIUrl":"10.1016/j.ssnmr.2020.101653","url":null,"abstract":"<div>Four polymorphic forms of carbamazepine have been simultaneously investigated by 1H NMR and 14N NQR. The results show that the proton spin-lattice relaxation time and the 14N NQR spectra can be used to differentiate between various polymorphic forms. Spontaneous transformations from Form II to Form III and from Form IV to Form III have been investigated through their influence on the 14N NQR spectrum and the proton NMR signal and spin-lattice relaxation. The 14N NQR spectra prove that in the observed polymorphic forms of carbamazepine the hydrogen bonded dimers of carbamazepine molecules are the basic elements of the crystal structure. The dimers are centrosymmetric in Forms III and IV and in metastable polymorphic form occurring during the transformation of Form IV to Form III. Two non-equivalent molecular positions are observed in Form II with the occupation ratio 1:1 and in Form I with the occupation ratio either 2:1 or 3:1. The 14N NQR data are related to the published crystal structures. Possible reasons for the mismatch of the X-ray and NQR data for Forms I and II are discussed.</div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"107 ","pages":"Article 101653"},"PeriodicalIF":3.2,"publicationDate":"2020-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ssnmr.2020.101653","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"37679961","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: 6

Sensitivity enhancement in 2D Double Cross Polarization experiments under fast MAS by recycling unused protons 利用回收未使用质子增强快速MAS下二维双交叉极化实验的灵敏度

IF 3.2 3区化学

Solid state nuclear magnetic resonance Pub Date : 2020-06-01 DOI: 10.1016/j.ssnmr.2020.101652

Sundaresan Jayanthi , Adonis Lupulescu

{"title":"Sensitivity enhancement in 2D Double Cross Polarization experiments under fast MAS by recycling unused protons","authors":"Sundaresan Jayanthi , Adonis Lupulescu","doi":"10.1016/j.ssnmr.2020.101652","DOIUrl":"10.1016/j.ssnmr.2020.101652","url":null,"abstract":"<div>We demonstrate sensitivity enhancement via recycling of proton magnetization in 2D Double Cross Polarization (Double CP) experiments performed on fully protonated and uniformly labeled (13C, 15N) samples at a magic angle spinning rate of 60 kHz. Unused proton magnetization is preserved during t1 evolution either by locking it with CW irradiation or by employing rotor-synchronized pi pulses. A flip-back pulse together with a modified second CP block preserves unused proton magnetization resulting in enhanced sensitivity. We have achieved sensitivity enhancements of 15–20% and 25–28% in 1H–13C and 1H–15N 2D Double CP experiments respectively. At shorter recycle delays (∼0.25T1), relative sensitivity enhancements of 40–45% and 55% were obtained in 1H–13C and 1H–15N 2D Double CP experiments respectively. An analysis of the sensitivity enhancements and theoretical estimation of lineshapes in indirect dimension in the presence of proton recycling is provided.</div>","PeriodicalId":21937,"journal":{"name":"Solid state nuclear magnetic resonance","volume":"107 ","pages":"Article 101652"},"PeriodicalIF":3.2,"publicationDate":"2020-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ssnmr.2020.101652","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"37722724","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: 4