Progress in Nuclear Magnetic Resonance Spectroscopy最新文献

{"title":"Multiplexing experiments in NMR and multi-nuclear MRI","authors":"Ēriks Kupče ,&nbsp;Kaustubh R. Mote ,&nbsp;Andrew Webb ,&nbsp;Perunthiruthy K. Madhu ,&nbsp;Tim D.W. Claridge","doi":"10.1016/j.pnmrs.2021.03.001","DOIUrl":"10.1016/j.pnmrs.2021.03.001","url":null,"abstract":"<div><p>Multiplexing NMR experiments by direct detection of multiple free induction decays (FIDs) in a single experiment offers a dramatic increase in the spectral information content and often yields significant improvement in sensitivity per unit time. Experiments with multi-FID detection have been designed with both homonuclear and multinuclear acquisition, and the advent of multiple receivers on commercial spectrometers opens up new possibilities for recording spectra from different nuclear species in parallel. Here we provide an extensive overview of such techniques, designed for applications in liquid- and solid-state NMR as well as in hyperpolarized samples. A brief overview of multinuclear MRI is also provided, to stimulate cross fertilization of ideas between the two areas of research (NMR and MRI). It is shown how such techniques enable the design of experiments that allow structure elucidation of small molecules from a single measurement. Likewise, in biomolecular NMR experiments multi-FID detection allows complete resonance assignment in proteins. Probes with multiple RF microcoils routed to multiple NMR receivers provide an alternative way of increasing the throughput of modern NMR systems, effectively reducing the cost of NMR analysis and increasing the information content at the same time. Solid-state NMR experiments have also benefited immensely from both parallel and sequential multi-FID detection in a variety of multi-dimensional pulse schemes. We are confident that multi-FID detection will become an essential component of future NMR methodologies, effectively increasing the sensitivity and information content of NMR measurements.</p></div>","PeriodicalId":20740,"journal":{"name":"Progress in Nuclear Magnetic Resonance Spectroscopy","volume":"124 ","pages":"Pages 1-56"},"PeriodicalIF":6.1,"publicationDate":"2021-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.pnmrs.2021.03.001","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"39382270","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Unveiling protein dynamics in solution with field-cycling NMR relaxometry","authors":"Giacomo Parigi,&nbsp;Enrico Ravera,&nbsp;Marco Fragai,&nbsp;Claudio Luchinat","doi":"10.1016/j.pnmrs.2021.05.001","DOIUrl":"10.1016/j.pnmrs.2021.05.001","url":null,"abstract":"<div><p><span>Field-cycling NMR relaxometry is a well-established technique that can give information on molecular structure and dynamics of biological systems. It provides the nuclear relaxation rates as a function of the applied magnetic field, starting from fields as low as ~ 10</span>⁻⁴ T up to about 1–3 T. The profiles so collected, called nuclear magnetic relaxation dispersion (NMRD) profiles, can be extended to include the relaxation rates at the largest fields achievable with high resolution NMR spectrometers. By exploiting this wide range of frequencies, the NMRD profiles can provide information on motions occurring on time scales from 10⁻⁶ to 10⁻⁹ s. ¹<span>H NMRD measurements have proved very useful also for the characterization of paramagnetic proteins, because they can help characterise a number of parameters including the number, distance and residence time of water molecules coordinated to the paramagnetic center<span>, the reorientation correlation times and the electron spin relaxation time, and the electronic structure at the metal site.</span></span></p></div>","PeriodicalId":20740,"journal":{"name":"Progress in Nuclear Magnetic Resonance Spectroscopy","volume":"124 ","pages":"Pages 85-98"},"PeriodicalIF":6.1,"publicationDate":"2021-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.pnmrs.2021.05.001","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"39382274","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Swelling layered minerals applications: A solid state NMR overview","authors":"Esperanza Pavón ,&nbsp;María D. Alba","doi":"10.1016/j.pnmrs.2021.04.001","DOIUrl":"10.1016/j.pnmrs.2021.04.001","url":null,"abstract":"<div><p>Swelling layered clay minerals form an important sub-group of the phyllosilicate family. They are characterized by their ability to expand or contract in the presence or absence of water. This property makes them useful for a variety of applications, ranging from environmental technologies to heterogeneous catalysis, and including pharmaceutical and industrial applications. Solid State Nuclear Magnetic Resonance (SS-NMR) has been extensively applied in the characterization of these materials, providing useful information on their dynamics and structure that is inaccessible using other characterization methods such as X-ray diffraction. In this review, we present the key contributions of SS-NMR to the understanding of the mechanisms that govern some of the main applications associated to swelling clay minerals. The article is divided in two parts. The first part presents SS-NMR conventional applications to layered clay minerals, while the second part comprises an in-depth review of the information that SS-NMR can provide about the different properties of swelling layered clay minerals.</p></div>","PeriodicalId":20740,"journal":{"name":"Progress in Nuclear Magnetic Resonance Spectroscopy","volume":"124 ","pages":"Pages 99-128"},"PeriodicalIF":6.1,"publicationDate":"2021-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.pnmrs.2021.04.001","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"39382275","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"NMR studies of adsorption and diffusion in porous carbonaceous materials","authors":"Alexander C. Forse ,&nbsp;Céline Merlet ,&nbsp;Clare P. Grey ,&nbsp;John M. Griffin","doi":"10.1016/j.pnmrs.2021.03.003","DOIUrl":"10.1016/j.pnmrs.2021.03.003","url":null,"abstract":"<div><p>Porous carbonaceous materials have many important industrial applications including energy storage, water purification, and adsorption of volatile organic compounds. Most of their applications rely upon the adsorption of molecules or ions within the interior pore volume of the carbon particles. Understanding the behaviour and properties of adsorbate species on the molecular level is therefore key for optimising porous carbon materials, but this is very challenging owing to the complexity of the disordered carbon structure and the presence of multiple phases in the system. In recent years, NMR spectroscopy has emerged as one of the few experimental techniques that can resolve adsorbed species from those outside the pore network. Adsorbed, or “in-pore” species are shielded with respect to their free (or “ex-pore”) counterparts. This shielding effect arises primarily due to ring currents in the carbon structure in the presence of a magnetic field, such that the observed chemical shift differences upon adsorption are independent of the observed nucleus to a first approximation. Theoretical modelling has played an important role in rationalising and explaining these experimental observations. Together, experiments and simulations have enabled a large amount of information to be gained on the adsorption and diffusion of adsorbed species, as well as on the structural and magnetic properties of the porous carbon adsorbent. Here, we review the methodological developments and applications of NMR spectroscopy and related modelling in this field, and provide perspectives on possible future applications and research directions.</p></div>","PeriodicalId":20740,"journal":{"name":"Progress in Nuclear Magnetic Resonance Spectroscopy","volume":"124 ","pages":"Pages 57-84"},"PeriodicalIF":6.1,"publicationDate":"2021-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.pnmrs.2021.03.003","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"39382272","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Silent zero TE MR neuroimaging: Current state-of-the-art and future directions","authors":"Emil Ljungberg ,&nbsp;Nikou L. Damestani ,&nbsp;Tobias C. Wood ,&nbsp;David J. Lythgoe ,&nbsp;Fernando Zelaya ,&nbsp;Steven C.R. Williams ,&nbsp;Ana Beatriz Solana ,&nbsp;Gareth J. Barker ,&nbsp;Florian Wiesinger","doi":"10.1016/j.pnmrs.2021.03.002","DOIUrl":"10.1016/j.pnmrs.2021.03.002","url":null,"abstract":"<div><p>Magnetic Resonance Imaging (MRI) scanners produce loud acoustic noise originating from vibrational Lorentz forces induced by rapidly changing currents in the magnetic field gradient coils. Using zero echo time (ZTE) MRI pulse sequences, gradient switching can be reduced to a minimum, which enables near silent operation.<!--> <!-->Besides silent MRI, ZTE offers further interesting characteristics, including a nominal echo time of TE = 0 (thus capturing short-lived signals from MR tissues which are otherwise MR-invisible), 3D radial sampling (providing motion robustness), and ultra-short repetition times (providing fast and efficient scanning).<!--> <!-->In this work we describe the main concepts behind ZTE imaging with a focus on conceptual understanding of the imaging sequences, relevant acquisition parameters, commonly observed image artefacts, and image contrasts. We will further describe a range of methods for anatomical and functional neuroimaging, together with recommendations for successful implementation.</p></div>","PeriodicalId":20740,"journal":{"name":"Progress in Nuclear Magnetic Resonance Spectroscopy","volume":"123 ","pages":"Pages 73-93"},"PeriodicalIF":6.1,"publicationDate":"2021-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.pnmrs.2021.03.002","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"39054985","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Single-crystal NMR spectroscopy","authors":"Thomas Vosegaard","doi":"10.1016/j.pnmrs.2021.01.001","DOIUrl":"10.1016/j.pnmrs.2021.01.001","url":null,"abstract":"<div><p>Single-crystal (SC) NMR spectroscopy is a solid-state NMR method that has been used since the early days of NMR to study the magnitude and orientation of tensorial nuclear spin interactions in solids. This review first presents the field of SC NMR instrumentation, then provides a survey of software for analysis of SC NMR data, and finally it highlights selected applications of SC NMR in various fields of research. The aim of the last part is not to provide a complete review of all SC NMR literature but to provide examples that demonstrate interesting applications of SC NMR.</p></div>","PeriodicalId":20740,"journal":{"name":"Progress in Nuclear Magnetic Resonance Spectroscopy","volume":"123 ","pages":"Pages 51-72"},"PeriodicalIF":6.1,"publicationDate":"2021-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.pnmrs.2021.01.001","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"39054984","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Tailoring the nuclear Overhauser effect for the study of small and medium-sized molecules by solvent viscosity manipulation","authors":"Pedro Lameiras,&nbsp;Jean-Marc Nuzillard","doi":"10.1016/j.pnmrs.2020.12.001","DOIUrl":"10.1016/j.pnmrs.2020.12.001","url":null,"abstract":"<div><p>The nuclear Overhauser effect (NOE) is a consequence of cross-relaxation between nuclear spins mediated by dipolar coupling. Its sensitivity to internuclear distances has made it an increasingly important tool for the determination of through-space atom proximity relationships within molecules of sizes ranging from the smallest systems to large biopolymers. With the support of sophisticated FT-NMR techniques, the NOE plays an essential role in structure elucidation, conformational and dynamic investigations in liquid-state NMR. The efficiency of magnetization transfer by the NOE depends on the molecular rotational correlation time, whose value depends on solution viscosity. The magnitude of the NOE between ¹H nuclei varies from +50% when molecular tumbling is fast to −100% when it is slow, the latter case corresponding to the spin diffusion limit. In an intermediate tumbling regime, the NOE may be vanishingly small. Increasing the viscosity of the solution increases the motional correlation time, and as a result, otherwise unobservable NOEs may be revealed and brought close to the spin diffusion limit. The goal of this review is to report the resolution of structural problems that benefited from the manipulation of the negative NOE by means of viscous solvents, including examples of molecular structure determination, conformation elucidation and mixture analysis (the <em>ViscY</em> method).</p></div>","PeriodicalId":20740,"journal":{"name":"Progress in Nuclear Magnetic Resonance Spectroscopy","volume":"123 ","pages":"Pages 1-50"},"PeriodicalIF":6.1,"publicationDate":"2021-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.pnmrs.2020.12.001","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"39054983","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Magnetic resonance spectroscopy for the study of cns malignancies","authors":"Victor Ruiz-Rodado ,&nbsp;Jeffery R. Brender ,&nbsp;Murali K. Cherukuri ,&nbsp;Mark R. Gilbert ,&nbsp;Mioara Larion","doi":"10.1016/j.pnmrs.2020.11.001","DOIUrl":"10.1016/j.pnmrs.2020.11.001","url":null,"abstract":"&lt;div&gt;&lt;p&gt;Despite intensive research, brain tumors are amongst the malignancies with the worst prognosis; therefore, a prompt diagnosis and thoughtful assessment of the disease is required. The resistance of brain tumors to most forms of conventional therapy has led researchers to explore the underlying biology in search of new vulnerabilities and biomarkers. The unique metabolism of brain tumors represents one potential vulnerability and the basis for a system of classification. Profiling this aberrant metabolism requires a method to accurately measure and report differences in metabolite concentrations. Magnetic resonance-based techniques provide a framework for examining tumor tissue and the evolution of disease. Nuclear Magnetic Resonance (NMR) analysis of biofluids collected from patients suffering from brain cancer can provide biological information about disease status. In particular, urine and plasma can serve to monitor the evolution of disease through the changes observed in the metabolic profiles. Moreover, cerebrospinal fluid can be utilized as a direct reporter of cerebral activity since it carries the chemicals exchanged with the brain tissue and the tumor mass. Metabolic reprogramming has recently been included as one of the hallmarks of cancer. Accordingly, the metabolic rewiring experienced by these tumors to sustain rapid growth and proliferation can also serve as a potential therapeutic target. The combination of &lt;sup&gt;13&lt;/sup&gt;C tracing approaches with the utilization of different NMR spectral modalities has allowed investigations of the upregulation of glycolysis in the aggressive forms of brain tumors, including glioblastomas, and the discovery of the utilization of acetate as an alternative cellular fuel in brain metastasis and gliomas. One of the major contributions of magnetic resonance to the assessment of brain tumors has been the non-invasive determination of 2-hydroxyglutarate (2HG) in tumors harboring a mutation in isocitrate dehydrogenase 1 (IDH1). The mutational status of this enzyme already serves as a key feature in the clinical classification of brain neoplasia in routine clinical practice and pilot studies have established the use of &lt;em&gt;in vivo&lt;/em&gt; magnetic resonance spectroscopy (MRS) for monitoring disease progression and treatment response in IDH mutant gliomas. However, the development of bespoke methods for 2HG detection by MRS has been required, and this has prevented the wider implementation of MRS methodology into the clinic. One of the main challenges for improving the management of the disease is to obtain an accurate insight into the response to treatment, so that the patient can be promptly diverted into a new therapy if resistant or maintained on the original therapy if responsive. The implementation of &lt;sup&gt;13&lt;/sup&gt;C hyperpolarized magnetic resonance spectroscopic imaging (MRSI) has allowed detection of changes in tumor metabolism associated with a treatment, and as such has been revealed as a remar","PeriodicalId":20740,"journal":{"name":"Progress in Nuclear Magnetic Resonance Spectroscopy","volume":"122 ","pages":"Pages 23-41"},"PeriodicalIF":6.1,"publicationDate":"2021-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.pnmrs.2020.11.001","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"25405553","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Symmetry versus entropy: Long-lived states and coherences","authors":"Florin Teleanu ,&nbsp;Aude Sadet ,&nbsp;Paul R. Vasos","doi":"10.1016/j.pnmrs.2020.12.002","DOIUrl":"10.1016/j.pnmrs.2020.12.002","url":null,"abstract":"<div><p>In recent years, new molecular symmetry-based approaches for magnetic resonance have been invented. The implications of these discoveries will be significant for molecular imaging via magnetic resonance, <em>in vitro</em> as well as <em>in vivo</em>, for quantum computing and for other fields. Since the initial observation in 2004 in Southampton that effective spin symmetry can be instilled in a molecule during magnetic resonance experiments, spin states that are resilient to relaxation mechanisms have been increasingly used. Most of these states are related to the nuclear singlet in a pair of <em>J</em>-coupled spins. Tailored relaxation rate constants for magnetization became available in molecules of different sizes and structures, as experimental developments broadened the scope of symmetry-adapted spin states. The ensuing access to timescales longer than the classically-attained ones by circa one order of magnitude allows the study of processes such as slow diffusion or slow exchange that were previously beyond reach. Long-lived states formed by differences between populations of singlets and triplets have overcome the limitations imposed by longitudinal relaxation times (<em>T₁</em>) by factors up to 40. Long-lived coherences formed by superpositions of singlets and triplets have overcome the limit of classical transverse coherence (<em>T₂</em>) by a factor 9. We present here an overview of the development and applications of long-lived states (LLS) and long-lived coherences (LLC’s) and considerations on future perspectives.</p></div>","PeriodicalId":20740,"journal":{"name":"Progress in Nuclear Magnetic Resonance Spectroscopy","volume":"122 ","pages":"Pages 63-75"},"PeriodicalIF":6.1,"publicationDate":"2021-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.pnmrs.2020.12.002","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"25405552","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Cardiac magnetic resonance fingerprinting: Trends in technical development and potential clinical applications","authors":"Brendan L. Eck ,&nbsp;Scott D. Flamm ,&nbsp;Deborah H. Kwon ,&nbsp;W.H. Wilson Tang ,&nbsp;Claudia Prieto Vasquez ,&nbsp;Nicole Seiberlich","doi":"10.1016/j.pnmrs.2020.10.001","DOIUrl":"10.1016/j.pnmrs.2020.10.001","url":null,"abstract":"<div><p>Quantitative cardiac magnetic resonance has emerged in recent years as an approach for evaluating a range of cardiovascular conditions, with T₁ and T₂ mapping at the forefront of these developments. Cardiac Magnetic Resonance Fingerprinting (cMRF) provides a rapid and robust framework for simultaneous quantification of myocardial T₁ and T₂ in addition to other tissue properties. Since the advent of cMRF, a number of technical developments and clinical validation studies have been reported. This review provides an overview of cMRF, recent technical developments, healthy subject and patient studies, anticipated technical improvements, and potential clinical applications. Recent technical developments include slice profile and pulse efficiency corrections, improvements in image reconstruction, simultaneous multislice imaging, 3D whole-ventricle imaging, motion-resolved imaging, fat–water separation, and machine learning for rapid dictionary generation. Future technical developments in cMRF, such as B₀ and B₁ field mapping, acceleration of acquisition and reconstruction, imaging of patients with implanted devices, and quantification of additional tissue properties are also described. Potential clinical applications include characterization of infiltrative, inflammatory, and ischemic cardiomyopathies, tissue characterization in the left atrium and right ventricle, post-cardiac transplantation assessment, reduction of contrast material, pre-procedural planning for electrophysiology interventions, and imaging of patients with implanted devices.</p></div>","PeriodicalId":20740,"journal":{"name":"Progress in Nuclear Magnetic Resonance Spectroscopy","volume":"122 ","pages":"Pages 11-22"},"PeriodicalIF":6.1,"publicationDate":"2021-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.pnmrs.2020.10.001","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"25405551","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}