Portable, Low-cost NMR with Laser-Lathe Lithography Produced

Energy Technology Data Exchange (ETDEWEB)

Herberg, J L; Demas, V; Malba, V; Bernhardt, A; Evans, L; Harvey, C; Chinn, S; Maxwell, R; Reimer, J; Pines, A

2006-12-21

Nuclear Magnetic Resonance (NMR) is unsurpassed in its ability to non-destructively probe chemical identity. Portable, low-cost NMR sensors would enable on-site identification of potentially hazardous substances, as well as the study of samples in a variety of industrial applications. Recent developments in RF microcoil construction (i.e. coils much smaller than the standard 5 mm NMR RF coils), have dramatically increased NMR sensitivity and decreased the limits-of-detection (LOD). We are using advances in laser pantographic microfabrication techniques, unique to LLNL, to produce RF microcoils for field deployable, high sensitivity NMR-based detectors. This same fabrication technique can be used to produce imaging coils for MRI as well as for standard hardware shimming or 'ex-situ' shimming of field inhomogeneities typically associated with inexpensive magnets. This paper describes a portable NMR system based on a laser-fabricated microcoil and homebuilt probe design. For testing this probe, we used a hand-held 2 kg Halbach magnet that can fit into the palm of a hand, and an RF probe with laser-fabricated microcoils. The focus of the paper is on the evaluation of the microcoils, RF probe, and first generation gradient coils. The setup of this system, initial results, sensitivity measurements, and future plans are discussed. The results, even though preliminary, are promising and provide the foundation for developing a portable, inexpensive NMR system for chemical analysis. Such a system will be ideal for chemical identification of trace substances on site.

Introduction to quantum calculation methods in high resolution NMR

International Nuclear Information System (INIS)

Goldman, M.

1996-01-01

New techniques as for instance the polarization transfer, the coherence with several quanta and the double Fourier transformation have appeared fifteen years ago. These techniques constitute a considerable advance in NMR. Indeed, they allow to study more complex molecules than it was before possible. But with these advances, the classical description of the NMR is not enough to understand precisely the physical phenomena induced by these methods. It is then necessary to resort to quantum calculation methods. The aim of this work is to present these calculation methods. After some recalls of quantum mechanics, the author describes the NMR with the density matrix, reviews the main methods of double Fourier transformation and then gives the principle of the relaxation times calculation. (O.M.)

Recent Advances in Multinuclear NMR Spectroscopy for Chiral Recognition of Organic Compounds

Directory of Open Access Journals (Sweden)

Márcio S. Silva

2017-02-01

Full Text Available Nuclear magnetic resonance (NMR is a powerful tool for the elucidation of chemical structure and chiral recognition. In the last decade, the number of probes, media, and experiments to analyze chiral environments has rapidly increased. The evaluation of chiral molecules and systems has become a routine task in almost all NMR laboratories, allowing for the determination of molecular connectivities and the construction of spatial relationships. Among the features that improve the chiral recognition abilities by NMR is the application of different nuclei. The simplicity of the multinuclear NMR spectra relative to 1H, the minimal influence of the experimental conditions, and the larger shift dispersion make these nuclei especially suitable for NMR analysis. Herein, the recent advances in multinuclear (19F, 31P, 13C, and 77Se NMR spectroscopy for chiral recognition of organic compounds are presented. The review describes new chiral derivatizing agents and chiral solvating agents used for stereodiscrimination and the assignment of the absolute configuration of small organic compounds.

Advanced in-flight measurement techniques

CERN Document Server

Lawson, Nicholas; Jentink, Henk; Kompenhans, Jürgen

2013-01-01

The book presents a synopsis of the main results achieved during the 3 year EU-project "Advanced Inflight Measurement Techniques (AIM)" which applied advanced image based measurement techniques to industrial flight testing. The book is intended to be not only an overview on the AIM activities but also a guide on the application of advanced optical measurement techniques for future flight testing. Furthermore it is a useful guide for engineers in the field of experimental methods and flight testing who face the challenge of a future requirement for the development of highly accurate non-intrusive in-flight measurement techniques.

Techniques for Ultra-high Magnetic Field Gradient NMR Diffusion Measurements

Science.gov (United States)

Sigmund, Eric E.; Mitrovic, Vesna F.; Calder, Edward S.; Will Thomas, G.; Halperin, William P.; Reyes, Arneil P.; Kuhns, Philip L.; Moulton, William G.

2001-03-01

We report on development and application of techniques for ultraslow diffusion coefficient measurements through nuclear magnetic resonance (NMR) in high magnetic field gradients. We have performed NMR experiments in a steady fringe field gradient of 175 T/m from a 23 T resistive Bitter magnet, as well as in a gradient of 42 T/m from an 8 T superconducting magnet. New techniques to provide optimum sensitivity in these experiments are described. To eliminate parasitic effects of the temporal instability of the resistive magnet, we have introduced a passive filter: a highly conductive cryogen-cooled inductive shield. We show experimental demonstration of such a shield’s effect on NMR performed in the Bitter magnet. For enhanced efficiency, we have employed “frequency jumping” in our spectrometer system. Application of these methods has made possible measurements of diffusion coefficients as low as 10-10 cm^2/s, probing motion on a 250 nm length scale.

MetaboLab - advanced NMR data processing and analysis for metabolomics

Directory of Open Access Journals (Sweden)

Günther Ulrich L

2011-09-01

Full Text Available Abstract Background Despite wide-spread use of Nuclear Magnetic Resonance (NMR in metabolomics for the analysis of biological samples there is a lack of graphically driven, publicly available software to process large one and two-dimensional NMR data sets for statistical analysis. Results Here we present MetaboLab, a MATLAB based software package that facilitates NMR data processing by providing automated algorithms for processing series of spectra in a reproducible fashion. A graphical user interface provides easy access to all steps of data processing via a script builder to generate MATLAB scripts, providing an option to alter code manually. The analysis of two-dimensional spectra (1H,13C-HSQC spectra is facilitated by the use of a spectral library derived from publicly available databases which can be extended readily. The software allows to display specific metabolites in small regions of interest where signals can be picked. To facilitate the analysis of series of two-dimensional spectra, different spectra can be overlaid and assignments can be transferred between spectra. The software includes mechanisms to account for overlapping signals by highlighting neighboring and ambiguous assignments. Conclusions The MetaboLab software is an integrated software package for NMR data processing and analysis, closely linked to the previously developed NMRLab software. It includes tools for batch processing and gives access to a wealth of algorithms available in the MATLAB framework. Algorithms within MetaboLab help to optimize the flow of metabolomics data preparation for statistical analysis. The combination of an intuitive graphical user interface along with advanced data processing algorithms facilitates the use of MetaboLab in a broader metabolomics context.

Applications of solid-state Nuclear Magnetic Resonance (NMR) in studies of Portland cements-based materials

DEFF Research Database (Denmark)

Skibsted, Jørgen; Andersen, Morten Daugaard; Jakobsen, Hans Jørgen

2007-01-01

Solid-state NMR spectroscopy represents an important research tool in the characterization of a range of structural properties for cement-based materials. Different approaches of the technique can be used to obtain information on hydration kinetics, mobile and bound water, porosity, and local...... atomic structures. After a short introduction to these NMR techniques, it is exemplified how magic-angle spinning (MAS) NMR can provide quantitative and structural information about specific phases in anhydrous and hydrated Portland cements with main emphasis on the incorporation of Al3+ ions...

Portable, low-cost NMR with laser-lathe lithography produced microcoils.

Science.gov (United States)

Demas, Vasiliki; Herberg, Julie L; Malba, Vince; Bernhardt, Anthony; Evans, Lee; Harvey, Christopher; Chinn, Sarah C; Maxwell, Robert S; Reimer, Jeffrey

2007-11-01

Nuclear Magnetic Resonance (NMR) is unsurpassed in its ability to non-destructively probe chemical identity. Portable, low-cost NMR sensors would enable on-site identification of potentially hazardous substances, as well as the study of samples in a variety of industrial applications. Recent developments in RF microcoil construction (i.e. coils much smaller than the standard 5mm NMR RF coils), have dramatically increased NMR sensitivity and decreased the limits-of-detection (LOD). We are using advances in laser pantographic microfabrication techniques, unique to LLNL, to produce RF microcoils for field deployable, high sensitivity NMR-based detectors. This same fabrication technique can be used to produce imaging coils for MRI as well as for standard hardware shimming or "ex-situ" shimming of field inhomogeneities typically associated with inexpensive magnets. This paper describes a portable NMR system based on the use of a 2 kg hand-held permanent magnet, laser-fabricated microcoils, and a compact spectrometer. The main limitations for such a system are the low resolution and sensitivity associated with the low field values and quality of small permanent magnets, as well as the lack of large amounts of sample of interest in most cases. The focus of the paper is on the setting up of this system, initial results, sensitivity measurements, discussion of the limitations and future plans. The results, even though preliminary, are promising and provide the foundation for developing a portable, inexpensive NMR system for chemical analysis. Such a system will be ideal for chemical identification of trace substances on site.

New strategy for stable-isotope-aided, multidimensional NMR spectroscopy of DNA oligomers

Energy Technology Data Exchange (ETDEWEB)

Ono, Okira; Tate, Shin-Ichi; Kainosho, Masatsune [Tokyo Metropolitan Univ., Tokyo (Japan)

1994-12-01

Nuclear Magnetic Resonance (NMR) is the most efficient method for determining the solution structures of biomolecules. By applying multidimensional heteronuclear NMR techniques to {sup 13}C/{sup 15}N-labeled proteins, we can determine the solution structures of proteins with molecular mass of 20 to 30kDa at an accuracy similar to that of x-ray crystallography. Improvements in NMR instrumentation and techniques as well as the development of protein engineering methods for labeling proteins have rapidly advanced multidimensional heteronuclear NMR of proteins. In contrast, multidimensional heteronuclear NMR studies of nucleic acids is less advanced because there were no efficient methods for preparing large amounts of labeled DNA/RNA oligomers. In this report, we focused on the chemical synthesis of DNA oligomers labeled at specific residue(s). RNA oligomers with specific labels, which are difficult to synthesize by the enzyme method, can be synthesized by the chemical method. The specific labels are useful for conformational analysis of larger molecules such as protein-nucleic acid complexes.

Fluid-Rock Characterization and Interactions in NMR Well Logging

Energy Technology Data Exchange (ETDEWEB)

George J. Hirasaki; Kishore K. Mohanty

2005-09-05

The objective of this report is to characterize the fluid properties and fluid-rock interactions that are needed for formation evaluation by NMR well logging. The advances made in the understanding of NMR fluid properties are summarized in a chapter written for an AAPG book on NMR well logging. This includes live oils, viscous oils, natural gas mixtures, and the relation between relaxation time and diffusivity. Oil based drilling fluids can have an adverse effect on NMR well logging if it alters the wettability of the formation. The effect of various surfactants on wettability and surface relaxivity are evaluated for silica sand. The relation between the relaxation time and diffusivity distinguishes the response of brine, oil, and gas in a NMR well log. A new NMR pulse sequence in the presence of a field gradient and a new inversion technique enables the T{sub 2} and diffusivity distributions to be displayed as a two-dimensional map. The objectives of pore morphology and rock characterization are to identify vug connectivity by using X-ray CT scan, and to improve NMR permeability correlation. Improved estimation of permeability from NMR response is possible by using estimated tortuosity as a parameter to interpolate between two existing permeability models.

13C-NMR assignment, structure, and dynamics of deoxyoligonucleotides

International Nuclear Information System (INIS)

Zanatta, N.; Borer, P.N.; Levy, G.C.

1986-01-01

The unique spectral properties of 13 C-NMR for studying nucleic acids and some of the important features of 13 C-NMR in oligonucleotide studies are demostrated. The main difficulty in studying oligonucleotides by 13 C-NMR and recent improvements in NMR instrumentation and advances in oligonucleotide synthesis are presented. The high resolution 13 C-NMR spectra, T 1 relaxation times and NOEs were measured for duplex of the self-complementary oligo-DNAs: d(CG) 3 and d(GGTATACC) are studied. The target of this study is to developed a systematic 13 C-NMR spectral assignment and to investigate the structure and dynamics of these two sequences by this techniques. (M.J.C.) [pt

Successful Sampling Strategy Advances Laboratory Studies of NMR Logging in Unconsolidated Aquifers

Science.gov (United States)

Behroozmand, Ahmad A.; Knight, Rosemary; Müller-Petke, Mike; Auken, Esben; Barfod, Adrian A. S.; Ferré, Ty P. A.; Vilhelmsen, Troels N.; Johnson, Carole D.; Christiansen, Anders V.

2017-11-01

The nuclear magnetic resonance (NMR) technique has become popular in groundwater studies because it responds directly to the presence and mobility of water in a porous medium. There is a need to conduct laboratory experiments to aid in the development of NMR hydraulic conductivity models, as is typically done in the petroleum industry. However, the challenge has been obtaining high-quality laboratory samples from unconsolidated aquifers. At a study site in Denmark, we employed sonic drilling, which minimizes the disturbance of the surrounding material, and extracted twelve 7.6 cm diameter samples for laboratory measurements. We present a detailed comparison of the acquired laboratory and logging NMR data. The agreement observed between the laboratory and logging data suggests that the methodologies proposed in this study provide good conditions for studying NMR measurements of unconsolidated near-surface aquifers. Finally, we show how laboratory sample size and condition impact the NMR measurements.

Surface characterization of hydrophobic core-shell QDs using NMR techniques

Science.gov (United States)

Zhang, Chengqi; Zeng, Birong; Palui, Goutam; Mattoussi, Hedi

2018-02-01

Using a few solution phase NMR spectroscopy techniques, including 1H NMR and 31P NMR, we have characterized the organic shell on CdSe-ZnS core-shell quantum dots and tracked changes in its composition when the QD dispersions are subjected to varying degrees of purification. Combining solution phase NMR with diffusion ordered spectroscopy (DOSY), we were able to distinguish between freely diffusing ligands in the sample from those bound on the surfaces. Additionally, matrix assisted laser desorption ionization (MALDI) and FTIR measurements were used to provide complementary and supporting information on the organic ligand coating for these nanocrystals. We found that the organic shell is dominated by monomeric or oligomeric n-hexylphosphonic acid (HPA), along with small portion of 1-hexadecyl amine (HDA). The presence of TOP/TOPO (tri-n-octylphosphine / tri-noctylphosphine oxide) molecules is much smaller, even though large excess of TOP/TOPO were used during the QD growth. These results indicate that HPA (alkyl phosphonate) exhibits the strongest coordination affinity to ZnS-rich QD surfaces grown using the high temperature injection route.

The application of NMR-based milk metabolite analysis in milk authenticity identification.

Science.gov (United States)

Li, Qiangqiang; Yu, Zunbo; Zhu, Dan; Meng, Xianghe; Pang, Xiumei; Liu, Yue; Frew, Russell; Chen, He; Chen, Gang

2017-07-01

Milk is an important food component in the human diet and is a target for fraud, including many unsafe practices. For example, the unscrupulous adulteration of soymilk into bovine and goat milk or of bovine milk into goat milk in order to gain profit without declaration is a health risk, as the adulterant source and sanitary history are unknown. A robust and fit-for-purpose technique is required to enforce market surveillance and hence protect consumer health. Nuclear magnetic resonance (NMR) is a powerful technique for characterization of food products based on measuring the profile of metabolites. In this study, 1D NMR in conjunction with multivariate chemometrics as well as 2D NMR was applied to differentiate milk types and to identify milk adulteration. Ten metabolites were found which differed among milk types, hence providing characteristic markers for identifying the milk. These metabolites were used to establish mathematical models for milk type differentiation. The limit of quantification (LOQ) of adulteration was 2% (v/v) for soymilk in bovine milk, 2% (v/v) for soymilk in goat milk and 5% (v/v) for bovine milk in goat milk, with relative standard deviation (RSD) less than 10%, which can meet the needs of daily inspection. The NMR method described here is effective for milk authenticity identification, and the study demonstrates that the NMR-based milk metabolite analysis approach provides a means of detecting adulteration at expected levels and can be used for dairy quality monitoring. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

Applications of NMR spectroscopy to xenobiotic metabolism

International Nuclear Information System (INIS)

Harris, T.M.

1989-01-01

Recent years have seen high field NMR spectrometers become commonplace in research laboratories. At the same time, major advances in methodology for structural analysis have occurred, particularly notable among these being the development of two-dimensional spectroscopic techniques. Many applications have been made of NMR spectroscopy in the study of xenobiotic metabolic processes. This deals with two specific applications which have been made in the author's laboratory and involve mechanistic studies of the reactions of the carcinogens ethylene dibromide and aflatoxin with DNA

Quantum theory of NMR adiabatic pulses and their applications

International Nuclear Information System (INIS)

Ke, Y.

1993-01-01

Recently explosive developments of in vivo NMR spectroscopy (NMRS) and imaging (NMRI) in biological and medical sciences have resulted in the establishment of NMR as one of the most advanced major technique in life sciences. These developments have created huge demands for a variety of NMR adiabatic pulses with play a very important role in NMR experiments in vivo. In order to develop new NMR adiabatic pulses, a rigorous systematical quantum theory for this kind of pulses is greatly needed. Providing such a theory is one of the important goals of this dissertation. Quantum density matrix theory and product operator method have been used throughout this dissertation. Another goal, which is the major goal of this thesis research, is to use the quantum theory as a guide to develop new NMR adiabatic pulses and their applications. To fill this goal, a technique to construct a new type of adiabatic pulses, narrow band selective adiabatic pulses, has been invented, which is described through the example of constructing an adiabatic DANTE inversion pulse. This new adiabatic pulse is the first narrow band selective adiabatic pulses: Adiabatic homonuclear and heteronuclear spectral editing sequences. Unique to the first pulse sequence is a B 1 -field filter which is built by using two non-refocusing adiabatic full passage pulses to refocus the wanted signal and dephase unwanted signals. This extra filter greatly enhance the editing efficiency. Unlike commonly used heteronuclear spectral editing sequences which depend on the polarization transfer or spectral subtraction by phase cycling techniques, the second pulse sequences accomplishes the editing of heteronuclear J-coupled signals based on the fact that this sequence is transparent to the uncoupled spins and is equivalent a 90 degrees excitation pulse to the heteronuclear J-coupled spins. Experimental results have confirmed the ability of spectral editing with these two new sequences

NMR Techniques in Metabolomic Studies: A Quick Overview on Examples of Utilization.

Science.gov (United States)

Kruk, Joanna; Doskocz, Marek; Jodłowska, Elżbieta; Zacharzewska, Anna; Łakomiec, Joanna; Czaja, Kornelia; Kujawski, Jacek

2017-01-01

Metabolomics is a rapidly developing branch of science that concentrates on identifying biologically active molecules with potential biomarker properties. To define the best biomarkers for diseases, metabolomics uses both models (in vitro, animals) and human, as well as, various techniques such as mass spectroscopy, gas chromatography, liquid chromatography, infrared and UV-VIS spectroscopy and nuclear magnetic resonance. The last one takes advantage of the magnetic properties of certain nuclei, such as 1 H, 13 C, 31 P, 19 F, especially their ability to absorb and emit energy, what is crucial for analyzing samples. Among many spectroscopic NMR techniques not only one-dimensional (1D) techniques are known, but for many years two-dimensional (2D, for example, COSY, DOSY, JRES, HETCORE, HMQS), three-dimensional (3D, DART-MS, HRMAS, HSQC, HMBC) and solid-state NMR have been used. In this paper, authors taking apart fundamental division of nuclear magnetic resonance techniques intend to shown their wide application in metabolomic studies, especially in identifying biomarkers.

Autonomous driving in NMR.

Science.gov (United States)

Perez, Manuel

2017-01-01

The automatic analysis of NMR data has been a much-desired endeavour for the last six decades, as it is the case with any other analytical technique. This need for automation has only grown as advances in hardware; pulse sequences and automation have opened new research areas to NMR and increased the throughput of data. Full automatic analysis is a worthy, albeit hard, challenge, but in a world of artificial intelligence, instant communication and big data, it seems that this particular fight is happening with only one technique at a time (let this be NMR, MS, IR, UV or any other), when the reality of most laboratories is that there are several types of analytical instrumentation present. Data aggregation, verification and elucidation by using complementary techniques (e.g. MS and NMR) is a desirable outcome to pursue, although a time-consuming one if performed manually; hence, the use of automation to perform the heavy lifting for users is required to make the approach attractive for scientists. Many of the decisions and workflows that could be implemented under automation will depend on the two-way communication with databases that understand analytical data, because it is desirable not only to query these databases but also to grow them in as much of an automatic manner as possible. How these databases are designed, set up and the data inside classified will determine what workflows can be implemented. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Effect of magnetic field strength on NMR-based metabonomic human urine data. Comparative study of 250, 400, 500, and 800 MHz

DEFF Research Database (Denmark)

Bertram, Hanne Christine; Malmendal, Anders; Petersen, Bent O.

2007-01-01

Metabonomic analysis of urine utilizing high-resolution NMR spectroscopy and chemometric techniques has proven valuable in characterizing the biochemical response to an intervention. To assess the effect of magnetic field strength on information contained in NMR-based metabonomic data sets, 1H NMR...

Sulfated oligosaccharide structures, as determined by NMR techniques

International Nuclear Information System (INIS)

Noseda, M.D.; Duarte, M.E.R.; Tischer, C.A.; Gorin, P.A.J.; Cerezo, A.S.

1997-01-01

Carrageenans are sulfated polysaccharides, produced by red seaweeds (Rhodophyta), that have important biological and physico-chemical properties. Using partial autohydrolysis, we obtained sulfated oligosaccharides from a λ-carrageenan (Noseda and Cerezo, 1993). These oligosaccharides are valuable not only for the study of the structures of the parent carrageenans but also for their possible biological activities. In this work we determined the chemical structure of one of the sulfated oligosaccharides using 1D and 2D NMR techniques. (author)

Molecular dynamics computer simulations based on NMR data

International Nuclear Information System (INIS)

Vlieg, J. de.

1989-01-01

In the work described in this thesis atom-atom distance information obtained from two-dimensional cuclear magnetic resonance is combined with molecular dynamics simulaitons. The simulation is used to improve the accuracy of a structure model constructed on the basis of NMR data. During the MD refinement the crude NMR structure is simultaneously optimized with respect to the atomic interaction function and to the set of atom-atom distances or other NMR information. This means that insufficient experimental data is completed with theoretical knowledge and the combination will lead to more reliable structures than would be obtained from one technique alone. (author). 191 refs.; 17 figs.; 12 schemes; 22 tabs

NMR-Fragment Based Virtual Screening: A Brief Overview.

Science.gov (United States)

Singh, Meenakshi; Tam, Benjamin; Akabayov, Barak

2018-01-25

Fragment-based drug discovery (FBDD) using NMR has become a central approach over the last twenty years for development of small molecule inhibitors against biological macromolecules, to control a variety of cellular processes. Yet, several considerations should be taken into account for obtaining a therapeutically relevant agent. In this review, we aim to list the considerations that make NMR fragment screening a successful process for yielding potent inhibitors. Factors that may govern the competence of NMR in fragment based drug discovery are discussed, as well as later steps that involve optimization of hits obtained by NMR-FBDD.

NMR-Fragment Based Virtual Screening: A Brief Overview

Directory of Open Access Journals (Sweden)

Meenakshi Singh

2018-01-01

Full Text Available Fragment-based drug discovery (FBDD using NMR has become a central approach over the last twenty years for development of small molecule inhibitors against biological macromolecules, to control a variety of cellular processes. Yet, several considerations should be taken into account for obtaining a therapeutically relevant agent. In this review, we aim to list the considerations that make NMR fragment screening a successful process for yielding potent inhibitors. Factors that may govern the competence of NMR in fragment based drug discovery are discussed, as well as later steps that involve optimization of hits obtained by NMR-FBDD.

GPU Pro 5 advanced rendering techniques

CERN Document Server

Engel, Wolfgang

2014-01-01

In GPU Pro5: Advanced Rendering Techniques, section editors Wolfgang Engel, Christopher Oat, Carsten Dachsbacher, Michal Valient, Wessam Bahnassi, and Marius Bjorge have once again assembled a high-quality collection of cutting-edge techniques for advanced graphics processing unit (GPU) programming. Divided into six sections, the book covers rendering, lighting, effects in image space, mobile devices, 3D engine design, and compute. It explores rasterization of liquids, ray tracing of art assets that would otherwise be used in a rasterized engine, physically based area lights, volumetric light

Sulfated oligosaccharide structures, as determined by NMR techniques

Energy Technology Data Exchange (ETDEWEB)

Noseda, M.D.; Duarte, M.E.R.; Tischer, C.A.; Gorin, P.A.J. [Parana Univ., Curitiba, PR (Brazil). Dept. De Bioquimica; Cerezo, A.S. [Buenos Aires Univ. Nacional (Argentina). Dept. de Quimica Organica

1997-12-31

Carrageenans are sulfated polysaccharides, produced by red seaweeds (Rhodophyta), that have important biological and physico-chemical properties. Using partial autohydrolysis, we obtained sulfated oligosaccharides from a {lambda}-carrageenan (Noseda and Cerezo, 1993). These oligosaccharides are valuable not only for the study of the structures of the parent carrageenans but also for their possible biological activities. In this work we determined the chemical structure of one of the sulfated oligosaccharides using 1D and 2D NMR techniques. (author) 4 refs., 8 figs., 1 tabs.

NMR-based metabolomics in human disease diagnosis: Applications, limitations, and recommendations

KAUST Repository

Emwas, Abdul-Hamid M.

2013-04-03

Metabolomics is a dynamic and emerging research field, similar to proteomics, transcriptomics and genomics in affording global understanding of biological systems. It is particularly useful in functional genomic studies in which metabolism is thought to be perturbed. Metabolomics provides a snapshot of the metabolic dynamics that reflect the response of living systems to both pathophysiological stimuli and/or genetic modification. Because this approach makes possible the examination of interactions between an organism and its diet or environment, it is particularly useful for identifying biomarkers of disease processes that involve the environment. For example, the interaction of a high fat diet with cardiovascular disease can be studied via such a metabolomics approach by modeling the interaction between genes and diet. The high reproducibility of NMR-based techniques gives this method a number of advantages over other analytical techniques in large-scale and long-term metabolomic studies, such as epidemiological studies. This approach has been used to study a wide range of diseases, through the examination of biofluids, including blood plasma/serum, urine, blister fluid, saliva and semen, as well as tissue extracts and intact tissue biopsies. However, complicating the use of NMR spectroscopy in biomarker discovery is the fact that numerous variables can effect metabolic composition including, fasting, stress, drug administration, diet, gender, age, physical activity, life style and the subject\\'s health condition. To minimize the influence of these variations in the datasets, all experimental conditions including sample collection, storage, preparation as well as NMR spectroscopic parameters and data analysis should be optimized carefully and conducted in an identical manner as described by the local standard operating protocol. This review highlights the potential applications of NMR-based metabolomics studies and gives some recommendations to improve sample

Camphor: a good model for illustrating NMR techniques; Canfora: um bom modelo para ilustrar tecnicas de RMN

Energy Technology Data Exchange (ETDEWEB)

Yoneda, Julliane Diniz; Leal, Katia Zaccur [Universidade Federal Fluminense (UFF), Niteroi, RJ (Brazil). Dept. de Fisico-Quimica]. E-mail: kzl@rmn.uff.br; Seidl, Peter Rudolf [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Escola de Quimica. Dept. de Processos Organicos; Azeredo, Rodrigo Bagueira de V. [Universidade Federal Fluminense (UFF), Niteroi, RJ (Brazil). Inst. de Quimica. Dept. de Quimica Organica; Kleinpeter, Erich [Universitaet Potsdam (Germany). Chemisches Institut

2007-07-01

The use of Nuclear Magnetic Resonance spectroscopy to establish the three-dimensional structures of molecules is an important component of modern Chemistry courses. The combination of techniques that can be used for this purpose is conveniently illustrated by their application to the camphor molecule. This paper presents applications of several techniques used in NMR spectral interpretation in an increasing order of complexity. The result of individual experiments is illustrated in order to familiarize the user with the way connectivity through bonds and through space is established from 1D/2D-NMR spectra and molecular stereochemistry is determined from different NMR experiments. (author)

Advantages and disadvantages of nuclear magnetic resonance spectroscopy as a hyphenated technique

International Nuclear Information System (INIS)

Silva Elipe, Maria Victoria

2003-01-01

A general overview of the advancements and applications of nuclear magnetic resonance (NMR) hyphenated with other analytical techniques is given from a practical point of view. Details on the advantages and disadvantages of the hyphenation of NMR with liquid chromatography as LC-NMR and also with mass spectrometry as LC-MS-NMR are demonstrated with two examples. Current developments of NMR with other analytical separation techniques, especially with capillary liquid chromatography (capLC) are discussed

Advances in fragment-based drug discovery platforms.

Science.gov (United States)

Orita, Masaya; Warizaya, Masaichi; Amano, Yasushi; Ohno, Kazuki; Niimi, Tatsuya

2009-11-01

Fragment-based drug discovery (FBDD) has been established as a powerful alternative and complement to traditional high-throughput screening techniques for identifying drug leads. At present, this technique is widely used among academic groups as well as small biotech and large pharmaceutical companies. In recent years, > 10 new compounds developed with FBDD have entered clinical development, and more and more attention in the drug discovery field is being focused on this technique. Under the FBDD approach, a fragment library of relatively small compounds (molecular mass = 100 - 300 Da) is screened by various methods and the identified fragment hits which normally weakly bind to the target are used as starting points to generate more potent drug leads. Because FBDD is still a relatively new drug discovery technology, further developments and optimizations in screening platforms and fragment exploitation can be expected. This review summarizes recent advances in FBDD platforms and discusses the factors important for the successful application of this technique. Under the FBDD approach, both identifying the starting fragment hit to be developed and generating the drug lead from that starting fragment hit are important. Integration of various techniques, such as computational technology, X-ray crystallography, NMR, surface plasmon resonance, isothermal titration calorimetry, mass spectrometry and high-concentration screening, must be applied in a situation-appropriate manner.

Recent Advances in Techniques for Starch Esters and the Applications: A Review

Directory of Open Access Journals (Sweden)

Jing Hong

2016-07-01

Full Text Available Esterification is one of the most important methods to alter the structure of starch granules and improve its applications. Conventionally, starch esters are prepared by conventional or dual modification techniques, which have the disadvantages of being expensive, have regent overdoses, and are time-consuming. In addition, the degree of substitution (DS is often considered as the primary factor in view of its contribution to estimate substituted groups of starch esters. In order to improve the detection accuracy and production efficiency, different detection techniques, including titration, nuclear magnetic resonance (NMR, Fourier transform infrared spectroscopy (FT-IR, thermal gravimetric analysis/infrared spectroscopy (TGA/IR and headspace gas chromatography (HS-GC, have been developed for DS. This paper gives a comprehensive overview on the recent advances in DS analysis and starch esterification techniques. Additionally, the advantages, limitations, some perspectives on future trends of these techniques and the applications of their derivatives in the food industry are also presented.

NMR approaches in structure-based lead discovery: recent developments and new frontiers for targeting multi-protein complexes.

Science.gov (United States)

Dias, David M; Ciulli, Alessio

2014-01-01

Nuclear magnetic resonance (NMR) spectroscopy is a pivotal method for structure-based and fragment-based lead discovery because it is one of the most robust techniques to provide information on protein structure, dynamics and interaction at an atomic level in solution. Nowadays, in most ligand screening cascades, NMR-based methods are applied to identify and structurally validate small molecule binding. These can be high-throughput and are often used synergistically with other biophysical assays. Here, we describe current state-of-the-art in the portfolio of available NMR-based experiments that are used to aid early-stage lead discovery. We then focus on multi-protein complexes as targets and how NMR spectroscopy allows studying of interactions within the high molecular weight assemblies that make up a vast fraction of the yet untargeted proteome. Finally, we give our perspective on how currently available methods could build an improved strategy for drug discovery against such challenging targets. Copyright © 2014 The Authors. Published by Elsevier Ltd.. All rights reserved.

Advanced sensing techniques for cognitive radio

CERN Document Server

Zhao, Guodong; Li, Shaoqian

2017-01-01

This SpringerBrief investigates advanced sensing techniques to detect and estimate the primary receiver for cognitive radio systems. Along with a comprehensive overview of existing spectrum sensing techniques, this brief focuses on the design of new signal processing techniques, including the region-based sensing, jamming-based probing, and relay-based probing. The proposed sensing techniques aim to detect the nearby primary receiver and estimate the cross-channel gain between the cognitive transmitter and primary receiver. The performance of the proposed algorithms is evaluated by simulations in terms of several performance parameters, including detection probability, interference probability, and estimation error. The results show that the proposed sensing techniques can effectively sense the primary receiver and improve the cognitive transmission throughput. Researchers and postgraduate students in electrical engineering will find this an exceptional resource.

Probing the Carbonyl Functionality of a Petroleum Resin and Asphaltene through Oximation and Schiff Base Formation in Conjunction with N-15 NMR.

Directory of Open Access Journals (Sweden)

Kevin A Thorn

Full Text Available Despite recent advances in spectroscopic techniques, there is uncertainty regarding the nature of the carbonyl groups in the asphaltene and resin fractions of crude oil, information necessary for an understanding of the physical properties and environmental fate of these materials. Carbonyl and hydroxyl group functionalities are not observed in natural abundance 13C nuclear magnetic resonance (NMR spectra of asphaltenes and resins and therefore require spin labeling techniques for detection. In this study, the carbonyl functionalities of the resin and asphaltene fractions from a light aliphatic crude oil that is the source of groundwater contamination at the long term USGS study site near Bemidji, Minnesota, have been examined through reaction with 15N-labeled hydroxylamine and aniline in conjunction with analysis by solid and liquid state 15N NMR. Ketone groups were revealed through 15N NMR detection of their oxime and Schiff base derivatives, and esters through their hydroxamic acid derivatives. Anilinohydroquinone adducts provided evidence for quinones. Some possible configurations of the ketone groups in the resin and asphaltene fractions can be inferred from a consideration of the likely reactions that lead to heterocyclic condensation products with aniline and to the Beckmann reaction products from the initially formed oximes. These include aromatic ketones and ketones adjacent to quaternary carbon centers, β-hydroxyketones, β-diketones, and β-ketoesters. In a solid state cross polarization/magic angle spinning (CP/MAS 15N NMR spectrum recorded on the underivatized asphaltene as a control, carbazole and pyrrole-like nitrogens were the major naturally abundant nitrogens detected.

Probing the carbonyl functionality of a petroleum resin and asphaltene through oximation and schiff base formation in conjunction with N-15 NMR

Science.gov (United States)

Thorn, Kevin A.; Cox, Larry G.

2015-01-01

Despite recent advances in spectroscopic techniques, there is uncertainty regarding the nature of the carbonyl groups in the asphaltene and resin fractions of crude oil, information necessary for an understanding of the physical properties and environmental fate of these materials. Carbonyl and hydroxyl group functionalities are not observed in natural abundance 13C nuclear magnetic resonance (NMR) spectra of asphaltenes and resins and therefore require spin labeling techniques for detection. In this study, the carbonyl functionalities of the resin and asphaltene fractions from a light aliphatic crude oil that is the source of groundwater contamination at the long term USGS study site near Bemidji, Minnesota, have been examined through reaction with 15N-labeled hydroxylamine and aniline in conjunction with analysis by solid and liquid state 15N NMR. Ketone groups were revealed through 15N NMR detection of their oxime and Schiff base derivatives, and esters through their hydroxamic acid derivatives. Anilinohydroquinone adducts provided evidence for quinones. Some possible configurations of the ketone groups in the resin and asphaltene fractions can be inferred from a consideration of the likely reactions that lead to heterocyclic condensation products with aniline and to the Beckmann reaction products from the initially formed oximes. These include aromatic ketones and ketones adjacent to quaternary carbon centers, β-hydroxyketones, β-diketones, and β-ketoesters. In a solid state cross polarization/magic angle spinning (CP/MAS) 15N NMR spectrum recorded on the underivatized asphaltene as a control, carbazole and pyrrole-like nitrogens were the major naturally abundant nitrogens detected.

Crystallographically-based analysis of the NMR spectra of maghemite

International Nuclear Information System (INIS)

Spiers, K.M.; Cashion, J.D.

2012-01-01

All possible iron environments with respect to nearest neighbour vacancies in vacancy-ordered and vacancy-disordered maghemite have been evaluated and used as the foundation for a crystallographically-based analysis of the published NMR spectra of maghemite. The spectral components have been assigned to particular configurations and excellent agreement obtained in comparing predicted spectra with published spectra taken in applied magnetic fields. The broadness of the published NMR lines has been explained by calculations of the magnetic dipole fields at the various iron sites and consideration of the supertransferred hyperfine fields. - Highlights: ► Analysis of 57 Fe NMR of maghemite based on vacancy ordering and nearest neighbour vacancies. ► Assignment of NMR spectral components based on crystallographic analysis of unique iron sites. ► Strong agreement between predicted spectra and published spectra taken in applied magnetic fields. ► Maghemite NMR spectral broadening due to various iron sites and supertransferred hyperfine field.

Interactive NMR: A Simulation Based Teaching Tool for Fundamentals to Applications with Tangible Analogies

Science.gov (United States)

Griesse-Nascimento, Sarah; Bridger, Joshua; Brown, Keith; Westervelt, Robert

2011-03-01

Interactive computer simulations increase students' understanding of difficult concepts and their ability to explain complex ideas. We created a module of eight interactive programs and accompanying lesson plans for teaching the fundamental concepts of Nuclear Magnetic Resonance (NMR) and Magnetic Resonance Imaging (MRI) that we call interactive NMR (iNMR). We begin with an analogy between nuclear spins and metronomes to start to build intuition about the dynamics of spins in a magnetic field. We continue to explain T1, T2, and pulse sequences with the metronome analogy. The final three programs are used to introduce and explain the Magnetic Resonance Switch, a recent diagnostic technique based on NMR. A modern relevant application is useful to generate interest in the topic and confidence in the students' ability to apply their knowledge. The iNMR module was incorporated into a high school AP physics class. In a preliminary evaluation of implementation, students expressed enthusiasm and demonstrated enhanced understanding of the material relative to the previous year. Funded by NSF PHY-0646094 grant.

NMR studies concerning base-base interactions in oligonucleotides

International Nuclear Information System (INIS)

Hoogen, Y.T. van den.

1988-01-01

Two main subjects are treated in the present thesis. The firsst part principally deals with the base-base interactions in single-stranded oligoribonucleotides. The second part presents NMR and model-building studies of DNA and RNA duplexes containing an unpaired base. (author). 242 refs.; 26 figs.; 24 tabs

Recent Advances in Computational Methods for Nuclear Magnetic Resonance Data Processing

KAUST Repository

Gao, Xin

2013-01-11

Although three-dimensional protein structure determination using nuclear magnetic resonance (NMR) spectroscopy is a computationally costly and tedious process that would benefit from advanced computational techniques, it has not garnered much research attention from specialists in bioinformatics and computational biology. In this paper, we review recent advances in computational methods for NMR protein structure determination. We summarize the advantages of and bottlenecks in the existing methods and outline some open problems in the field. We also discuss current trends in NMR technology development and suggest directions for research on future computational methods for NMR.

High resolution NMR theory and chemical applications

CERN Document Server

Becker, Edwin D

1999-01-01

High Resolution NMR provides a broad treatment of the principles and theory of nuclear magnetic resonance (NMR) as it is used in the chemical sciences. It is written at an "intermediate" level, with mathematics used to augment, rather than replace, clear verbal descriptions of the phenomena. The book is intended to allow a graduate student, advanced undergraduate, or researcher to understand NMR at a fundamental level, and to see illustrations of the applications of NMR to the determination of the structure of small organic molecules and macromolecules, including proteins. Emphasis is on the study of NMR in liquids, but the treatment also includes high resolution NMR in the solid state and the principles of NMR imaging and localized spectroscopy. Careful attention is given to developing and interrelating four approaches - steady state energy levels, the rotating vector picture, the density matrix, and the product operator formalism. The presentation is based on the assumption that the reader has an acquaintan...

Techniques and approaches to proton NMR imaging of the head

International Nuclear Information System (INIS)

Pykett, I.L.; Buonanno, F.S.; Brady, T.J.; Kistler, J.P.

1983-01-01

The next few years will undoubtedly see a refinement of proton imaging technology and a broader data base will indicate to what extent proton relaxation parameters are able to detect and characterize disease. In addition, it is likely that imaging of other nuclei (e.g. 31 P, 23 Na, 19 F) will become a reality, although it must be stated that due to their inherently lower sensitivity to NMR detection and/or lower physiological concentration, clinical images of nuclei other than 1 H will undoubtedly have a low spatial resolution and may require relatively long imaging times. Nonetheless, herein lies the exciting possibility of non-invasive metabolic or functional imaging. The realm of NMR contrast agents is just beginning to be explored, and developments in high-speed imaging indicate useful applications in cardiology. So whilst improvements in image quality can be expected, as was the case with X-ray CT, the application of NMR in medicine will diversify to yield information of a more specifically functional nature. This, together with the very low attendant biological risk, heralds a bright future for NMR in clinical diagnosis

LC-NMR Technique in the Analysis of Phytosterols in Natural Extracts

Czech Academy of Sciences Publication Activity Database

Horník, Štěpán; Sajfrtová, Marie; Karban, Jindřich; Sýkora, Jan; Březinová, Anna; Wimmer, Zdeněk

2013-01-01

Roč. 2013, č. 2013 (2013), ID 526818 ISSN 2090-8865 R&D Projects: GA TA ČR TA01010578 Grant - others:GA ČR(CZ) GAP503/11/0616 Program:GA Institutional support: RVO:67985858 ; RVO:61388963 ; RVO:61389030 Keywords : LC-NMR technique * phytosterols * analyses Subject RIV: CC - Organic Chemistry; EE - Microbiology, Virology (UEB-Q) Impact factor: 0.948, year: 2013

Chemical and nanometer-scale structure of kerogen and its change during thermal maturation investigated by advanced solid-state 13C NMR spectroscopy

Science.gov (United States)

Mao, J.; Fang, X.; Lan, Y.; Schimmelmann, A.; Mastalerz, Maria; Xu, L.; Schmidt-Rohr, K.

2010-01-01

We have used advanced and quantitative solid-state nuclear magnetic resonance (NMR) techniques to investigate structural changes in a series of type II kerogen samples from the New Albany Shale across a range of maturity (vitrinite reflectance R0 from 0.29% to 1.27%). Specific functional groups such as CH3, CH2, alkyl CH, aromatic CH, aromatic C-O, and other nonprotonated aromatics, as well as "oil prone" and "gas prone" carbons, have been quantified by 13C NMR; atomic H/C and O/C ratios calculated from the NMR data agree with elemental analysis. Relationships between NMR structural parameters and vitrinite reflectance, a proxy for thermal maturity, were evaluated. The aromatic cluster size is probed in terms of the fraction of aromatic carbons that are protonated (???30%) and the average distance of aromatic C from the nearest protons in long-range H-C dephasing, both of which do not increase much with maturation, in spite of a great increase in aromaticity. The aromatic clusters in the most mature sample consist of ???30 carbons, and of ???20 carbons in the least mature samples. Proof of many links between alkyl chains and aromatic rings is provided by short-range and long-range 1H-13C correlation NMR. The alkyl segments provide most H in the samples; even at a carbon aromaticity of 83%, the fraction of aromatic H is only 38%. While aromaticity increases with thermal maturity, most other NMR structural parameters, including the aromatic C-O fractions, decrease. Aromaticity is confirmed as an excellent NMR structural parameter for assessing thermal maturity. In this series of samples, thermal maturation mostly increases aromaticity by reducing the length of the alkyl chains attached to the aromatic cores, not by pronounced growth of the size of the fused aromatic ring clusters. ?? 2010 Elsevier Ltd. All rights reserved.

nmrML: A Community Supported Open Data Standard for the Description, Storage, and Exchange of NMR Data.

Science.gov (United States)

Schober, Daniel; Jacob, Daniel; Wilson, Michael; Cruz, Joseph A; Marcu, Ana; Grant, Jason R; Moing, Annick; Deborde, Catherine; de Figueiredo, Luis F; Haug, Kenneth; Rocca-Serra, Philippe; Easton, John; Ebbels, Timothy M D; Hao, Jie; Ludwig, Christian; Günther, Ulrich L; Rosato, Antonio; Klein, Matthias S; Lewis, Ian A; Luchinat, Claudio; Jones, Andrew R; Grauslys, Arturas; Larralde, Martin; Yokochi, Masashi; Kobayashi, Naohiro; Porzel, Andrea; Griffin, Julian L; Viant, Mark R; Wishart, David S; Steinbeck, Christoph; Salek, Reza M; Neumann, Steffen

2018-01-02

NMR is a widely used analytical technique with a growing number of repositories available. As a result, demands for a vendor-agnostic, open data format for long-term archiving of NMR data have emerged with the aim to ease and encourage sharing, comparison, and reuse of NMR data. Here we present nmrML, an open XML-based exchange and storage format for NMR spectral data. The nmrML format is intended to be fully compatible with existing NMR data for chemical, biochemical, and metabolomics experiments. nmrML can capture raw NMR data, spectral data acquisition parameters, and where available spectral metadata, such as chemical structures associated with spectral assignments. The nmrML format is compatible with pure-compound NMR data for reference spectral libraries as well as NMR data from complex biomixtures, i.e., metabolomics experiments. To facilitate format conversions, we provide nmrML converters for Bruker, JEOL and Agilent/Varian vendor formats. In addition, easy-to-use Web-based spectral viewing, processing, and spectral assignment tools that read and write nmrML have been developed. Software libraries and Web services for data validation are available for tool developers and end-users. The nmrML format has already been adopted for capturing and disseminating NMR data for small molecules by several open source data processing tools and metabolomics reference spectral libraries, e.g., serving as storage format for the MetaboLights data repository. The nmrML open access data standard has been endorsed by the Metabolomics Standards Initiative (MSI), and we here encourage user participation and feedback to increase usability and make it a successful standard.

MR fingerprinting using the quick echo splitting NMR imaging technique.

Science.gov (United States)

Jiang, Yun; Ma, Dan; Jerecic, Renate; Duerk, Jeffrey; Seiberlich, Nicole; Gulani, Vikas; Griswold, Mark A

2017-03-01

The purpose of the study is to develop a quantitative method for the relaxation properties with a reduced radio frequency (RF) power deposition by combining magnetic resonance fingerprinting (MRF) technique with quick echo splitting NMR imaging technique (QUEST). A QUEST-based MRF sequence was implemented to acquire high-order echoes by increasing the gaps between RF pulses. Bloch simulations were used to calculate a dictionary containing the range of physically plausible signal evolutions using a range of T 1 and T 2 values based on the pulse sequence. MRF-QUEST was evaluated by comparing to the results of spin-echo methods. The specific absorption rate (SAR) of MRF-QUEST was compared with the clinically available methods. MRF-QUEST quantifies the relaxation properties with good accuracy at the estimated head SAR of 0.03 W/kg. T 1 and T 2 values estimated by MRF-QUEST are in good agreement with the traditional methods. The combination of the MRF and the QUEST provides an accurate quantification of T 1 and T 2 simultaneously with reduced RF power deposition. The resulting lower SAR may provide a new acquisition strategy for MRF when RF energy deposition is problematic. Magn Reson Med 77:979-988, 2017. © 2016 International Society for Magnetic Resonance in Medicine. © 2016 International Society for Magnetic Resonance in Medicine.

1H NMR spectroscopy-based interventional metabolic phenotyping

DEFF Research Database (Denmark)

Lauridsen, Michael B; Bliddal, Henning; Christensen, Robin

2010-01-01

1H NMR spectroscopy-based metabolic phenotyping was used to identify biomarkers in the plasma of patients with rheumatoid arthritis (RA). Forty-seven patients with RA (23 with active disease at baseline and 24 in remission) and 51 healthy subjects were evaluated during a one-year follow-up with a......1H NMR spectroscopy-based metabolic phenotyping was used to identify biomarkers in the plasma of patients with rheumatoid arthritis (RA). Forty-seven patients with RA (23 with active disease at baseline and 24 in remission) and 51 healthy subjects were evaluated during a one-year follow......-up with assessments of disease activity (DAS-28) and 1H NMR spectroscopy of plasma samples. Discriminant analysis provided evidence that the metabolic profiles predicted disease severity. Cholesterol, lactate, acetylated glycoprotein, and lipid signatures were found to be candidate biomarkers for disease severity.......0007). However, after 31 days of optimized therapy, the two patient groups were not significantly different (P=0.91). The metabolic profiles of both groups of RA patients were different from the healthy subjects. 1H NMR-based metabolic phenotyping of plasma samples in patients with RA is well suited...

Composition and structure of natural organic matter through advanced nuclear magnetic resonance techniques

Directory of Open Access Journals (Sweden)

Dainan Zhang

2017-02-01

Full Text Available Abstract Natural organic matter (NOM plays important roles in biological, chemical, and physical processes within the terrestrial and aquatic ecosystem. Despite its importance, a clear and exhaustive knowledge on NOM chemistry still lacks. Aiming to prove that advanced solid-state 13C nuclear magnetic resonance (NMR techniques may contribute to fill such a gap, in this paper we reported relevant examples of its applicability to NOM components, such as biomass, deposition material, sediments, and kerogen samples. It is found that nonhydrolyzable organic carbons (NHC, chars, and polymethylene carbons are important in the investigated samples. The structure of each of the NHC fractions is similar to that of kerogens, highlighting the importance of selective preservation of NOM to the kerogen origin in the investigated aquatic ecosystems. Moreover, during the artificial maturation experiments of kerogen, the chemical and structural characteristics such as protonated aromatic, nonprotonated carbons, and aromatic cluster size play important roles in the origin and variation of nanoporosity during kerogen maturation. Graphical abstract NMR parameters of thermally stimulated kerogens

Advances in solid-state NMR of cellulose.

Science.gov (United States)

Foston, Marcus

2014-06-01

Nuclear magnetic resonance (NMR) spectroscopy is a well-established analytical and enabling technology in biofuel research. Over the past few decades, lignocellulosic biomass and its conversion to supplement or displace non-renewable feedstocks has attracted increasing interest. The application of solid-state NMR spectroscopy has long been seen as an important tool in the study of cellulose and lignocellulose structure, biosynthesis, and deconstruction, especially considering the limited number of effective solvent systems and the significance of plant cell wall three-dimensional microstructure and component interaction to conversion yield and rate profiles. This article reviews common and recent applications of solid-state NMR spectroscopy methods that provide insight into the structural and dynamic processes of cellulose that control bulk properties and biofuel conversion. Copyright © 2014 Elsevier Ltd. All rights reserved.

Self-diffusion measurements in heterogeneous systems using NMR pulsed field gradient technique

International Nuclear Information System (INIS)

Heink, W.; Kaerger, J.; Walter, A.

1978-01-01

The experimental pecularities of the NMR pulsed field gradient technique are critical surveyed in its application to zeolite adsorbate adsorbent systems. After a presentation of the different transport parameters accessible by this technique, the consequences of the existence of inner field gradients being inherent to heterogeneous systems are analyzed. Experimental conditions and consequences of an application of pulsed field gradients of high intensity which are necessary for the measurement of small intracrystalline self-diffusion coefficients, are discussed. Gradient pulses of 0.15 Tcm -1 with pulse widths of 2 ms maximum and relative deviations of less than 0.01 per mille can be realized. Since for a number of adsorbate adsorbent systems a distinct dependence of the intracrystalline self-diffusion coeffcients on adsorbate concentration is observed, determination of zeolite pore fiiling factor is of considerable importance for the interpretation of the diffusivities obtained. It is demonstrated that also this information can be obtained by NMR technique in a straightforward way with a mean error of less than 5 to 10 %. Applying this new method and using an optimum experimental device as described, pore filling factor dependences of the self-diffusion coefficients of alkanes in NaX zeolites can be followed over more than two orders of magnitude. (author)

Principles of modern radar advanced techniques

CERN Document Server

Melvin, William

2012-01-01

Principles of Modern Radar: Advanced Techniques is a professional reference for practicing engineers that provides a stepping stone to advanced practice with in-depth discussions of the most commonly used advanced techniques for radar design. It will also serve advanced radar academic and training courses with a complete set of problems for students as well as solutions for instructors.

The GNAT: A new tool for processing NMR data.

Science.gov (United States)

Castañar, Laura; Poggetto, Guilherme Dal; Colbourne, Adam A; Morris, Gareth A; Nilsson, Mathias

2018-06-01

The GNAT (General NMR Analysis Toolbox) is a free and open-source software package for processing, visualising, and analysing NMR data. It supersedes the popular DOSY Toolbox, which has a narrower focus on diffusion NMR. Data import of most common formats from the major NMR platforms is supported, as well as a GNAT generic format. Key basic processing of NMR data (e.g., Fourier transformation, baseline correction, and phasing) is catered for within the program, as well as more advanced techniques (e.g., reference deconvolution and pure shift FID reconstruction). Analysis tools include DOSY and SCORE for diffusion data, ROSY T 1 /T 2 estimation for relaxation data, and PARAFAC for multilinear analysis. The GNAT is written for the MATLAB® language and comes with a user-friendly graphical user interface. The standard version is intended to run with a MATLAB installation, but completely free-standing compiled versions for Windows, Mac, and Linux are also freely available. © 2018 The Authors Magnetic Resonance in Chemistry Published by John Wiley & Sons Ltd.

I. Advances in NMR Signal Processing. II. Spin Dynamics in Quantum Dissipative Systems

Energy Technology Data Exchange (ETDEWEB)

Lin, Yung-Ya [Univ. of California, Berkeley, CA (United States)

1998-11-01

Part I. Advances in IVMR Signal Processing. Improvements of sensitivity and resolution are two major objects in the development of NMR/MRI. A signal enhancement method is first presented which recovers signal from noise by a judicious combination of a priordmowledge to define the desired feasible solutions and a set theoretic estimation for restoring signal properties that have been lost due to noise contamination. The effect of noise can be significantly mitigated through the process of iteratively modifying the noisy data set to the smallest degree necessary so that it possesses a collection of prescribed properties and also lies closest to the original data set. A novel detection-estimation scheme is then introduced to analyze noisy and/or strongly damped or truncated FIDs. Based on exponential modeling, the number of signals is detected based on information estimated using the matrix pencil method. theory and the spectral parameters are Part II. Spin Dynamics in body dipole-coupled systems Quantum Dissipative Systems. Spin dynamics in manyconstitutes one of the most fundamental problems in magnetic resonance and condensed-matter physics. Its many-spin nature precludes any rigorous treatment. ‘Therefore, the spin-boson model is adopted to describe in the rotating frame the influence of the dipolar local fields on a tagged spin. Based on the polaronic transform and a perturbation treatment, an analytical solution is derived, suggesting the existence of self-trapped states in the. strong coupling limit, i.e., when transverse local field >> longitudinal local field. Such nonlinear phenomena originate from the joint action of the lattice fluctuations and the reaction field. Under semiclassical approximation, it is found that the main effect of the reaction field is the renormalization of the Hamiltonian of interest. Its direct consequence is the two-step relaxation process: the spin is initially localized in a quasiequilibrium state, which is later detrapped by

High-field EPR on membrane proteins - crossing the gap to NMR.

Science.gov (United States)

Möbius, Klaus; Lubitz, Wolfgang; Savitsky, Anton

2013-11-01

In this review on advanced EPR spectroscopy, which addresses both the EPR and NMR communities, considerable emphasis is put on delineating the complementarity of NMR and EPR concerning the measurement of molecular interactions in large biomolecules. From these interactions, detailed information can be revealed on structure and dynamics of macromolecules embedded in solution- or solid-state environments. New developments in pulsed microwave and sweepable cryomagnet technology as well as ultrafast electronics for signal data handling and processing have pushed to new horizons the limits of EPR spectroscopy and its multifrequency extensions concerning the sensitivity of detection, the selectivity with respect to interactions, and the resolution in frequency and time domains. One of the most important advances has been the extension of EPR to high magnetic fields and microwave frequencies, very much in analogy to what happens in NMR. This is exemplified by referring to ongoing efforts for signal enhancement in both NMR and EPR double-resonance techniques by exploiting dynamic nuclear or electron spin polarization via unpaired electron spins and their electron-nuclear or electron-electron interactions. Signal and resolution enhancements are particularly spectacular for double-resonance techniques such as ENDOR and PELDOR at high magnetic fields. They provide greatly improved orientational selection for disordered samples that approaches single-crystal resolution at canonical g-tensor orientations - even for molecules with small g-anisotropies. Exchange of experience between the EPR and NMR communities allows for handling polarization and resolution improvement strategies in an optimal manner. Consequently, a dramatic improvement of EPR detection sensitivity could be achieved, even for short-lived paramagnetic reaction intermediates. Unique structural and dynamic information is thus revealed that can hardly be obtained by any other analytical techniques. Micromolar

Review of advanced imaging techniques

Directory of Open Access Journals (Sweden)

Yu Chen

2012-01-01

Full Text Available Pathology informatics encompasses digital imaging and related applications. Several specialized microscopy techniques have emerged which permit the acquisition of digital images ("optical biopsies" at high resolution. Coupled with fiber-optic and micro-optic components, some of these imaging techniques (e.g., optical coherence tomography are now integrated with a wide range of imaging devices such as endoscopes, laparoscopes, catheters, and needles that enable imaging inside the body. These advanced imaging modalities have exciting diagnostic potential and introduce new opportunities in pathology. Therefore, it is important that pathology informaticists understand these advanced imaging techniques and the impact they have on pathology. This paper reviews several recently developed microscopic techniques, including diffraction-limited methods (e.g., confocal microscopy, 2-photon microscopy, 4Pi microscopy, and spatially modulated illumination microscopy and subdiffraction techniques (e.g., photoactivated localization microscopy, stochastic optical reconstruction microscopy, and stimulated emission depletion microscopy. This article serves as a primer for pathology informaticists, highlighting the fundamentals and applications of advanced optical imaging techniques.

Functional studies using NMR

International Nuclear Information System (INIS)

McCready, V.R.; Leach, M.O.; Sutton; Ell, P.

1986-01-01

The object of this book is to discuss and evaluate an area of Nuclear Magnetic Resonance which to date has been less emphasized than it might be, namely the use of NMR for functional studies. The book commences with a discussion of the areas in which the NMR techniques might be needed due to deficiencies in other techniques. The physics of NMR especially relating to functional measurement are then explained. Technical factors in producing functional images are discussed and the use of paramagnetic substances for carrying out flow studies are detailed. Particular attention is paid to specific studies in the various organs. The book ends with a survey of imaging in each organ and the relation of NMR images to other techniques such as ultrasound, nuclear medicine and X-rays

Pediatric brain MRI. Pt. 2. Advanced techniques

Energy Technology Data Exchange (ETDEWEB)

Ho, Mai-Lan; Campeau, Norbert G.; Welker, Kirk M. [Mayo Clinic, Department of Radiology, Rochester, MN (United States); Ngo, Thang D. [Nemours Children' s Hospital, Department of Radiology, Orlando, FL (United States); Udayasankar, Unni K. [University of Arizona, Department of Radiology, Tucson, AZ (United States)

2017-05-15

Pediatric neuroimaging is a complex and specialized field that uses magnetic resonance (MR) imaging as the workhorse for diagnosis. MR protocols should be tailored to the specific indication and reviewed by the supervising radiologist in real time. Targeted advanced imaging sequences can be added to provide information regarding tissue microstructure, perfusion, metabolism and function. In part 2 of this review, we highlight the utility of advanced imaging techniques for superior evaluation of pediatric neurologic disease. We focus on the following techniques, with clinical examples: phase-contrast imaging, perfusion-weighted imaging, vessel wall imaging, diffusion tensor imaging, task-based functional MRI and MR spectroscopy. (orig.)

NMR imaging: A 'chemical' microscope for coal analysis

International Nuclear Information System (INIS)

French, D.C.; Dieckman, S.L.; Gopalsami, N.; Botto, R.E.

1991-01-01

This paper presents a new three-dimensional (3-D) nuclear magnetic resonance (NMR) imaging technique for spatially mapping proton distributions in whole coals and solvent-swollen coal samples. The technique is based on a 3-D back-projection protocol for data acquisition, and a reconstruction technique based on 3-D Radon transform inversion. In principle, the 3-D methodology provides higher spatial resolution of solid materials than is possible with conventional slice-selection protocols. The applicability of 3-D NMR imaging has been demonstrated by mapping the maceral phases in Utah Blind Canyon (APCS number-sign 6) coal and the distribution of mobile phases in Utah coal swollen with deuterated and protic pyridine. 7 refs., 5 figs

Protein folding kinetics by combined use of rapid mixing techniques and NMR observation of individual amide protons

International Nuclear Information System (INIS)

Roder, H.; Wuethrich, K.

1986-01-01

A method to be used for experimental studies of protein folding introduced by Schmid and Baldwin, which is based on the competition between amide hydrogen exchange and protein refolding, was extended by using rapid mixing techniques and 1 H NMR to provide site-resolved kinetic information on the early phases of protein structure acquisition. In this method, a protonated solution of the unfolded protein is rapidly mixed with a deuterated buffer solution at conditions assuring protein refolding in the mixture. This simultaneously initiates the exchange of unprotected amide protons with solvent deuterium and the refolding of protein segments which can protect amide groups from further exchange. After variable reaction times the amide proton exchange is quenched while folding to the native form continues to completion. By using 1 H NMR, the extent of exchange at individual amide sites is then measured in the refolded protein. Competition experiments at variable reaction times or variable pH indicate the time at which each amide group is protected in the refolding process. This technique was applied to the basic pancreatic trypsin inhibitor, for which sequence-specific assignments of the amide proton NMR lines had previously been obtained. For eight individual amide protons located in the beta-sheet and the C-terminal alpha-helix of this protein, apparent refolding rates in the range from 15 s-1 to 60 s-1 were observed. These rates are on the time scale of the fast folding phase observed with optical probes

Computational Diffusion Magnetic Resonance Imaging Based on Time-Dependent Bloch NMR Flow Equation and Bessel Functions.

Science.gov (United States)

Awojoyogbe, Bamidele O; Dada, Michael O; Onwu, Samuel O; Ige, Taofeeq A; Akinwande, Ninuola I

2016-04-01

Magnetic resonance imaging (MRI) uses a powerful magnetic field along with radio waves and a computer to produce highly detailed "slice-by-slice" pictures of virtually all internal structures of matter. The results enable physicians to examine parts of the body in minute detail and identify diseases in ways that are not possible with other techniques. For example, MRI is one of the few imaging tools that can see through bones, making it an excellent tool for examining the brain and other soft tissues. Pulsed-field gradient experiments provide a straightforward means of obtaining information on the translational motion of nuclear spins. However, the interpretation of the data is complicated by the effects of restricting geometries as in the case of most cancerous tissues and the mathematical concept required to account for this becomes very difficult. Most diffusion magnetic resonance techniques are based on the Stejskal-Tanner formulation usually derived from the Bloch-Torrey partial differential equation by including additional terms to accommodate the diffusion effect. Despite the early success of this technique, it has been shown that it has important limitations, the most of which occurs when there is orientation heterogeneity of the fibers in the voxel of interest (VOI). Overcoming this difficulty requires the specification of diffusion coefficients as function of spatial coordinate(s) and such a phenomenon is an indication of non-uniform compartmental conditions which can be analyzed accurately by solving the time-dependent Bloch NMR flow equation analytically. In this study, a mathematical formulation of magnetic resonance flow sequence in restricted geometry is developed based on a general second order partial differential equation derived directly from the fundamental Bloch NMR flow equations. The NMR signal is obtained completely in terms of NMR experimental parameters. The process is described based on Bessel functions and properties that can make it

Establishing structure-property correlations and classification of base oils using statistical techniques and artificial neural networks

International Nuclear Information System (INIS)

Kapur, G.S.; Sastry, M.I.S.; Jaiswal, A.K.; Sarpal, A.S.

2004-01-01

The present paper describes various classification techniques like cluster analysis, principal component (PC)/factor analysis to classify different types of base stocks. The API classification of base oils (Group I-III) has been compared to a more detailed NMR derived chemical compositional and molecular structural parameters based classification in order to point out the similarities of the base oils in the same group and the differences between the oils placed in different groups. The detailed compositional parameters have been generated using 1 H and 13 C nuclear magnetic resonance (NMR) spectroscopic methods. Further, oxidation stability, measured in terms of rotating bomb oxidation test (RBOT) life, of non-conventional base stocks and their blends with conventional base stocks, has been quantitatively correlated with their 1 H NMR and elemental (sulphur and nitrogen) data with the help of multiple linear regression (MLR) and artificial neural networks (ANN) techniques. The MLR based model developed using NMR and elemental data showed a high correlation between the 'measured' and 'estimated' RBOT values for both training (R=0.859) and validation (R=0.880) data sets. The ANN based model, developed using fewer number of input variables (only 1 H NMR data) also showed high correlation between the 'measured' and 'estimated' RBOT values for training (R=0.881), validation (R=0.860) and test (R=0.955) data sets

NMR imaging and pharmaceutical sciences

International Nuclear Information System (INIS)

Beall, P.T.; Good, W.R.

1986-01-01

Described is the technique of NMR-imaging in diagnostic medicine. Proton and phosphorus NMR in diagnosis of abnormal tissue pathology. Discussed is the value of NMR to the pharmaceutical sciences. NMR may play an important role in monitoring the response of tissues to drugs, determining the localization of drugs, performing real time pharmacokinetics and testing the use of NMR contrast pharmaceuticals

Cânfora: um bom modelo para ilustrar técnicas de RMN Camphor: a good model for illustrating NMR techniques

Directory of Open Access Journals (Sweden)

Julliane Diniz Yoneda

2007-01-01

Full Text Available The use of Nuclear Magnetic Resonance spectroscopy to establish the three-dimensional structures of molecules is an important component of modern Chemistry courses. The combination of techniques that can be used for this purpose is conveniently illustrated by their application to the camphor molecule. This paper presents applications of several techniques used in NMR spectral interpretation in an increasing order of complexity. The result of individual experiments is illustrated in order to familiarize the user with the way connectivity through bonds and through space is established from 1D/2D-NMR spectra and molecular stereochemistry is determined from different NMR experiments.

Evaluation of Pacific white shrimp (Litopenaeus vannamei health during a superintensive aquaculture growout using NMR-based metabolomics.

Directory of Open Access Journals (Sweden)

Tracey B Schock

Full Text Available Success of the shrimp aquaculture industry requires technological advances that increase production and environmental sustainability. Indoor, superintensive, aquaculture systems are being developed that permit year-round production of farmed shrimp at high densities. These systems are intended to overcome problems of disease susceptibility and of water quality issues from waste products, by operating as essentially closed systems that promote beneficial microbial communities (biofloc. The resulting biofloc can assimilate and detoxify wastes, may provide nutrition for the farmed organisms resulting in improved growth, and may aid in reducing disease initiated from external sources. Nuclear magnetic resonance (NMR-based metabolomic techniques were used to assess shrimp health during a full growout cycle from the nursery phase through harvest in a minimal-exchange, superintensive, biofloc system. Aberrant shrimp metabolomes were detected from a spike in total ammonia nitrogen in the nursery, from a reduced feeding period that was a consequence of surface scum build-up in the raceway, and from the stocking transition from the nursery to the growout raceway. The biochemical changes in the shrimp that were induced by the stressors were essential for survival and included nitrogen detoxification and energy conservation mechanisms. Inosine and trehalose may be general biomarkers of stress in Litopenaeus vannamei. This study demonstrates one aspect of the practicality of using NMR-based metabolomics to enhance the aquaculture industry by providing physiological insight into common environmental stresses that may limit growth or better explain reduced survival and production.

Evaluation of Pacific White Shrimp (Litopenaeus vannamei) Health during a Superintensive Aquaculture Growout Using NMR-Based Metabolomics

Science.gov (United States)

Schock, Tracey B.; Duke, Jessica; Goodson, Abby; Weldon, Daryl; Brunson, Jeff; Leffler, John W.; Bearden, Daniel W.

2013-01-01

Success of the shrimp aquaculture industry requires technological advances that increase production and environmental sustainability. Indoor, superintensive, aquaculture systems are being developed that permit year-round production of farmed shrimp at high densities. These systems are intended to overcome problems of disease susceptibility and of water quality issues from waste products, by operating as essentially closed systems that promote beneficial microbial communities (biofloc). The resulting biofloc can assimilate and detoxify wastes, may provide nutrition for the farmed organisms resulting in improved growth, and may aid in reducing disease initiated from external sources. Nuclear magnetic resonance (NMR)-based metabolomic techniques were used to assess shrimp health during a full growout cycle from the nursery phase through harvest in a minimal-exchange, superintensive, biofloc system. Aberrant shrimp metabolomes were detected from a spike in total ammonia nitrogen in the nursery, from a reduced feeding period that was a consequence of surface scum build-up in the raceway, and from the stocking transition from the nursery to the growout raceway. The biochemical changes in the shrimp that were induced by the stressors were essential for survival and included nitrogen detoxification and energy conservation mechanisms. Inosine and trehalose may be general biomarkers of stress in Litopenaeus vannamei. This study demonstrates one aspect of the practicality of using NMR-based metabolomics to enhance the aquaculture industry by providing physiological insight into common environmental stresses that may limit growth or better explain reduced survival and production. PMID:23555690

Fourier transform n.m.r. spectroscopy

International Nuclear Information System (INIS)

Shaw, D.

1976-01-01

This book is orientated to techniques rather than applications. The basic theory of n.m.r. is dealt with in a unified approach to the Fourier theory. The middle section of the book concentrates on the practical aspects of Fourier n.m.r., both instrumental and experimental. The final chapters briefly cover general application of n.m.r., but concentrate strongly on those areas where Fourier n.m.r. can give information which is not available by conventional techniques

Fragment based drug discovery: practical implementation based on ¹⁹F NMR spectroscopy.

Science.gov (United States)

Jordan, John B; Poppe, Leszek; Xia, Xiaoyang; Cheng, Alan C; Sun, Yax; Michelsen, Klaus; Eastwood, Heather; Schnier, Paul D; Nixey, Thomas; Zhong, Wenge

2012-01-26

Fragment based drug discovery (FBDD) is a widely used tool for discovering novel therapeutics. NMR is a powerful means for implementing FBDD, and several approaches have been proposed utilizing (1)H-(15)N heteronuclear single quantum coherence (HSQC) as well as one-dimensional (1)H and (19)F NMR to screen compound mixtures against a target of interest. While proton-based NMR methods of fragment screening (FBS) have been well documented and are widely used, the use of (19)F detection in FBS has been only recently introduced (Vulpetti et al. J. Am. Chem. Soc.2009, 131 (36), 12949-12959) with the aim of targeting "fluorophilic" sites in proteins. Here, we demonstrate a more general use of (19)F NMR-based fragment screening in several areas: as a key tool for rapid and sensitive detection of fragment hits, as a method for the rapid development of structure-activity relationship (SAR) on the hit-to-lead path using in-house libraries and/or commercially available compounds, and as a quick and efficient means of assessing target druggability.

Theory of NMR probe design

International Nuclear Information System (INIS)

Schnall, M.D.

1988-01-01

The NMR probe is the intrinsic part of the NMR system which allows transmission of a stimulus to a sample and the reception of a resulting signal from a sample. NMR probes are used in both imaging and spectroscopy. Optimal probe design is important to the production of adequate signal/moise. It is important for anyone using NMR techniques to understand how NMR probes work and how to optimize probe design

Two dimensional solid state NMR

International Nuclear Information System (INIS)

Kentgens, A.P.M.

1987-01-01

This thesis illustrates, by discussing some existing and newly developed 2D solid state experiments, that two-dimensional NMR of solids is a useful and important extension of NMR techniques. Chapter 1 gives an overview of spin interactions and averaging techniques important in solid state NMR. As 2D NMR is already an established technique in solutions, only the basics of two dimensional NMR are presented in chapter 2, with an emphasis on the aspects important for solid spectra. The following chapters discuss the theoretical background and applications of specific 2D solid state experiments. An application of 2D-J resolved NMR, analogous to J-resolved spectroscopy in solutions, to natural rubber is given in chapter 3. In chapter 4 the anisotropic chemical shift is mapped out against the heteronuclear dipolar interaction to obtain information about the orientation of the shielding tensor in poly-(oxymethylene). Chapter 5 concentrates on the study of super-slow molecular motions in polymers using a variant of the 2D exchange experiment developed by us. Finally chapter 6 discusses a new experiment, 2D nutation NMR, which makes it possible to study the quadrupole interaction of half-integer spins. 230 refs.; 48 figs.; 8 tabs

Advanced Techniques in Biophysics

CERN Document Server

Arrondo, José Luis R

2006-01-01

Technical advancements are basic elements in our life. In biophysical studies, new applications and improvements in well-established techniques are being implemented every day. This book deals with advancements produced not only from a technical point of view, but also from new approaches that are being taken in the study of biophysical samples, such as nanotechniques or single-cell measurements. This book constitutes a privileged observatory for reviewing novel applications of biophysical techniques that can help the reader enter an area where the technology is progressing quickly and where a comprehensive explanation is not always to be found.

NMR-based urine analysis in rats: prediction of proximal tubule kidney toxicity and phospholipidosis.

Science.gov (United States)

Lienemann, Kai; Plötz, Thomas; Pestel, Sabine

2008-01-01

The aim of safety pharmacology is early detection of compound-induced side-effects. NMR-based urine analysis followed by multivariate data analysis (metabonomics) identifies efficiently differences between toxic and non-toxic compounds; but in most cases multiple administrations of the test compound are necessary. We tested the feasibility of detecting proximal tubule kidney toxicity and phospholipidosis with metabonomics techniques after single compound administration as an early safety pharmacology approach. Rats were treated orally, intravenously, inhalatively or intraperitoneally with different test compounds. Urine was collected at 0-8 h and 8-24 h after compound administration, and (1)H NMR-patterns were recorded from the samples. Variation of post-processing and feature extraction methods led to different views on the data. Support Vector Machines were trained on these different data sets and then aggregated as experts in an Ensemble. Finally, validity was monitored with a cross-validation study using a training, validation, and test data set. Proximal tubule kidney toxicity could be predicted with reasonable total classification accuracy (85%), specificity (88%) and sensitivity (78%). In comparison to alternative histological studies, results were obtained quicker, compound need was reduced, and very importantly fewer animals were needed. In contrast, the induction of phospholipidosis by the test compounds could not be predicted using NMR-based urine analysis or the previously published biomarker PAG. NMR-based urine analysis was shown to effectively predict proximal tubule kidney toxicity after single compound administration in rats. Thus, this experimental design allows early detection of toxicity risks with relatively low amounts of compound in a reasonably short period of time.

Fast method of NMR imaging based on trains of spin echoes

International Nuclear Information System (INIS)

Hennel, F.

1993-01-01

A theoretical introduction to Fourier NMR imaging and a discussion of fast methods are presented. Then an application of the method of echo-planar imaging (EPI) with spin echoes in a micro-imaging system is described together with introduced modifications of the sequence. A new technique for the measurement of flow profiles in liquids which results from a modification of x-pulsed EPI is presented. The development of new software for a NMR micro-imaging system is described, too. 51 refs, 29 refs

NMR in a crystallography-based high-throughput protein structure-determination environment

International Nuclear Information System (INIS)

Wüthrich, Kurt

2010-01-01

As an introduction to three papers on comparisons of corresponding crystal and NMR solution structures determined by the Joint Center for Structural Genomics (JCSG), an outline is provided of the JCSG strategy for combined use of the two techniques. A special commentary addresses the potentialities of the concept of ‘reference crystal structures’, which is introduced in the following three papers. An introduction is provided to three papers which compare corresponding protein crystal and NMR solution structures determined by the Joint Center for Structural Genomics (JCSG). Special mention is made of the JCSG strategy for combined use of the two techniques, and of potential applications of the concept of ‘reference crystal structures’, which is introduced in the following three papers

NMRFx Processor: a cross-platform NMR data processing program

International Nuclear Information System (INIS)

Norris, Michael; Fetler, Bayard; Marchant, Jan; Johnson, Bruce A.

2016-01-01

NMRFx Processor is a new program for the processing of NMR data. Written in the Java programming language, NMRFx Processor is a cross-platform application and runs on Linux, Mac OS X and Windows operating systems. The application can be run in both a graphical user interface (GUI) mode and from the command line. Processing scripts are written in the Python programming language and executed so that the low-level Java commands are automatically run in parallel on computers with multiple cores or CPUs. Processing scripts can be generated automatically from the parameters of NMR experiments or interactively constructed in the GUI. A wide variety of processing operations are provided, including methods for processing of non-uniformly sampled datasets using iterative soft thresholding. The interactive GUI also enables the use of the program as an educational tool for teaching basic and advanced techniques in NMR data analysis.

NMRFx Processor: a cross-platform NMR data processing program

Energy Technology Data Exchange (ETDEWEB)

Norris, Michael; Fetler, Bayard [One Moon Scientific, Inc. (United States); Marchant, Jan [University of Maryland Baltimore County, Howard Hughes Medical Institute (United States); Johnson, Bruce A., E-mail: bruce.johnson@asrc.cuny.edu [One Moon Scientific, Inc. (United States)

2016-08-15

NMRFx Processor is a new program for the processing of NMR data. Written in the Java programming language, NMRFx Processor is a cross-platform application and runs on Linux, Mac OS X and Windows operating systems. The application can be run in both a graphical user interface (GUI) mode and from the command line. Processing scripts are written in the Python programming language and executed so that the low-level Java commands are automatically run in parallel on computers with multiple cores or CPUs. Processing scripts can be generated automatically from the parameters of NMR experiments or interactively constructed in the GUI. A wide variety of processing operations are provided, including methods for processing of non-uniformly sampled datasets using iterative soft thresholding. The interactive GUI also enables the use of the program as an educational tool for teaching basic and advanced techniques in NMR data analysis.

Comparative 1H NMR-based metabonomic analysis of HIV-1 sera

International Nuclear Information System (INIS)

Philippeos, C.; Steffens, F. E.; Meyer, D.

2009-01-01

1 H NMR spectroscopy of sera from HIV-1 infected and uninfected individuals was performed on 300 and 600 MHz instruments. The resultant spectra were automatically data reduced to 90 and 180 integral segments of equal length. Analysis of variance identified significant differences between the sample groups, especially for the samples analyzed on 600 MHz and reduced to fewer segments. Linear discriminant analysis correctly classified 100% of the samples analyzed on the 300 MHz NMR (reduced to 180 segments); an increase in instrument sensitivity resulted in lower percentages of correctly classified samples. Multinomial logistic regression (MLR) resulted in 100% correct classification of all samples from both instruments. Thus 1 H-NMR metabonomics on either instrument distinguishes HIV-positive individuals using or not using anti retroviral therapy, but the sensitivity of the instrument impacts on data reduction. Furthermore, MLR is a novel multivariate statistical technique for improved classification of biological data analyzed in NMR

Recent advances in solid state NMR and its application to ceramics

International Nuclear Information System (INIS)

Maekawa, Hideki

2006-01-01

The basic principles of solid state NMR are explained. Four application examples contained amorphous glass, determination of defects of oxide crystal, nano particle and ionic materials. The structure of inorganic glass is measured by 29 Si, 11 B, 31 P and 23 Na NMR and Magic Angle Spinning NMR (MAS-NMR), chemical species near hydrogen by Cross-Polarization Magic Angle Spinning (CP/MAS) method, and hydrogen by Combined Rotation And Multiple Pulse Spectroscopy (CRAMPS) and MAS-NMR. Hydrous and anhydrous silicate glass with condensed 17 O was measured by 17 O Multi Quantum Magic Angle Spinning (MQ/MAS). 27 Al in slags was analyzed by 27 Al 5Q-MAS. 89 Y NMR spectrum of YSZ (Yttria Stabilization Zirconia, Y 2 O 3 -ZrO 2 ) was explained. The ion transfer phenomena in the electrolyte are observed directly by the solid state NMR. (S.Y.)

Push-through Direction Injectin NMR Automation

Science.gov (United States)

Nuclear magnetic resonance (NMR) and mass spectrometry (MS) are the two major spectroscopic techniques successfully used in metabolomics studies. The non-invasive, quantitative and reproducible characteristics make NMR spectroscopy an excellent technique for detection of endogeno...

NMR studies of isotopically labeled RNA

Energy Technology Data Exchange (ETDEWEB)

Pardi, A. [Univ. of Colorado, Boulder, CO (United States)

1994-12-01

In summary, the ability to generate NMR quantities of {sup 15}N and {sup 13}C-labeled RNAs has led to the development of heteronuclear multi-dimensional NMR techniques for simplifying the resonance assignment and structure determination of RNAs. These methods for synthesizing isotopically labeled RNAs are only several years old, and thus there are still relatively few applications of heteronuclear multi-dimensional NMR techniques to RNA. However, given the critical role that RNAs play in cellular function, one can expect to see an increasing number of NMR structural studies of biologically active RNAs.

CcpNmr AnalysisAssign: a flexible platform for integrated NMR analysis

International Nuclear Information System (INIS)

Skinner, Simon P.; Fogh, Rasmus H.; Boucher, Wayne; Ragan, Timothy J.; Mureddu, Luca G.; Vuister, Geerten W.

2016-01-01

NMR spectroscopy is an indispensably powerful technique for the analysis of biomolecules under ambient conditions, both for structural- and functional studies. However, in practice the complexity of the technique has often frustrated its application by non-specialists. In this paper, we present CcpNmr version-3, the latest software release from the Collaborative Computational Project for NMR, for all aspects of NMR data analysis, including liquid- and solid-state NMR data. This software has been designed to be simple, functional and flexible, and aims to ensure that routine tasks can be performed in a straightforward manner. We have designed the software according to modern software engineering principles and leveraged the capabilities of modern graphics libraries to simplify a variety of data analysis tasks. We describe the process of backbone assignment as an example of the flexibility and simplicity of implementing workflows, as well as the toolkit used to create the necessary graphics for this workflow. The package can be downloaded from www.ccpn.ac.uk/v3-software/downloads http://www.ccpn.ac.uk/v3-software/downloads and is freely available to all non-profit organisations.

CcpNmr AnalysisAssign: a flexible platform for integrated NMR analysis

Energy Technology Data Exchange (ETDEWEB)

Skinner, Simon P.; Fogh, Rasmus H. [University of Leicester, Department of Molecular and Cell Biology, Leicester Institute for Structural- and Chemical Biology (United Kingdom); Boucher, Wayne [University of Cambridge, Department of Biochemistry (United Kingdom); Ragan, Timothy J.; Mureddu, Luca G.; Vuister, Geerten W., E-mail: gv29@le.ac.uk [University of Leicester, Department of Molecular and Cell Biology, Leicester Institute for Structural- and Chemical Biology (United Kingdom)

2016-10-15

NMR spectroscopy is an indispensably powerful technique for the analysis of biomolecules under ambient conditions, both for structural- and functional studies. However, in practice the complexity of the technique has often frustrated its application by non-specialists. In this paper, we present CcpNmr version-3, the latest software release from the Collaborative Computational Project for NMR, for all aspects of NMR data analysis, including liquid- and solid-state NMR data. This software has been designed to be simple, functional and flexible, and aims to ensure that routine tasks can be performed in a straightforward manner. We have designed the software according to modern software engineering principles and leveraged the capabilities of modern graphics libraries to simplify a variety of data analysis tasks. We describe the process of backbone assignment as an example of the flexibility and simplicity of implementing workflows, as well as the toolkit used to create the necessary graphics for this workflow. The package can be downloaded from www.ccpn.ac.uk/v3-software/downloads http://www.ccpn.ac.uk/v3-software/downloads and is freely available to all non-profit organisations.

The characterisation of polymers using pulsed NMR

International Nuclear Information System (INIS)

Charlesby, A.

1983-01-01

Broad line pulsed NMR is applied to obtain information on radiation-induced polymer changes and other aspects of polymer science based on the interpretation of spin-spin relaxation curves. Calculations are made to determine the molecular weight, the crosslink density of simple, low molecular weight, flexible polymers. For higher molecular weight polymers, a conclusion can be drawn on the concentrations of entangled and crosslinked units by means of pulsed NMR. Some typical applications of the technique are illustrated by the examples of polyethylenes, rubbers, filled polymeric systems and aqueous polyethylene oxide solutions. The morphology of polymers can be followed by pulsed NMR. (V.N.)

Annual reports on NMR spectroscopy

CERN Document Server

Webb, Graham A; McCarthy, M J

1995-01-01

Over recent years, no other technique has grown to such importance as that of NMR spectroscopy. It is used in all branches of science where precise structural determination is required and where the nature of interactions and reactions in solution is being studied. Annual Reports on NMR Spectroscopy has established itself as a means for the specialist and non-specialist alike to become familiar with new applications of the technique in all branches of chemistry, including biochemistry, and pharmaceutics. This volume focuses on theoretical aspects of NMR nuclear shielding and on applications of

Spectroscopic techniques (Moessbauer spectrometry, NMR, ESR...) as tools to resolve doubtful NMR images: Study of the craniopharyngioma tumor

International Nuclear Information System (INIS)

Rimbert, J.N.; Dumas, F.; Lafargue, C.; Kellershohn, C.; Brunelle, F.; Lallemand, D.

1990-01-01

Craniopharyngioma, an intracranial tumor, exhibits hyperintensity in the Spin-Echo-T 2 -NMR image and a hyposignal in the SE-T 1 -image. However, in some cases (15-20% cases), hypersignals are seen in both SE-T 1 and T 2 -MRI. Using spectroscopic techniques, Moessbauer spectrometry in particular, we have demonstrated that the T 1 hypersignal is due to ferritin, dissolved in the cystic liquid, after tumor cell lysis, in the course of time. Other possible reasons inducing a shortening of the T 1 relaxation time (presence of lipids, intratumoral hemorrhage) have been rejected. (orig.)

$^{31}$Mg $\\beta$-NMR applied in chemistry and biochemistry

CERN Multimedia

Magnesium ions, Mg$^{2+}$, are essential in biological systems, taking part in practically all phosphate chemistry, in photosynthesis as an integral component of chlorophyll, and they are regulated via transport through selective membrane proteins. Nonetheless, the function of magnesium ions in biochemistry is difficult to characterize, as it is practically invisible to current experimental techniques. With this proposal we aim to advance the use of $^{31}$Mg $\\beta$-NMR to liquid samples, building on the experience from the successful Letter of Intent INTC-I-088 “$\\beta$-NMR as a novel technique for biological applications”. Initially a series of experiments will be conducted aiming to characterize the coordination chemistry of Mg$^{2+}$ in ionic liquids (ILs), demonstrating that it is possible within the lifetime of the radioisotope to achieve binding of Mg$^{2+}$ to a molecule dissolved in the IL. ILs are chosen as they display a very low vapor pressure, and are thus straightforwardly compatible with t...

Standardizing the experimental conditions for using urine in NMR-based metabolomic studies with a particular focus on diagnostic studies: a review

KAUST Repository

Emwas, Abdul-Hamid M.

2014-11-21

The metabolic composition of human biofluids can provide important diagnostic and prognostic information. Among the biofluids most commonly analyzed in metabolomic studies, urine appears to be particularly useful. It is abundant, readily available, easily stored and can be collected by simple, noninvasive techniques. Moreover, given its chemical complexity, urine is particularly rich in potential disease biomarkers. This makes it an ideal biofluid for detecting or monitoring disease processes. Among the metabolomic tools available for urine analysis, NMR spectroscopy has proven to be particularly well-suited, because the technique is highly reproducible and requires minimal sample handling. As it permits the identification and quantification of a wide range of compounds, independent of their chemical properties, NMR spectroscopy has been frequently used to detect or discover disease fingerprints and biomarkers in urine. Although protocols for NMR data acquisition and processing have been standardized, no consensus on protocols for urine sample selection, collection, storage and preparation in NMR-based metabolomic studies have been developed. This lack of consensus may be leading to spurious biomarkers being reported and may account for a general lack of reproducibility between laboratories. Here, we review a large number of published studies on NMR-based urine metabolic profiling with the aim of identifying key variables that may affect the results of metabolomics studies. From this survey, we identify a number of issues that require either standardization or careful accounting in experimental design and provide some recommendations for urine collection, sample preparation and data acquisition.

Standardizing the experimental conditions for using urine in NMR-based metabolomic studies with a particular focus on diagnostic studies: a review

KAUST Repository

Emwas, Abdul-Hamid M.; Luchinat, Claudio; Turano, Paola; Tenori, Leonardo; Roy, Raja; Salek, Reza M.; Ryan, Danielle; Merzaban, Jasmeen; Kaddurah-Daouk, Rima; Zeri, Ana Carolina; Nagana Gowda, G. A.; Raftery, Daniel; Wang, Yulan; Brennan, Lorraine; Wishart, David S.

2014-01-01

The metabolic composition of human biofluids can provide important diagnostic and prognostic information. Among the biofluids most commonly analyzed in metabolomic studies, urine appears to be particularly useful. It is abundant, readily available, easily stored and can be collected by simple, noninvasive techniques. Moreover, given its chemical complexity, urine is particularly rich in potential disease biomarkers. This makes it an ideal biofluid for detecting or monitoring disease processes. Among the metabolomic tools available for urine analysis, NMR spectroscopy has proven to be particularly well-suited, because the technique is highly reproducible and requires minimal sample handling. As it permits the identification and quantification of a wide range of compounds, independent of their chemical properties, NMR spectroscopy has been frequently used to detect or discover disease fingerprints and biomarkers in urine. Although protocols for NMR data acquisition and processing have been standardized, no consensus on protocols for urine sample selection, collection, storage and preparation in NMR-based metabolomic studies have been developed. This lack of consensus may be leading to spurious biomarkers being reported and may account for a general lack of reproducibility between laboratories. Here, we review a large number of published studies on NMR-based urine metabolic profiling with the aim of identifying key variables that may affect the results of metabolomics studies. From this survey, we identify a number of issues that require either standardization or careful accounting in experimental design and provide some recommendations for urine collection, sample preparation and data acquisition.

Standardizing the experimental conditions for using urine in NMR-based metabolomic studies with a particular focus on diagnostic studies: a review.

Science.gov (United States)

Emwas, Abdul-Hamid; Luchinat, Claudio; Turano, Paola; Tenori, Leonardo; Roy, Raja; Salek, Reza M; Ryan, Danielle; Merzaban, Jasmeen S; Kaddurah-Daouk, Rima; Zeri, Ana Carolina; Nagana Gowda, G A; Raftery, Daniel; Wang, Yulan; Brennan, Lorraine; Wishart, David S

The metabolic composition of human biofluids can provide important diagnostic and prognostic information. Among the biofluids most commonly analyzed in metabolomic studies, urine appears to be particularly useful. It is abundant, readily available, easily stored and can be collected by simple, noninvasive techniques. Moreover, given its chemical complexity, urine is particularly rich in potential disease biomarkers. This makes it an ideal biofluid for detecting or monitoring disease processes. Among the metabolomic tools available for urine analysis, NMR spectroscopy has proven to be particularly well-suited, because the technique is highly reproducible and requires minimal sample handling. As it permits the identification and quantification of a wide range of compounds, independent of their chemical properties, NMR spectroscopy has been frequently used to detect or discover disease fingerprints and biomarkers in urine. Although protocols for NMR data acquisition and processing have been standardized, no consensus on protocols for urine sample selection, collection, storage and preparation in NMR-based metabolomic studies have been developed. This lack of consensus may be leading to spurious biomarkers being reported and may account for a general lack of reproducibility between laboratories. Here, we review a large number of published studies on NMR-based urine metabolic profiling with the aim of identifying key variables that may affect the results of metabolomics studies. From this survey, we identify a number of issues that require either standardization or careful accounting in experimental design and provide some recommendations for urine collection, sample preparation and data acquisition.

Application progress of solid 29Si, 27Al NMR in the research of cement-based materials

International Nuclear Information System (INIS)

Feng Chunhua; Wang Xijian; Li Dongxu

2014-01-01

Background: The solid-state Nuclear Magnetic Resonance (NMR) is an effective method for the research of cement-based materials. Now it focuses on using solid 29 Si and 27 Al NMR to research the hydration structure of the cement-based materials in cement chemistry. Purpose: A theoretical guidance is proposed for solid 29 Si and 27 Al NMR technology used in cement chemistry research. Methods: We reviewed the application of solid 29 Si and 27 Al NMR in the cement-based materials and analyzed the problem among the researches. Results: This paper introduced an fundamental, relevant-conditions and basic parameters of NMR, and studied the technical parameters of solid 29 Si and 27 Ai NMR together with the relationship among the hydration structure of cement based material. Moreover, this paper reviewed the related domestic and overseas achievements in the research of hydration structure of the cement-based materials using solid 29 Si and 27 Al NMR. Conclusion: There were some problems in the research on cement-based materials by technology of solid 29 Si and 27 Al NMR. NMR will promote the Hydration theory of cement-based material greatly. (authors)

Advances in magnetic resonance 6

CERN Document Server

Waugh, John S

2013-01-01

Advances in Magnetic Resonance, Volume 6 focuses on the theoretical and practical aspects of applying magnetic resonance methods to various problems in physical chemistry, emphasizing the different aspects of the exegesis of these problems. This book discusses the gas phase magnetic resonance of electronically excited molecules; techniques for observing excited electronic states; NMR studies in liquids at high pressure; and effect of pressure on self-diffusion in liquids. The nuclear magnetic resonance investigations of organic free radicals; measurement of proton coupling constants by NMR; an

Compact NMR

Energy Technology Data Exchange (ETDEWEB)

Bluemich, Bernhard; Haber-Pohlmeier, Sabina; Zia, Wasif [RWTH Aachen Univ. (Germany). Inst. fuer Technische und Makromolekulare Chemie (ITMC)

2014-06-01

Nuclear Magnetic Resonance (NMR) spectroscopy is the most popular method for chemists to analyze molecular structures, while Magnetic Resonance Imaging (MRI) is a non-invasive diagnostic tool for medical doctors that provides high-contrast images of biological tissue. In both applications, the sample (or patient) is positioned inside a large, superconducting magnet to magnetize the atomic nuclei. Interrogating radio-frequency pulses result in frequency spectra that provide the chemist with molecular information, the medical doctor with anatomic images, and materials scientist with NMR relaxation parameters. Recent advances in magnet technology have led to a variety of small permanent magnets to allow compact and low-cost instruments. The goal of this book is to provide an introduction to the practical use of compact NMR at a level nearly as basic as the operation of a smart phone.

β-NMR sample optimization

CERN Document Server

Zakoucka, Eva

2013-01-01

During my summer student programme I was working on sample optimization for a new β-NMR project at the ISOLDE facility. The β-NMR technique is well-established in solid-state physics and just recently it is being introduced for applications in biochemistry and life sciences. The β-NMR collaboration will be applying for beam time to the INTC committee in September for three nuclei: Cu, Zn and Mg. Sample optimization for Mg was already performed last year during the summer student programme. Therefore sample optimization for Cu and Zn had to be completed as well for the project proposal. My part in the project was to perform thorough literature research on techniques studying Cu and Zn complexes in native conditions, search for relevant binding candidates for Cu and Zn applicable for ß-NMR and eventually evaluate selected binding candidates using UV-VIS spectrometry.

Solid-state NMR of inorganic semiconductors.

Science.gov (United States)

Yesinowski, James P

2012-01-01

Studies of inorganic semiconductors by solid-state NMR vary widely in terms of the nature of the samples investigated, the techniques employed to observe the NMR signal, and the types of information obtained. Compared with the NMR of diamagnetic non-semiconducting substances, important differences often result from the presence of electron or hole carriers that are the hallmark of semiconductors, and whose theoretical interpretation can be involved. This review aims to provide a broad perspective on the topic for the non-expert by providing: (1) a basic introduction to semiconductor physical concepts relevant to NMR, including common crystal structures and the various methods of making samples; (2) discussions of the NMR spin Hamiltonian, details of some of the NMR techniques and strategies used to make measurements and theoretically predict NMR parameters, and examples of how each of the terms in the Hamiltonian has provided useful information in bulk semiconductors; (3) a discussion of the additional considerations needed to interpret the NMR of nanoscale semiconductors, with selected examples. The area of semiconductor NMR is being revitalized by this interest in nanoscale semiconductors, the great improvements in NMR detection sensitivity and resolution that have occurred, and the current interest in optical pumping and spintronics-related studies. Promising directions for future research will be noted throughout.

nmr spectroscopic study and dft calculations of giao nmr shieldings

African Journals Online (AJOL)

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3Department of Physics, Arts and Science Faculty, Dumlupinar University, Kütahya, ... 1H, 13C NMR chemical shifts and 1JCH coupling constants of .... then estimated using the corresponding TMS shieldings calculated in advance at the same.

Comparative {sup 1}H NMR-based metabonomic analysis of HIV-1 sera

Energy Technology Data Exchange (ETDEWEB)

Philippeos, C. [University of Johannesburg, Department of Biochemistry (South Africa); Steffens, F. E. [University of Pretoria, Department of Statistics (South Africa); Meyer, D. [University of Pretoria, Department of Biochemistry (South Africa)], E-mail: debra.meyer@up.ac.za

2009-07-15

{sup 1}H NMR spectroscopy of sera from HIV-1 infected and uninfected individuals was performed on 300 and 600 MHz instruments. The resultant spectra were automatically data reduced to 90 and 180 integral segments of equal length. Analysis of variance identified significant differences between the sample groups, especially for the samples analyzed on 600 MHz and reduced to fewer segments. Linear discriminant analysis correctly classified 100% of the samples analyzed on the 300 MHz NMR (reduced to 180 segments); an increase in instrument sensitivity resulted in lower percentages of correctly classified samples. Multinomial logistic regression (MLR) resulted in 100% correct classification of all samples from both instruments. Thus {sup 1}H-NMR metabonomics on either instrument distinguishes HIV-positive individuals using or not using anti retroviral therapy, but the sensitivity of the instrument impacts on data reduction. Furthermore, MLR is a novel multivariate statistical technique for improved classification of biological data analyzed in NMR.

Use of NMR spectroscopy in combination with pattern recognition techniques for elucidation of origin and adulteration of foodstuffs

Energy Technology Data Exchange (ETDEWEB)

Standal, Inger Beate

2009-07-01

Consumers and food authorities are, to an increasing extent, concerned about factors such as the origin of food, how it is produced, and if it is healthy and safe. There are methods for general quality control to map the safety and nutritional value; however there is a need for suitable analytical methods to verify information such as the production method (wild/farmed), geographical origin, species, and process history of foods. This thesis evaluates the applicability of using nuclear magnetic resonance (NMR) spectroscopy combined with pattern recognition techniques for authentication of foodstuffs. Fish and marine oils were chosen as materials. 13C NMR was applied to authenticate marine oils and muscle lipids of both fatty and lean fish, according to production method (wild/farmed), geographical origin, species, and process history. 1H NMR was applied on low molecular weight compounds extracted from cod muscle to authenticate fish according to species and processing conditions. 13C NMR combined with pattern recognition techniques enabled the differentiation of marine oils according to wild/farmed and geographical origin of the raw material. It is suggested that this was mainly due to the different diets of the fish from which the oil was produced. It was also possible to authenticate marine oils according to species, and to say something about the level of mixtures detectable. The Sn-2 position specificity of fatty acids in triacylglycerols was shown to be an important characteristic to separate oils of different species. Esterified fish oil (concentrates) could easily be differentiated from natural fish oil by their 13C NMR profile. (Author)

Value of NMR logging for heavy oil characterization

Energy Technology Data Exchange (ETDEWEB)

Chen, S.; Chen, J.; Georgi, D. [Baker Hughes, Calgary, AB (Canada); Sun, B. [Chevron Energy Technology Co., Calgary, AB (Canada)

2008-07-01

Non-conventional, heavy oil fields are becoming increasingly important to the security of energy supplies and are becoming economically profitable to produce. Heavy oil reservoirs are difficult to evaluate since they are typically shallow and the connate waters are very fresh. Other heavy oil reservoirs are oil-wet where the resistivities are not indicative of saturation. Nuclear magnetic resonance (NMR) detects molecular level interactions. As such, it responds distinctively to different hydrocarbon molecules, thereby opening a new avenue for constituent analysis. This feature makes NMR a more powerful technique than bulk oil density or viscosity measurements for characterizing oils, and is the basis for detecting gas in heavy oil fields. NMR logging, which measures fluid in pore space directly, is capable of separating oil from water. It is possible to discern movable from bound water by analyzing NMR logs. The oil viscosity can be also quantified from NMR logs, NMR relaxation time and diffusivity estimates. The unique challenges for heavy oil reservoir characterization for the NMR technique were discussed with reference to the extra-fast decay of the NMR signal in response to extra-heavy oil/tars, and the lack of sensitivity in measuring very slow diffusion of heavy oil molecules. This paper presented various methods for analyzing heavy oil reservoirs in different viscosity ranges. Heavy oil fields in Venezuela, Kazakhstan, Canada, Alaska and the Middle East were analyzed using different data interpretation approaches based on the reservoir formation characteristics and the heavy oil type. NMR direct fluid typing was adequate for clean sands and carbonate reservoirs while integrated approaches were used to interpret extra heavy oils and tars. It was concluded that NMR logs can provide quantitative measures for heavy oil saturation, identify sweet spots or tar streaks, and quantify heavy oil viscosity within reasonable accuracy. 14 refs., 16 figs.

Advanced location-based technologies and services

CERN Document Server

Karimi, Hassan A

2013-01-01

Due to the rapid increase in the number of mobile device users worldwide, location-based services (LBSs) have become pervasive, and the demand for them will continue to grow. Exploring recent changes in the technology and its uses, Advanced Location-Based Technologies and Services takes an in-depth look at new and existing technologies, techniques, applications, and opportunities. Under the editorial guidance of Hassan Karimi, with contributions from experts in the field, the book examines the breadth and depth of advanced LBS technologies and techniques. The book provides up-to-date informati

GPU PRO 3 Advanced rendering techniques

CERN Document Server

Engel, Wolfgang

2012-01-01

GPU Pro3, the third volume in the GPU Pro book series, offers practical tips and techniques for creating real-time graphics that are useful to beginners and seasoned game and graphics programmers alike. Section editors Wolfgang Engel, Christopher Oat, Carsten Dachsbacher, Wessam Bahnassi, and Sebastien St-Laurent have once again brought together a high-quality collection of cutting-edge techniques for advanced GPU programming. With contributions by more than 50 experts, GPU Pro3: Advanced Rendering Techniques covers battle-tested tips and tricks for creating interesting geometry, realistic sha

Analysis of Polycyclic Aromatic Hydrocarbon (PAH Mixtures Using Diffusion-Ordered NMR Spectroscopy and Adsorption by Powdered Activated Carbon and Biochar

Directory of Open Access Journals (Sweden)

Dong An

2018-03-01

Full Text Available Analysis of polycyclic aromatic hydrocarbons (PAHs in air and water sources is a key part of environmental chemistry research, since most PAHs are well known to be associated with negative health impacts on humans. This study explores an approach for analyzing PAH mixtures with advanced nuclear magnetic resonance (NMR spectroscopic techniques including high-resolution one-dimensional (1D NMR spectroscopy and diffusion-ordered NMR spectroscopy (DOSY NMR. With this method, different kinds of PAHs can be detected and differentiated from a mixture with high resolution. The adsorption process of PAH mixtures by PAC and biochar was studied to understand the mechanism and assess the method.

Characterization of natural bentonite by NMR

International Nuclear Information System (INIS)

Leite, Sidnei Q.M.; Dieguez, Lidia C.; Menezes, Sonia M.C.; San Gil, Rosane A.S.

1993-01-01

Solid state NMR as well as several other instrumental chemical analysis techniques were used in order to characterize two natural occurring bentonite. The methodology is described. The NMR spectra, together with the other used techniques suggest that the observed differences are due to iron inclusions in tetrahedral and octahedral sites

$\\beta$-NMR of copper isotopes in ionic liquids

CERN Multimedia

We propose to test the feasibility of spin-polarization and $\\beta$-NMR studies on several short-lived copper isotopes, $^{58}$ Cu, $^{74}$Cu and $^{75}$Cu in crystals and liquids. The motivation is given by biological studies of Cu with $\\beta$-NMR in liquid samples, since Cu is present in a large number of enzymes involved in electron transfer and activation of oxygen. The technique is based on spin-polarization via optical pumping in the new VITO beamline. We will use the existing lasers, NMR magnet and NMR chambers and we will prepare a new optical pumping system. The studies will be devoted to tests of achieved $\\beta$-asymmetry in solid hosts, the behaviour of asymmetry when increasing vacuum, and finally NMR scans in ionic liquids. The achieved spin polarization will be also relevant for the plans to measure with high precision the magnetic moments of neutron-rich Cu isotopes.

Recent Advances in Wireless Indoor Localization Techniques and System

Directory of Open Access Journals (Sweden)

Zahid Farid

2013-01-01

Full Text Available The advances in localization based technologies and the increasing importance of ubiquitous computing and context-dependent information have led to a growing business interest in location-based applications and services. Today, most application requirements are locating or real-time tracking of physical belongings inside buildings accurately; thus, the demand for indoor localization services has become a key prerequisite in some markets. Moreover, indoor localization technologies address the inadequacy of global positioning system inside a closed environment, like buildings. Based on this, though, this paper aims to provide the reader with a review of the recent advances in wireless indoor localization techniques and system to deliver a better understanding of state-of-the-art technologies and motivate new research efforts in this promising field. For this purpose, existing wireless localization position system and location estimation schemes are reviewed, as we also compare the related techniques and systems along with a conclusion and future trends.

WaVPeak: Picking NMR peaks through wavelet-based smoothing and volume-based filtering

KAUST Repository

Liu, Zhi

2012-02-10

Motivation: Nuclear magnetic resonance (NMR) has been widely used as a powerful tool to determine the 3D structures of proteins in vivo. However, the post-spectra processing stage of NMR structure determination usually involves a tremendous amount of time and expert knowledge, which includes peak picking, chemical shift assignment and structure calculation steps. Detecting accurate peaks from the NMR spectra is a prerequisite for all following steps, and thus remains a key problem in automatic NMR structure determination. Results: We introduce WaVPeak, a fully automatic peak detection method. WaVPeak first smoothes the given NMR spectrum by wavelets. The peaks are then identified as the local maxima. The false positive peaks are filtered out efficiently by considering the volume of the peaks. WaVPeak has two major advantages over the state-of-the-art peak-picking methods. First, through wavelet-based smoothing, WaVPeak does not eliminate any data point in the spectra. Therefore, WaVPeak is able to detect weak peaks that are embedded in the noise level. NMR spectroscopists need the most help isolating these weak peaks. Second, WaVPeak estimates the volume of the peaks to filter the false positives. This is more reliable than intensity-based filters that are widely used in existing methods. We evaluate the performance of WaVPeak on the benchmark set proposed by PICKY (Alipanahi et al., 2009), one of the most accurate methods in the literature. The dataset comprises 32 2D and 3D spectra from eight different proteins. Experimental results demonstrate that WaVPeak achieves an average of 96%, 91%, 88%, 76% and 85% recall on 15N-HSQC, HNCO, HNCA, HNCACB and CBCA(CO)NH, respectively. When the same number of peaks are considered, WaVPeak significantly outperforms PICKY. The Author(s) 2012. Published by Oxford University Press.

NMR

International Nuclear Information System (INIS)

Kneeland, J.B.; Lee, B.C.P.; Whalen, J.P.; Knowles, R.J.R.; Cahill, P.T.

1984-01-01

Although still quite new, NMR imaging has already emerged as a safe, noninvasive, painless, and effective diagnostic modality requiring no ionizing radiation. Also, NMR appears already to have established itself as the method of choice for the examination of the brain spinal cord (excluding herniated disks). Another area in which NMR excels is in the examination of the pelvis. The use of surface coils offers the promise of visualizing structures with resolution unobtainable by any other means. In addition, NMR, with its superb visualization of vascular structures and potential ability to measure flow, may soon revolutionize the diagnosis of cardiovascular disease. Finally, NMR, through biochemically and physiologically based T/sub 1/ and T/sub 2/ indices or through spectroscopy, may provide a means of monitoring therapeutic response so as to permit tailoring of treatment to the individual patient. In short, NMR is today probably at the same stage as the x-ray was in Roentgen's day

Process of Fragment-Based Lead Discovery—A Perspective from NMR

Directory of Open Access Journals (Sweden)

Rongsheng Ma

2016-07-01

Full Text Available Fragment-based lead discovery (FBLD has proven fruitful during the past two decades for a variety of targets, even challenging protein–protein interaction (PPI systems. Nuclear magnetic resonance (NMR spectroscopy plays a vital role, from initial fragment-based screening to lead generation, because of its power to probe the intrinsically weak interactions between targets and low-molecular-weight fragments. Here, we review the NMR FBLD process from initial library construction to lead generation. We describe technical aspects regarding fragment library design, ligand- and protein-observed screening, and protein–ligand structure model generation. For weak binders, the initial hit-to-lead evolution can be guided by structural information retrieved from NMR spectroscopy, including chemical shift perturbation, transferred pseudocontact shifts, and paramagnetic relaxation enhancement. This perspective examines structure-guided optimization from weak fragment screening hits to potent leads for challenging PPI targets.

PSYCHE Pure Shift NMR Spectroscopy.

Science.gov (United States)

Foroozandeh, Mohammadali; Morris, Gareth; Nilsson, Mathias

2018-03-13

Broadband homodecoupling techniques in NMR, also known as "pure shift" methods, aim to enhance spectral resolution by suppressing the effects of homonuclear coupling interactions to turn multiplet signals into singlets. Such techniques typically work by selecting a subset of "active" nuclear spins to observe, and selectively inverting the remaining, "passive", spins to reverse the effects of coupling. Pure Shift Yielded by Chirp Excitation (PSYCHE) is one such method; it is relatively recent, but has already been successfully implemented in a range of different NMR experiments. Paradoxically, PSYCHE is one of the trickiest of pure shift NMR techniques to understand but one of the easiest to use. Here we offer some insights into theoretical and practical aspects of the method, and into the effects and importance of the experimental parameters. Some recent improvements that enhance the spectral purity of PSYCHE spectra will be presented, and some experimental frameworks including examples in 1D and 2D NMR spectroscopy, for the implementation of PSYCHE will be introduced. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Assessment of 1H NMR-based metabolomics analysis for normalization of urinary metals against creatinine.

Science.gov (United States)

Cassiède, Marc; Nair, Sindhu; Dueck, Meghan; Mino, James; McKay, Ryan; Mercier, Pascal; Quémerais, Bernadette; Lacy, Paige

2017-01-01

Proton nuclear magnetic resonance ( 1 H NMR, or NMR) spectroscopy and inductively coupled plasma-mass spectrometry (ICP-MS) are commonly used for metabolomics and metal analysis in urine samples. However, creatinine quantification by NMR for the purpose of normalization of urinary metals has not been validated. We assessed the validity of using NMR analysis for creatinine quantification in human urine samples in order to allow normalization of urinary metal concentrations. NMR and ICP-MS techniques were used to measure metabolite and metal concentrations in urine samples from 10 healthy subjects. For metabolite analysis, two magnetic field strengths (600 and 700MHz) were utilized. In addition, creatinine concentrations were determined by using the Jaffe method. Creatinine levels were strongly correlated (R 2 =0.99) between NMR and Jaffe methods. The NMR spectra were deconvoluted with a target database containing 151 metabolites that are present in urine. A total of 50 metabolites showed good correlation (R 2 =0.7-1.0) at 600 and 700MHz. Metal concentrations determined after NMR-measured creatinine normalization were comparable to previous reports. NMR analysis provided robust urinary creatinine quantification, and was sufficient for normalization of urinary metal concentrations. We found that NMR-measured creatinine-normalized urinary metal concentrations in our control subjects were similar to general population levels in Canada and the United Kingdom. Copyright © 2016 Elsevier B.V. All rights reserved.

Trispyrazolylborate Complexes: An Advanced Synthesis Experiment Using Paramagnetic NMR, Variable-Temperature NMR, and EPR Spectroscopies

Science.gov (United States)

Abell, Timothy N.; McCarrick, Robert M.; Bretz, Stacey Lowery; Tierney, David L.

2017-01-01

A structured inquiry experiment for inorganic synthesis has been developed to introduce undergraduate students to advanced spectroscopic techniques including paramagnetic nuclear magnetic resonance and electron paramagnetic resonance. Students synthesize multiple complexes with unknown first row transition metals and identify the unknown metals by…

Recent Advances in Paper-Based Sensors

Directory of Open Access Journals (Sweden)

Edith Chow

2012-08-01

Full Text Available Paper-based sensors are a new alternative technology for fabricating simple, low-cost, portable and disposable analytical devices for many application areas including clinical diagnosis, food quality control and environmental monitoring. The unique properties of paper which allow passive liquid transport and compatibility with chemicals/biochemicals are the main advantages of using paper as a sensing platform. Depending on the main goal to be achieved in paper-based sensors, the fabrication methods and the analysis techniques can be tuned to fulfill the needs of the end-user. Current paper-based sensors are focused on microfluidic delivery of solution to the detection site whereas more advanced designs involve complex 3-D geometries based on the same microfluidic principles. Although paper-based sensors are very promising, they still suffer from certain limitations such as accuracy and sensitivity. However, it is anticipated that in the future, with advances in fabrication and analytical techniques, that there will be more new and innovative developments in paper-based sensors. These sensors could better meet the current objectives of a viable low-cost and portable device in addition to offering high sensitivity and selectivity, and multiple analyte discrimination. This paper is a review of recent advances in paper-based sensors and covers the following topics: existing fabrication techniques, analytical methods and application areas. Finally, the present challenges and future outlooks are discussed.

Synchrotron-Based Microspectroscopic Analysis of Molecular and Biopolymer Structures Using Multivariate Techniques and Advanced Multi-Components Modeling

International Nuclear Information System (INIS)

Yu, P.

2008-01-01

More recently, advanced synchrotron radiation-based bioanalytical technique (SRFTIRM) has been applied as a novel non-invasive analysis tool to study molecular, functional group and biopolymer chemistry, nutrient make-up and structural conformation in biomaterials. This novel synchrotron technique, taking advantage of bright synchrotron light (which is million times brighter than sunlight), is capable of exploring the biomaterials at molecular and cellular levels. However, with the synchrotron RFTIRM technique, a large number of molecular spectral data are usually collected. The objective of this article was to illustrate how to use two multivariate statistical techniques: (1) agglomerative hierarchical cluster analysis (AHCA) and (2) principal component analysis (PCA) and two advanced multicomponent modeling methods: (1) Gaussian and (2) Lorentzian multi-component peak modeling for molecular spectrum analysis of bio-tissues. The studies indicated that the two multivariate analyses (AHCA, PCA) are able to create molecular spectral corrections by including not just one intensity or frequency point of a molecular spectrum, but by utilizing the entire spectral information. Gaussian and Lorentzian modeling techniques are able to quantify spectral omponent peaks of molecular structure, functional group and biopolymer. By application of these four statistical methods of the multivariate techniques and Gaussian and Lorentzian modeling, inherent molecular structures, functional group and biopolymer onformation between and among biological samples can be quantified, discriminated and classified with great efficiency.

NMR data-driven structure determination using NMR-I-TASSER in the CASD-NMR experiment

Energy Technology Data Exchange (ETDEWEB)

Jang, Richard [Huazhong University of Science and Technology, School of Software Engineering (China); Wang, Yan [Huazhong University of Science and Technology, School of Life Science and Technology (China); Xue, Zhidong, E-mail: zdxue@hust.edu.cn [Huazhong University of Science and Technology, School of Software Engineering (China); Zhang, Yang, E-mail: zhng@umich.edu [University of Michigan, Department of Computational Medicine and Bioinformatics (United States)

2015-08-15

NMR-I-TASSER, an adaption of the I-TASSER algorithm combining NMR data for protein structure determination, recently joined the second round of the CASD-NMR experiment. Unlike many molecular dynamics-based methods, NMR-I-TASSER takes a molecular replacement-like approach to the problem by first threading the target through the PDB to identify structural templates which are then used for iterative NOE assignments and fragment structure assembly refinements. The employment of multiple templates allows NMR-I-TASSER to sample different topologies while convergence to a single structure is not required. Retroactive and blind tests of the CASD-NMR targets from Rounds 1 and 2 demonstrate that even without using NOE peak lists I-TASSER can generate correct structure topology with 15 of 20 targets having a TM-score above 0.5. With the addition of NOE-based distance restraints, NMR-I-TASSER significantly improved the I-TASSER models with all models having the TM-score above 0.5. The average RMSD was reduced from 5.29 to 2.14 Å in Round 1 and 3.18 to 1.71 Å in Round 2. There is no obvious difference in the modeling results with using raw and refined peak lists, indicating robustness of the pipeline to the NOE assignment errors. Overall, despite the low-resolution modeling the current NMR-I-TASSER pipeline provides a coarse-grained structure folding approach complementary to traditional molecular dynamics simulations, which can produce fast near-native frameworks for atomic-level structural refinement.

Solid-State NMR Spectroscopy Proves the Presence of Penta-coordinated Sc Sites in MIL-100(Sc).

Science.gov (United States)

Giovine, Raynald; Volkringer, Christophe; Ashbrook, Sharon E; Trébosc, Julien; McKay, David; Loiseau, Thierry; Amoureux, Jean-Paul; Lafon, Olivier; Pourpoint, Frédérique

2017-07-18

Advanced solid-state NMR methods and first-principles calculations demonstrate for the first time the formation of penta-coordinated scandium sites. These coordinatively unsaturated sites were shown during the thermal activation of scandium-based metal-organic frameworks (MOFs). A 45 Sc NMR experiment allows their specific observation in activated Sc 3 BTB 2 (H 3 BTB=1,3,5-tris(4-carboxyphenyl)benzene) and MIL-100(Sc) MOFs. The assignment of the ScO 5 groups is supported by the DFT calculations of NMR parameters. The presence of ScO 5 Lewis acid sites in MIL-100(Sc) explains furthermore its catalytic activity. The first NMR experiment to probe 13 C- 45 Sc distances is also introduced. This advanced solid-state NMR pulse sequence allows the demonstration of the shrinkage of the MIL-100(Sc) network when the activation temperature is raised. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of the overall migration from silicone baking moulds into simulants and food using 1H-NMR techniques.

Science.gov (United States)

Helling, Ruediger; Mieth, Anja; Altmann, Stefan; Simat, Thomas Joachim

2009-03-01

Different silicone baking moulds (37 samples) were characterized with respect to potential migrating substances using 1H-NMR, RP-HPLC-UV/ELSD and GC techniques. In all cases cyclic organosiloxane oligomers with the formula [Si(CH3)2-O]n were identified (n = 6 ... 50). Additionally, linear, partly hydroxyl-terminated organosiloxanes HO-[Si(CH3)2-O]n-H (n = 7 ... 20) were found in 13 samples. No substances other than siloxanes could be detected, meaning the migrants mainly consist of organopolysiloxanes. Based on this knowledge, a 1H-NMR quantification method for siloxanes was established for the analysis of both simulants and foodstuffs. Validation of the 1H-NMR method gave suitable performance characteristics: limit of detection 8.7 mg kg(-1) oil, coefficient of variation 7.8% (at a level of 1.0 mg kg(-1) food). Migration studies were carried out with simulants (olive oil, isooctane, ethanol (95%), Tenax) as well as preparation of different cakes. From the 1st to 10th experiment, siloxane migration into cakes only slightly decreased, with a significant dependence on fat content. Migration never exceeded a level of 21 mg kg(-1) (3 mg dm(-2)) and was, therefore, well below the overall migration limit of 60 mg kg(-1) (10 mg dm(-2)). However, migration behaviour into simulants differed completely from these results.

Study of β-NMR for Liquid Biological Samples

CERN Document Server

Beattie, Caitlin

2017-01-01

β-NMR is an exotic form of NMR spectroscopy that allows for the characterization of matter based on the anisotropic β-decay of radioactive probe nuclei. This has been shown to be an effective spectroscopic technique for many different compounds, but its use for liquid biological samples is relatively unexplored. The work at the VITO line of ISOLDE seeks to employ this technique to study such samples. Currently, preparations are being made for an experiment to characterize DNA G-quadruplexes and their interactions with stabilizing cations. More specifically, the work in which I engaged as a summer student focused on the experiment’s liquid handling system and the stability of the relevant biological samples under vacuum.

Bentonite pore structure based on SAXS, chloride exclusion and NMR studies

International Nuclear Information System (INIS)

Muurinen, A.; Carlsson, T.

2013-11-01

Water-saturated bentonite is planned to be used in many countries as an important barrier component in high-level nuclear waste (HLW) repositories. Knowledge about the microstructure of the bentonite and the distribution of water between interlayer and non-interlayer pores is important for modelling of long-term processes. In this work the microstructure of water-saturated samples prepared from Na montmorillonite, Ca-montmorillonite, sodium bentonite MX-80 and calcium bentonite Deponit CaN were studied with nuclear magnetic resonance (NMR) and small-angle xray scattering spectroscopy (SAXS). The sample dry densities ranged between 0.3 and 1.6 g/cm 3 . The NMR technique was used to get information about the volumes of different water types in the bentonite samples. The results were obtained using 1H NMR spin-lattice T 1ρ relaxation time measurements using the short inter-pulse method. The interpretation of the NMR results was made by fitting distributions of exponentials to observed decay curves. The SAXS measurements were used to get information about the size distribution of the interlayer distance of montmorillonite. The chloride porosity measurements and Donnan exclusion calculations were used together with the SAXS results for evaluation of the bentonite microstructure. The NMR studies and SAXS studies coupled with Cl porosity measurements provided very similar pictures of how the porewater is divided in interlayer and non-interlayer water in MX-80 bentonite. In the case where MX-80 of a dry density 1.6 g/cm 3 was equilibrated with 0.1 M NaCl solution, the results indicated an interlayer porosity of 30 % and non-interlayer porosity of 12 %. The interlayer space mainly contained two water layers but also spaces with more water layers were present. The average size of the non-interlayer pores was evaluated to be 120 - 150 A. From the montmorillonite surface area 98 % was interlayer and 2 % non-interlayer. Evaluation of the interlayer and non

NMR reaction monitoring in flow synthesis.

Science.gov (United States)

Gomez, M Victoria; de la Hoz, Antonio

2017-01-01

Recent advances in the use of flow chemistry with in-line and on-line analysis by NMR are presented. The use of macro- and microreactors, coupled with standard and custom made NMR probes involving microcoils, incorporated into high resolution and benchtop NMR instruments is reviewed. Some recent selected applications have been collected, including synthetic applications, the determination of the kinetic and thermodynamic parameters and reaction optimization, even in single experiments and on the μL scale. Finally, software that allows automatic reaction monitoring and optimization is discussed.

Automics: an integrated platform for NMR-based metabonomics spectral processing and data analysis

Directory of Open Access Journals (Sweden)

Qu Lijia

2009-03-01

Full Text Available Abstract Background Spectral processing and post-experimental data analysis are the major tasks in NMR-based metabonomics studies. While there are commercial and free licensed software tools available to assist these tasks, researchers usually have to use multiple software packages for their studies because software packages generally focus on specific tasks. It would be beneficial to have a highly integrated platform, in which these tasks can be completed within one package. Moreover, with open source architecture, newly proposed algorithms or methods for spectral processing and data analysis can be implemented much more easily and accessed freely by the public. Results In this paper, we report an open source software tool, Automics, which is specifically designed for NMR-based metabonomics studies. Automics is a highly integrated platform that provides functions covering almost all the stages of NMR-based metabonomics studies. Automics provides high throughput automatic modules with most recently proposed algorithms and powerful manual modules for 1D NMR spectral processing. In addition to spectral processing functions, powerful features for data organization, data pre-processing, and data analysis have been implemented. Nine statistical methods can be applied to analyses including: feature selection (Fisher's criterion, data reduction (PCA, LDA, ULDA, unsupervised clustering (K-Mean and supervised regression and classification (PLS/PLS-DA, KNN, SIMCA, SVM. Moreover, Automics has a user-friendly graphical interface for visualizing NMR spectra and data analysis results. The functional ability of Automics is demonstrated with an analysis of a type 2 diabetes metabolic profile. Conclusion Automics facilitates high throughput 1D NMR spectral processing and high dimensional data analysis for NMR-based metabonomics applications. Using Automics, users can complete spectral processing and data analysis within one software package in most cases

Automics: an integrated platform for NMR-based metabonomics spectral processing and data analysis.

Science.gov (United States)

Wang, Tao; Shao, Kang; Chu, Qinying; Ren, Yanfei; Mu, Yiming; Qu, Lijia; He, Jie; Jin, Changwen; Xia, Bin

2009-03-16

Spectral processing and post-experimental data analysis are the major tasks in NMR-based metabonomics studies. While there are commercial and free licensed software tools available to assist these tasks, researchers usually have to use multiple software packages for their studies because software packages generally focus on specific tasks. It would be beneficial to have a highly integrated platform, in which these tasks can be completed within one package. Moreover, with open source architecture, newly proposed algorithms or methods for spectral processing and data analysis can be implemented much more easily and accessed freely by the public. In this paper, we report an open source software tool, Automics, which is specifically designed for NMR-based metabonomics studies. Automics is a highly integrated platform that provides functions covering almost all the stages of NMR-based metabonomics studies. Automics provides high throughput automatic modules with most recently proposed algorithms and powerful manual modules for 1D NMR spectral processing. In addition to spectral processing functions, powerful features for data organization, data pre-processing, and data analysis have been implemented. Nine statistical methods can be applied to analyses including: feature selection (Fisher's criterion), data reduction (PCA, LDA, ULDA), unsupervised clustering (K-Mean) and supervised regression and classification (PLS/PLS-DA, KNN, SIMCA, SVM). Moreover, Automics has a user-friendly graphical interface for visualizing NMR spectra and data analysis results. The functional ability of Automics is demonstrated with an analysis of a type 2 diabetes metabolic profile. Automics facilitates high throughput 1D NMR spectral processing and high dimensional data analysis for NMR-based metabonomics applications. Using Automics, users can complete spectral processing and data analysis within one software package in most cases. Moreover, with its open source architecture, interested

Application of 13C-labeling and 13C-13C COSY NMR experiments in the structure determination of a microbial natural product.

Science.gov (United States)

Kwon, Yun; Park, Sunghyouk; Shin, Jongheon; Oh, Dong-Chan

2014-08-01

The elucidation of the structures of complex natural products bearing many quaternary carbons remains challenging, even in this advanced spectroscopic era. (13)C-(13)C COSY NMR spectroscopy shows direct couplings between (13)C and (13)C, which comprise the backbone of a natural product. Thus, this type of experiment is particularly useful for natural products bearing consecutive quaternary carbons. However, the low sensitivity of (13)C-based NMR experiments, due to the low natural abundance of the (13)C nucleus, is problematic when applying these techniques. Our efforts in the (13)C labeling of a microbial natural product, cyclopiazonic acid (1), by feeding (13)C-labeled glucose to the fungal culture, enabled us to acquire (13)C-(13)C COSY NMR spectra on a milligram scale that clearly show the carbon backbone of the compound. This is the first application of (13)C-(13)C COSY NMR experiments for a natural product. The results suggest that (13)C-(13)C COSY NMR spectroscopy can be routinely used for the structure determination of microbial natural products by (13)C-enrichment of a compound with (13)C-glucose.

Optimized slice-selective 1H NMR experiments combined with highly accurate quantitative 13C NMR using an internal reference method

Science.gov (United States)

Jézéquel, Tangi; Silvestre, Virginie; Dinis, Katy; Giraudeau, Patrick; Akoka, Serge

2018-04-01

Isotope ratio monitoring by 13C NMR spectrometry (irm-13C NMR) provides the complete 13C intramolecular position-specific composition at natural abundance. It represents a powerful tool to track the (bio)chemical pathway which has led to the synthesis of targeted molecules, since it allows Position-specific Isotope Analysis (PSIA). Due to the very small composition range (which represents the range of variation of the isotopic composition of a given nuclei) of 13C natural abundance values (50‰), irm-13C NMR requires a 1‰ accuracy and thus highly quantitative analysis by 13C NMR. Until now, the conventional strategy to determine the position-specific abundance xi relies on the combination of irm-MS (isotopic ratio monitoring Mass Spectrometry) and 13C quantitative NMR. However this approach presents a serious drawback since it relies on two different techniques and requires to measure separately the signal of all the carbons of the analyzed compound, which is not always possible. To circumvent this constraint, we recently proposed a new methodology to perform 13C isotopic analysis using an internal reference method and relying on NMR only. The method combines a highly quantitative 1H NMR pulse sequence (named DWET) with a 13C isotopic NMR measurement. However, the recently published DWET sequence is unsuited for samples with short T1, which forms a serious limitation for irm-13C NMR experiments where a relaxing agent is added. In this context, we suggest two variants of the DWET called Multi-WET and Profiled-WET, developed and optimized to reach the same accuracy of 1‰ with a better immunity towards T1 variations. Their performance is evaluated on the determination of the 13C isotopic profile of vanillin. Both pulse sequences show a 1‰ accuracy with an increased robustness to pulse miscalibrations compared to the initial DWET method. This constitutes a major advance in the context of irm-13C NMR since it is now possible to perform isotopic analysis with high

Solid-state NMR on complex biomolecules: novel methods and applications

NARCIS (Netherlands)

Nand, D.

2011-01-01

Solid-state NMR (ssNMR) represents a versatile technique in providing atomic-resolution information without the need for crystals or fast molecular motion required for X-ray crystallography and solution-state NMR, respectively. Recent past has witnessed the ability of this technique in providing

Spectroscopic techniques (Mössbauer spectrometry, NMR, ESR,…) as tools to resolve doubtful NMR images: Study of the craniopharyngioma tumor

Science.gov (United States)

Rimbert, J. N.; Dumas, F.; Lafargue, C.; Kellershohn, C.; Brunelle, F.; Lallemand, D.

1990-07-01

Craniopharyngioma, an intracranial tumor, exhibits hyperintensity in the Spin-Echo-T2-NMR image and a hyposignal in the SE-T1-image. However, in some cases (15-20% cases), hypersignals are seen in both SE-T1 and T2-MRI. Using spectroscopic techniques, Mössbauer spectrometry in particular, we have demonstrated that the T1 hypersignal is due to ferritin, dissolved in the cystic liquid, after tumor cell lysis, in the course of time. Other possible reasons inducing a shortening of the T1 relaxation time (presence of lipids, intratumoral hemorrhage) have been rejected.

NMR reaction monitoring in flow synthesis

Directory of Open Access Journals (Sweden)

M. Victoria Gomez

2017-02-01

Full Text Available Recent advances in the use of flow chemistry with in-line and on-line analysis by NMR are presented. The use of macro- and microreactors, coupled with standard and custom made NMR probes involving microcoils, incorporated into high resolution and benchtop NMR instruments is reviewed. Some recent selected applications have been collected, including synthetic applications, the determination of the kinetic and thermodynamic parameters and reaction optimization, even in single experiments and on the μL scale. Finally, software that allows automatic reaction monitoring and optimization is discussed.

GPU Pro advanced rendering techniques

CERN Document Server

Engel, Wolfgang

2010-01-01

This book covers essential tools and techniques for programming the graphics processing unit. Brought to you by Wolfgang Engel and the same team of editors who made the ShaderX series a success, this volume covers advanced rendering techniques, engine design, GPGPU techniques, related mathematical techniques, and game postmortems. A special emphasis is placed on handheld programming to account for the increased importance of graphics on mobile devices, especially the iPhone and iPod touch.Example programs and source code can be downloaded from the book's CRC Press web page. 

NMR imaging of osteoarticular pathology

International Nuclear Information System (INIS)

Frocrain, L.; Duvauferrier, R.; Gagey, N.

1987-01-01

NMR imaging is assuming an increasingly important role in the diagnosis of osteo-articular disorders. Semiological descriptions of the mean pathological disorders of the locomotor system are presented. Some investigation strategies are proposed to compare NMR imaging with other imaging techniques in various pathological states [fr

Magic Angle Spinning NMR Metabolomics

Energy Technology Data Exchange (ETDEWEB)

Zhi Hu, Jian

2016-01-01

Nuclear Magnetic Resonance (NMR) spectroscopy is a non-destructive, quantitative, reproducible, untargeted and unbiased method that requires no or minimal sample preparation, and is one of the leading analytical tools for metabonomics research [1-3]. The easy quantification and the no need of prior knowledge about compounds present in a sample associated with NMR are advantageous over other techniques [1,4]. 1H NMR is especially attractive because protons are present in virtually all metabolites and its NMR sensitivity is high, enabling the simultaneous identification and monitoring of a wide range of low molecular weight metabolites.

GPU Pro 4 advanced rendering techniques

CERN Document Server

Engel, Wolfgang

2013-01-01

GPU Pro4: Advanced Rendering Techniques presents ready-to-use ideas and procedures that can help solve many of your day-to-day graphics programming challenges. Focusing on interactive media and games, the book covers up-to-date methods producing real-time graphics. Section editors Wolfgang Engel, Christopher Oat, Carsten Dachsbacher, Michal Valient, Wessam Bahnassi, and Sebastien St-Laurent have once again assembled a high-quality collection of cutting-edge techniques for advanced graphics processing unit (GPU) programming. Divided into six sections, the book begins with discussions on the abi

Automatic NMR-based identification of chemical reaction types in mixtures of co-occurring reactions.

Science.gov (United States)

Latino, Diogo A R S; Aires-de-Sousa, João

2014-01-01

The combination of chemoinformatics approaches with NMR techniques and the increasing availability of data allow the resolution of problems far beyond the original application of NMR in structure elucidation/verification. The diversity of applications can range from process monitoring, metabolic profiling, authentication of products, to quality control. An application related to the automatic analysis of complex mixtures concerns mixtures of chemical reactions. We encoded mixtures of chemical reactions with the difference between the (1)H NMR spectra of the products and the reactants. All the signals arising from all the reactants of the co-occurring reactions were taken together (a simulated spectrum of the mixture of reactants) and the same was done for products. The difference spectrum is taken as the representation of the mixture of chemical reactions. A data set of 181 chemical reactions was used, each reaction manually assigned to one of 6 types. From this dataset, we simulated mixtures where two reactions of different types would occur simultaneously. Automatic learning methods were trained to classify the reactions occurring in a mixture from the (1)H NMR-based descriptor of the mixture. Unsupervised learning methods (self-organizing maps) produced a reasonable clustering of the mixtures by reaction type, and allowed the correct classification of 80% and 63% of the mixtures in two independent test sets of different similarity to the training set. With random forests (RF), the percentage of correct classifications was increased to 99% and 80% for the same test sets. The RF probability associated to the predictions yielded a robust indication of their reliability. This study demonstrates the possibility of applying machine learning methods to automatically identify types of co-occurring chemical reactions from NMR data. Using no explicit structural information about the reactions participants, reaction elucidation is performed without structure elucidation of

Automatic NMR-based identification of chemical reaction types in mixtures of co-occurring reactions.

Directory of Open Access Journals (Sweden)

Diogo A R S Latino

Full Text Available The combination of chemoinformatics approaches with NMR techniques and the increasing availability of data allow the resolution of problems far beyond the original application of NMR in structure elucidation/verification. The diversity of applications can range from process monitoring, metabolic profiling, authentication of products, to quality control. An application related to the automatic analysis of complex mixtures concerns mixtures of chemical reactions. We encoded mixtures of chemical reactions with the difference between the (1H NMR spectra of the products and the reactants. All the signals arising from all the reactants of the co-occurring reactions were taken together (a simulated spectrum of the mixture of reactants and the same was done for products. The difference spectrum is taken as the representation of the mixture of chemical reactions. A data set of 181 chemical reactions was used, each reaction manually assigned to one of 6 types. From this dataset, we simulated mixtures where two reactions of different types would occur simultaneously. Automatic learning methods were trained to classify the reactions occurring in a mixture from the (1H NMR-based descriptor of the mixture. Unsupervised learning methods (self-organizing maps produced a reasonable clustering of the mixtures by reaction type, and allowed the correct classification of 80% and 63% of the mixtures in two independent test sets of different similarity to the training set. With random forests (RF, the percentage of correct classifications was increased to 99% and 80% for the same test sets. The RF probability associated to the predictions yielded a robust indication of their reliability. This study demonstrates the possibility of applying machine learning methods to automatically identify types of co-occurring chemical reactions from NMR data. Using no explicit structural information about the reactions participants, reaction elucidation is performed without structure

Comparison of PET and proton NMR imaging in the diagnosis of Alzheimer-type dementia

International Nuclear Information System (INIS)

Friedland, R.P.; Budinger, T.F.; Jagust, W.J.; Brant-Zawadzki, M.

1985-01-01

Despite recent advances in the understanding of the pathophysiology of Alzheimer's disease (AD), medical personnel remain unable to make the diagnosis noninvasively, except by exclusion. The more recently developed technique of positron emission tomography (PET) has been used with a labeled glucose analogue, ( 18 F)-2-fluoro-2-deoxy-D-glucose (FDG), to noninvasively study glucose metabolism in dementia. Specific regional alterations, particularly in the temporal-parietal cortex, have been found. Nuclear magnetic resonance (NMR) imaging is another powerful new technology that is beginning to be applied to dementia. The authors have compared the findings in PET studies using FDG with NMR imaging in two subjects with Alzheimer-type dementia

Potential effect of diaper and cotton ball contamination on NMR- and LC/MS-based metabonomics studies of urine from newborn babies.

Science.gov (United States)

Goodpaster, Aaron M; Ramadas, Eshwar H; Kennedy, Michael A

2011-02-01

Nuclear magnetic resonance (NMR) and liquid chromatography/mass spectrometry (LC/MS) based metabonomics screening of urine has great potential for discovery of biomarkers for diseases that afflict newborn and preterm infants. However, urine collection from newborn infants presents a potential confounding problem due to the possibility that contaminants might leach from materials used for urine collection and influence statistical analysis of metabonomics data. In this manuscript, we have analyzed diaper and cotton ball contamination using synthetic urine to assess its potential to influence the outcome of NMR- and LC/MS-based metabonomics studies of human infant urine. Eight diaper brands were examined using the "diaper plus cotton ball" technique. Data were analyzed using conventional principal components analysis, as well as a statistical significance algorithm developed for, and applied to, NMR data. Results showed most diaper brands had distinct contaminant profiles that could potentially influence NMR- and LC/MS-based metabonomics studies. On the basis of this study, it is recommended that diaper and cotton ball brands be characterized using metabonomics methodologies prior to initiating a metabonomics study to ensure that contaminant profiles are minimal or manageable and that the same diaper and cotton ball brands be used throughout a study to minimize variation.

Comparing pharmacophore models derived from crystallography and NMR ensembles

Science.gov (United States)

Ghanakota, Phani; Carlson, Heather A.

2017-11-01

NMR and X-ray crystallography are the two most widely used methods for determining protein structures. Our previous study examining NMR versus X-Ray sources of protein conformations showed improved performance with NMR structures when used in our Multiple Protein Structures (MPS) method for receptor-based pharmacophores (Damm, Carlson, J Am Chem Soc 129:8225-8235, 2007). However, that work was based on a single test case, HIV-1 protease, because of the rich data available for that system. New data for more systems are available now, which calls for further examination of the effect of different sources of protein conformations. The MPS technique was applied to Growth factor receptor bound protein 2 (Grb2), Src SH2 homology domain (Src-SH2), FK506-binding protein 1A (FKBP12), and Peroxisome proliferator-activated receptor-γ (PPAR-γ). Pharmacophore models from both crystal and NMR ensembles were able to discriminate between high-affinity, low-affinity, and decoy molecules. As we found in our original study, NMR models showed optimal performance when all elements were used. The crystal models had more pharmacophore elements compared to their NMR counterparts. The crystal-based models exhibited optimum performance only when pharmacophore elements were dropped. This supports our assertion that the higher flexibility in NMR ensembles helps focus the models on the most essential interactions with the protein. Our studies suggest that the "extra" pharmacophore elements seen at the periphery in X-ray models arise as a result of decreased protein flexibility and make very little contribution to model performance.

An introduction to biological NMR spectroscopy

International Nuclear Information System (INIS)

Marion, Dominique

2013-01-01

NMR spectroscopy is a powerful tool for biologists interested in the structure, dynamics, and interactions of biological macromolecules. This review aims at presenting in an accessible manner the requirements and limitations of this technique. As an introduction, the history of NMR will highlight how the method evolved from physics to chemistry and finally to biology over several decades. We then introduce the NMR spectral parameters used in structural biology, namely the chemical shift, the J-coupling, nuclear Overhauser effects, and residual dipolar couplings. Resonance assignment, the required step for any further NMR study, bears a resemblance to jigsaw puzzle strategy. The NMR spectral parameters are then converted into angle and distances and used as input using restrained molecular dynamics to compute a bundle of structures. When interpreting a NMR-derived structure, the biologist has to judge its quality on the basis of the statistics provided. When the 3D structure is a priori known by other means, the molecular interaction with a partner can be mapped by NMR: information on the binding interface as well as on kinetic and thermodynamic constants can be gathered. NMR is suitable to monitor, over a wide range of frequencies, protein fluctuations that play a crucial role in their biological function. In the last section of this review, intrinsically disordered proteins, which have escaped the attention of classical structural biology, are discussed in the perspective of NMR, one of the rare available techniques able to describe structural ensembles. This Tutorial is part of the International Proteomics Tutorial Programme (IPTP 16 MCP). (authors)

Dynamic NMR Study of Model CMP Slurry Containing Silica Particles as Abrasives

Science.gov (United States)

Odeh, F.; Al-Bawab, A.; Li, Y.

2018-02-01

Chemical mechanical planarization (CMP) should provide a good surface planarity with minimal surface defectivity. Since CMP slurries are multi-component systems, it is very important to understand the various processes and interactions taking place in such slurries. Several techniques have been employed for such task, however, most of them lack the molecular recognition to investigate molecular interactions without adding probes which in turn increase complexity and might alter the microenvironment of the slurry. Nuclear magnetic resonance (NMR) is a powerful technique that can be employed in such study. The longitudinal relaxation times (T1) of the different components of CMP slurries were measured using Spin Echo-NMR (SE-NMR) at a constant temperature. The fact that NMR is non-invasive and gives information on the molecular level gives more advantage to the technique. The model CMP slurry was prepared in D2O to enable monitoring of T1 for the various components' protons. SE-NMR provide a very powerful tool to study the various interactions and adsorption processes that take place in a model CMP silica based slurry which contains BTA and/or glycine and/or Cu+2 ions. It was found that BTA is very competitive towards complexation with Cu+2 ions and BTA-Cu complex adsorbs on silica surface.

NMR characterization of weak interactions between RhoGDI2 and fragment screening hits.

Science.gov (United States)

Liu, Jiuyang; Gao, Jia; Li, Fudong; Ma, Rongsheng; Wei, Qingtao; Wang, Aidong; Wu, Jihui; Ruan, Ke

2017-01-01

The delineation of intrinsically weak interactions between novel targets and fragment screening hits has long limited the pace of hit-to-lead evolution. Rho guanine-nucleotide dissociation inhibitor 2 (RhoGDI2) is a novel target that lacks any chemical probes for the treatment of tumor metastasis. Protein-observed and ligand-observed NMR spectroscopy was used to characterize the weak interactions between RhoGDI2 and fragment screening hits. We identified three hits of RhoGDI2 using streamlined NMR fragment-based screening. The binding site residues were assigned using non-uniformly sampled C α - and H α -based three dimensional NMR spectra. The molecular docking to the proposed geranylgeranyl binding pocket of RhoGDI2 was guided by NMR restraints of chemical shift perturbations and ligand-observed transferred paramagnetic relaxation enhancement. We further validated the weak RhoGDI2-hit interactions using mutagenesis and structure-affinity analysis. Weak interactions between RhoGDI2 and fragment screening hits were delineated using an integrated NMR approach. Binders to RhoGDI2 as a potential anti-cancer target have been first reported, and their weak interactions were depicted using NMR spectroscopy. Our work highlights the powerfulness and the versatility of the integrative NMR techniques to provide valuable structural insight into the intrinsically weak interactions between RhoGDI2 and the fragment screening hits, which could hardly be conceived using other biochemical techniques. Copyright © 2016 Elsevier B.V. All rights reserved.

Towards automatic metabolomic profiling of high-resolution one-dimensional proton NMR spectra

International Nuclear Information System (INIS)

Mercier, Pascal; Lewis, Michael J.; Chang, David; Baker, David; Wishart, David S.

2011-01-01

Nuclear magnetic resonance (NMR) and Mass Spectroscopy (MS) are the two most common spectroscopic analytical techniques employed in metabolomics. The large spectral datasets generated by NMR and MS are often analyzed using data reduction techniques like Principal Component Analysis (PCA). Although rapid, these methods are susceptible to solvent and matrix effects, high rates of false positives, lack of reproducibility and limited data transferability from one platform to the next. Given these limitations, a growing trend in both NMR and MS-based metabolomics is towards targeted profiling or “quantitative” metabolomics, wherein compounds are identified and quantified via spectral fitting prior to any statistical analysis. Despite the obvious advantages of this method, targeted profiling is hindered by the time required to perform manual or computer-assisted spectral fitting. In an effort to increase data analysis throughput for NMR-based metabolomics, we have developed an automatic method for identifying and quantifying metabolites in one-dimensional (1D) proton NMR spectra. This new algorithm is capable of using carefully constructed reference spectra and optimizing thousands of variables to reconstruct experimental NMR spectra of biofluids using rules and concepts derived from physical chemistry and NMR theory. The automated profiling program has been tested against spectra of synthetic mixtures as well as biological spectra of urine, serum and cerebral spinal fluid (CSF). Our results indicate that the algorithm can correctly identify compounds with high fidelity in each biofluid sample (except for urine). Furthermore, the metabolite concentrations exhibit a very high correlation with both simulated and manually-detected values.

Towards automatic metabolomic profiling of high-resolution one-dimensional proton NMR spectra

Energy Technology Data Exchange (ETDEWEB)

Mercier, Pascal; Lewis, Michael J.; Chang, David, E-mail: dchang@chenomx.com [Chenomx Inc (Canada); Baker, David [Pfizer Inc (United States); Wishart, David S. [University of Alberta, Department of Computing Science and Biological Sciences (Canada)

2011-04-15

Nuclear magnetic resonance (NMR) and Mass Spectroscopy (MS) are the two most common spectroscopic analytical techniques employed in metabolomics. The large spectral datasets generated by NMR and MS are often analyzed using data reduction techniques like Principal Component Analysis (PCA). Although rapid, these methods are susceptible to solvent and matrix effects, high rates of false positives, lack of reproducibility and limited data transferability from one platform to the next. Given these limitations, a growing trend in both NMR and MS-based metabolomics is towards targeted profiling or 'quantitative' metabolomics, wherein compounds are identified and quantified via spectral fitting prior to any statistical analysis. Despite the obvious advantages of this method, targeted profiling is hindered by the time required to perform manual or computer-assisted spectral fitting. In an effort to increase data analysis throughput for NMR-based metabolomics, we have developed an automatic method for identifying and quantifying metabolites in one-dimensional (1D) proton NMR spectra. This new algorithm is capable of using carefully constructed reference spectra and optimizing thousands of variables to reconstruct experimental NMR spectra of biofluids using rules and concepts derived from physical chemistry and NMR theory. The automated profiling program has been tested against spectra of synthetic mixtures as well as biological spectra of urine, serum and cerebral spinal fluid (CSF). Our results indicate that the algorithm can correctly identify compounds with high fidelity in each biofluid sample (except for urine). Furthermore, the metabolite concentrations exhibit a very high correlation with both simulated and manually-detected values.

Quantification of aluminium-27 NMR spectra of high-surface-area oxides

International Nuclear Information System (INIS)

Pearson, R.M.; Schramm, C.M.

1990-01-01

This paper discusses the quantitation of 27 Al NMR spectra. It is showns that the so called 'invisible' aluminium atoms seen by recent workers are completely consistent with known continuous wave NMR studies of the 27 Al NMR spectra of high surface area aluminium oxides. The use of pulsed NMR techniques further complicate the quantitative measurement of 27 Al NMR spectra, especially when high resolution NMR spectrometers are used for this purpose. Methods are described which allow both the estimation of aluminium not seen by continuous wave techniques and the amounts of the NMR spectra lost in pulsed work. (author). 24 refs.; 6 figs.; 1 tab

Paramagnetic NMR investigation of dendrimer-based host-guest interactions.

Directory of Open Access Journals (Sweden)

Fei Wang

Full Text Available In this study, the host-guest behavior of poly(amidoamine (PAMAM dendrimers bearing amine, hydroxyl, or carboxylate surface functionalities were investigated by paramagnetic NMR studies. 2,2,6,6-Tetramethylpiperidinyloxy (TEMPO derivatives were used as paramagnetic guest molecules. The results showed that TEMPO-COOH significantly broaden the ¹H NMR peaks of amine- and hydroxyl-terminated PAMAM dendrimers. In comparison, no paramagnetic relaxation enhancement (PRE was observed between TEMPO-NH₂, TEMPO-OH and the three types of PAMAM dendrimers. The PRE phenomenon observed is correlated with the encapsulation of TEMPO-COOH within dendrimer pockets. Protonation of the tertiary amine groups within PAMAM dendrimers plays an important role during this process. Interestingly, the absence of TEMPO-COOH encapsulation within carboxylate-terminated PAMAM dendrimer is observed due to the repulsion of TEMPO-COO- anion and anionic dendrimer surface. The combination of paramagnetic probes and ¹H NMR linewidth analysis can be used as a powerful tool in the analysis of dendrimer-based host-guest systems.

Simultaneous acquisition of three NMR spectra in a single ...

Indian Academy of Sciences (India)

Simultaneous acquisition of three NMR spectra in a single experiment ... set, which is based on a combination of different fast data acquisition techniques such as G-matrix ..... The sign and intensity of the CHn resonance depends on the delay.

Citrus Quality Control: An NMR/MRI Problem-Based Experiment

Science.gov (United States)

Erhart, Sarah E.; McCarrick, Robert M.; Lorigan, Gary A.; Yezierski, Ellen J.

2016-01-01

An experiment seated in an industrial context can provide an engaging framework and unique learning opportunity for an upper-division physical chemistry laboratory. An experiment that teaches NMR/MRI through a problem-based quality control of citrus products was developed. In this experiment, using a problem-based learning (PBL) approach, students…

Advances in estimation methods of vegetation water content based on optical remote sensing techniques

Institute of Scientific and Technical Information of China (English)

无

2010-01-01

Quantitative estimation of vegetation water content(VWC) using optical remote sensing techniques is helpful in forest fire as-sessment,agricultural drought monitoring and crop yield estimation.This paper reviews the research advances of VWC retrieval using spectral reflectance,spectral water index and radiative transfer model(RTM) methods.It also evaluates the reli-ability of VWC estimation using spectral water index from the observation data and the RTM.Focusing on two main definitions of VWC-the fuel moisture content(FMC) and the equivalent water thickness(EWT),the retrieval accuracies of FMC and EWT using vegetation water indices are analyzed.Moreover,the measured information and the dataset are used to estimate VWC,the results show there are significant correlations among three kinds of vegetation water indices(i.e.,WSI,NDⅡ,NDWI1640,WI/NDVI) and canopy FMC of winter wheat(n=45).Finally,the future development directions of VWC detection based on optical remote sensing techniques are also summarized.

Muscular pathology: echographic and NMR imaging aspects

International Nuclear Information System (INIS)

Pascal-Suisse, P.; Beaurain, P.; Mougniot, C.

1995-01-01

A comparison of echographic techniques and NMR imaging has been done for the diagnosis of muscular trauma and tumor pathologies. In traumatic pathology, the echographic analysis allows to determine the complete assessment of recent muscular injuries. NMR imaging can be used in granuloma or fibrous callosity appreciation and for the analysis of deep injury (muscles and muscles-tendon junctions) and of muscular aponeurosis. Echography must be used together with color coding Doppler technique in the diagnosis of tumor pathology and for the study of slow fluxes. The recently available energy Doppler technique seems to be powerful in the study of vascularization of small expansive formations, but their extension to adjacent bone or tissue can only be appreciated using NMR imaging. (J.S.)

Oriented solid-state NMR spectrosocpy

DEFF Research Database (Denmark)

Bertelsen, Kresten

This thesis is concerned with driving forward oriented solid-state NMR spectroscopy as a viable technique for studying peptides in membrane bilayers. I will show that structural heterogeneity is an intrinsic part of the peptide/lipid system and that NMR can be used to characterize static...... and dynamic structural features of the peptides and its local surroundings. In fact one need to take into account the dynamical features of the system in order to correctly predict the structure from oriented solid-state NMR spectra.      ...

Fluid-Rock Characterization and Interactions in NMR Well Logging

Energy Technology Data Exchange (ETDEWEB)

Hirasaki, George J.; Mohanty, Kishore K.

2003-02-10

The objective of this project was to characterize the fluid properties and fluid-rock interactions that are needed for formation evaluation by NMR well logging. The advances made in the understanding of NMR fluid properties are summarized in a chapter written for an AAPG book on NMR well logging. This includes live oils, viscous oils, natural gas mixtures, and the relation between relaxation time and diffusivity.

NMR in pulsed magnetic field

KAUST Repository

Abou-Hamad, Edy; Bontemps, P.; Rikken, Geert L J A

2011-01-01

Nuclear magnetic resonance (NMR) experiments in pulsed magnetic fields up to 30.4 T focused on 1H and 93Nb nuclei are reported. Here we discuss the advantage and limitation of pulsed field NMR and why this technique is able to become a promising research tool. © 2011 Elsevier Inc. All Rights Reserved.

NMR in pulsed magnetic field

KAUST Repository

Abou-Hamad, Edy

2011-09-01

Nuclear magnetic resonance (NMR) experiments in pulsed magnetic fields up to 30.4 T focused on 1H and 93Nb nuclei are reported. Here we discuss the advantage and limitation of pulsed field NMR and why this technique is able to become a promising research tool. © 2011 Elsevier Inc. All Rights Reserved.

NMRbox: A Resource for Biomolecular NMR Computation.

Science.gov (United States)

Maciejewski, Mark W; Schuyler, Adam D; Gryk, Michael R; Moraru, Ion I; Romero, Pedro R; Ulrich, Eldon L; Eghbalnia, Hamid R; Livny, Miron; Delaglio, Frank; Hoch, Jeffrey C

2017-04-25

Advances in computation have been enabling many recent advances in biomolecular applications of NMR. Due to the wide diversity of applications of NMR, the number and variety of software packages for processing and analyzing NMR data is quite large, with labs relying on dozens, if not hundreds of software packages. Discovery, acquisition, installation, and maintenance of all these packages is a burdensome task. Because the majority of software packages originate in academic labs, persistence of the software is compromised when developers graduate, funding ceases, or investigators turn to other projects. To simplify access to and use of biomolecular NMR software, foster persistence, and enhance reproducibility of computational workflows, we have developed NMRbox, a shared resource for NMR software and computation. NMRbox employs virtualization to provide a comprehensive software environment preconfigured with hundreds of software packages, available as a downloadable virtual machine or as a Platform-as-a-Service supported by a dedicated compute cloud. Ongoing development includes a metadata harvester to regularize, annotate, and preserve workflows and facilitate and enhance data depositions to BioMagResBank, and tools for Bayesian inference to enhance the robustness and extensibility of computational analyses. In addition to facilitating use and preservation of the rich and dynamic software environment for biomolecular NMR, NMRbox fosters the development and deployment of a new class of metasoftware packages. NMRbox is freely available to not-for-profit users. Copyright © 2017 Biophysical Society. All rights reserved.

Carbon-13 NMR spectroscopy of biological systems

CERN Document Server

Beckmann, Nicolau

1995-01-01

This book is intended to provide an in-depth understanding of 13C NMR as a tool in biological research. 13C NMR has provided unique information concerning complex biological systems, from proteins and nucleic acids to animals and humans. The subjects addressed include multidimensional heteronuclear techniques for structural studies of molecules in the liquid and solid states, the investigation of interactions in model membranes, the elucidation of metabolic pathwaysin vitro and in vivo on animals, and noninvasive metabolic studies performed on humans. The book is a unique mix of NMR methods and biological applications which makes it a convenient reference for those interested in research in this interdisciplinary area of physics, chemistry, biology, and medicine.Key Features* An interdisciplinary text with emphasis on both 13C NMR methodology and the relevant biological and biomedical issues* State-of-the-art 13C NMR techniques are described; Whenever possible, their advantages over other approaches are empha...

MetAssimulo:Simulation of Realistic NMR Metabolic Profiles

Directory of Open Access Journals (Sweden)

De Iorio Maria

2010-10-01

Full Text Available Abstract Background Probing the complex fusion of genetic and environmental interactions, metabolic profiling (or metabolomics/metabonomics, the study of small molecules involved in metabolic reactions, is a rapidly expanding 'omics' field. A major technique for capturing metabolite data is 1H-NMR spectroscopy and this yields highly complex profiles that require sophisticated statistical analysis methods. However, experimental data is difficult to control and expensive to obtain. Thus data simulation is a productive route to aid algorithm development. Results MetAssimulo is a MATLAB-based package that has been developed to simulate 1H-NMR spectra of complex mixtures such as metabolic profiles. Drawing data from a metabolite standard spectral database in conjunction with concentration information input by the user or constructed automatically from the Human Metabolome Database, MetAssimulo is able to create realistic metabolic profiles containing large numbers of metabolites with a range of user-defined properties. Current features include the simulation of two groups ('case' and 'control' specified by means and standard deviations of concentrations for each metabolite. The software enables addition of spectral noise with a realistic autocorrelation structure at user controllable levels. A crucial feature of the algorithm is its ability to simulate both intra- and inter-metabolite correlations, the analysis of which is fundamental to many techniques in the field. Further, MetAssimulo is able to simulate shifts in NMR peak positions that result from matrix effects such as pH differences which are often observed in metabolic NMR spectra and pose serious challenges for statistical algorithms. Conclusions No other software is currently able to simulate NMR metabolic profiles with such complexity and flexibility. This paper describes the algorithm behind MetAssimulo and demonstrates how it can be used to simulate realistic NMR metabolic profiles with

Investigation of zeolites by solid state quadrapole NMR

International Nuclear Information System (INIS)

Janssen, R.

1990-01-01

The subject of this thesis is the NMR investigation of zeolites. The nature and properties of zeolites are discussed. Some of the basic priniples of NMR techniques on quadrupole nuclei are presented. A special technique, namely a two-dimensional nutation experiment is discussed in detail. The theory of the nutation experiment for quadrupole spin species with spin quantum number 3/2 as well as 5/2 is presented. For both spin spcies the theoretical spectra are compared with experimental results. It is also shown that the nutation expeirment can be performed with several pulse schemes. It is shown how phase-sensitive pure-absorption nutation spectra can be obtained and an NMR-probe is presented that is capable of performing NMR experiments at high (up to 500 degree C) temperatures. The two-dimensional nutation NMR technique has been applied to sodium cations in zeolite NaA. For this purpose a numbre of zeolite samples were prepared that contained different amounts of water. With the aid of nutation NMR the hydration of the zeolite can be studied and conclusions can be drawn about the symmetry of the surrounding of the sodium cations. With the aid of an extension of the nutation NMR experiment: Rotary Echo Nutation NMR, it is shown that in zeolite NaA, in various stages of hydration, the sodium cations or water molecules are mobile. Proof is given by means of high-temperature 23 Na-NMR that dehydrates zeolite NaA undergoes a phase transition at ca. 120 degree C. In a high-temperature NMR investigation of zeolite ZSM-5 it is shown that the sodium ions start to execute motions when the temperature is increased. (author). 198 refs.; 72 figs.; 6 tabs

Recommendations of the wwPDB NMR Validation Task Force

Science.gov (United States)

Montelione, Gaetano T.; Nilges, Michael; Bax, Ad; Güntert, Peter; Herrmann, Torsten; Richardson, Jane S.; Schwieters, Charles; Vranken, Wim F.; Vuister, Geerten W.; Wishart, David S.; Berman, Helen M.; Kleywegt, Gerard J.; Markley, John L.

2013-01-01

As methods for analysis of biomolecular structure and dynamics using nuclear magnetic resonance spectroscopy (NMR) continue to advance, the resulting 3D structures, chemical shifts, and other NMR data are broadly impacting biology, chemistry, and medicine. Structure model assessment is a critical area of NMR methods development, and is an essential component of the process of making these structures accessible and useful to the wider scientific community. For these reasons, the Worldwide Protein Data Bank (wwPDB) has convened an NMR Validation Task Force (NMR-VTF) to work with the wwPDB partners in developing metrics and policies for biomolecular NMR data harvesting, structure representation, and structure quality assessment. This paper summarizes the recommendations of the NMR-VTF, and lays the groundwork for future work in developing standards and metrics for biomolecular NMR structure quality assessment. PMID:24010715

Two-dimensional NMR spectrometry

International Nuclear Information System (INIS)

Farrar, T.C.

1987-01-01

This article is the second in a two-part series. In part one (ANALYTICAL CHEMISTRY, May 15) the authors discussed one-dimensional nuclear magnetic resonance (NMR) spectra and some relatively advanced nuclear spin gymnastics experiments that provide a capability for selective sensitivity enhancements. In this article and overview and some applications of two-dimensional NMR experiments are presented. These powerful experiments are important complements to the one-dimensional experiments. As in the more sophisticated one-dimensional experiments, the two-dimensional experiments involve three distinct time periods: a preparation period, t 0 ; an evolution period, t 1 ; and a detection period, t 2

NMR studies of multiphase flows II

Energy Technology Data Exchange (ETDEWEB)

Altobelli, S.A.; Caprihan, A.; Fukushima, E. [Lovelace Institutes, Albuquerque, NM (United States)] [and others

1995-12-31

NMR techniques for measurements of spatial distribution of material phase, velocity and velocity fluctuation are being developed and refined. Versions of these techniques which provide time average liquid fraction and fluid phase velocity have been applied to several concentrated suspension systems which will not be discussed extensively here. Technical developments required to further extend the use of NMR to the multi-phase flow arena and to provide measurements of previously unobtainable parameters are the focus of this report.

NMR spectrometers as "magnetic tongues": prediction of sensory descriptors in canned tomatoes

DEFF Research Database (Denmark)

Malmendal, Anders; Amoresano, Claudia; Trotta, Roberta

2011-01-01

The perception of odor and flavor of food is a complicated physiological and psychological process that cannot be explained by simple models. Quantitative descriptive analysis is a technique used to describe sensory features. Nevertheless, the availability of a number of instrumental techniques has...... opened up the possibility to calibrate the sensory perception. In this frame, we have tested the potentiality of nuclear magnetic resonance spectroscopy as a predictive tool to measure sensory descriptors. In particular, we have used an NMR metabolomic approach that allowed us to differentiate...... the analyzed samples based on their chemical composition. We were able to correlate the NMR metabolomic fingerprints recorded for canned tomato samples to the sensory descriptors bitterness, sweetness, sourness, saltiness, tomato and metal taste, redness, and density, suggesting that NMR might be a very useful...

A novel alkaloid isolated from Crotalaria paulina and identified by NMR and DFT calculations

Science.gov (United States)

Oliveira, Ramon Prata; Demuner, Antonio Jacinto; Alvarenga, Elson Santiago; Barbosa, Luiz Claudio Almeida; de Melo Silva, Thiago

2018-01-01

Pyrrolizidine alkaloids (PAs) are secondary metabolites found in Crotalaria genus and are known to have several biological activities. A novel macrocycle bislactone alkaloid, coined ethylcrotaline, was isolated and purified from the aerial parts of Crotalaria paulina. The novel macrocycle was identified with the aid of high resolution mass spectrometry and advanced nuclear magnetic resonance techniques. The relative stereochemistry of the alkaloid was defined by comparing the calculated quantum mechanical hydrogen and carbon chemical shifts of eight candidate structures with the experimental NMR data. The best fit between the eight candidate structures and the experimental NMR chemical shifts was defined by the DP4 statistical analyses and the Mean Absolute Error (MAE) calculations.

Recombinant Kinase Production and Fragment Screening by NMR Spectroscopy.

Science.gov (United States)

Han, Byeonggu; Ahn, Hee-Chul

2016-01-01

During the past decade fragment-based drug discovery (FBDD) has rapidly evolved and several drugs or drug candidates developed by FBDD approach are clinically in use or in clinical trials. For example, vemurafenib, a V600E mutated BRAF inhibitor, was developed by utilizing FBDD approach and approved by FDA in 2011. In FBDD, screening of fragments is the starting step for identification of hits and lead generation. Fragment screening usually relies on biophysical techniques by which the protein-bound small molecules can be detected. NMR spectroscopy has been extensively used to study the molecular interaction between the protein and the ligand, and has many advantages in fragment screening over other biophysical techniques. This chapter describes the practical aspects of fragment screening by saturation transfer difference NMR.

Advanced electron beam techniques

International Nuclear Information System (INIS)

Hirotsu, Yoshihiko; Yoshida, Yoichi

2007-01-01

After 100 years from the time of discovery of electron, we now have many applications of electron beam in science and technology. In this report, we review two important applications of electron beam: electron microscopy and pulsed-electron beam. Advanced electron microscopy techniques to investigate atomic and electronic structures, and pulsed-electron beam for investigating time-resolved structural change are described. (author)

High resolution NMR spectroscopy of synthetic polymers in bulk

International Nuclear Information System (INIS)

Komorski, R.A.

1986-01-01

The contents of this book are: Overview of high-resolution NMR of solid polymers; High-resolution NMR of glassy amorphous polymers; Carbon-13 solid-state NMR of semicrystalline polymers; Conformational analysis of polymers of solid-state NMR; High-resolution NMR studies of oriented polymers; High-resolution solid-state NMR of protons in polymers; and Deuterium NMR of solid polymers. This work brings together the various approaches for high-resolution NMR studies of bulk polymers into one volume. Heavy emphasis is, of course, given to 13C NMR studies both above and below Tg. Standard high-power pulse and wide-line techniques are not covered

Advanced single-wafer sequential multiprocessing techniques for semiconductor device fabrication

International Nuclear Information System (INIS)

Moslehi, M.M.; Davis, C.

1989-01-01

Single-wafer integrated in-situ multiprocessing (SWIM) is recognized as the future trend for advanced microelectronics production in flexible fast turn- around computer-integrated semiconductor manufacturing environments. The SWIM equipment technology and processing methodology offer enhanced equipment utilization, improved process reproducibility and yield, and reduced chip manufacturing cost. They also provide significant capabilities for fabrication of new and improved device structures. This paper describes the SWIM techniques and presents a novel single-wafer advanced vacuum multiprocessing technology developed based on the use of multiple process energy/activation sources (lamp heating and remote microwave plasma) for multilayer epitaxial and polycrystalline semiconductor as well as dielectric film processing. Based on this technology, multilayer in-situ-doped homoepitaxial silicon and heteroepitaxial strained layer Si/Ge x Si 1 - x /Si structures have been grown and characterized. The process control and the ultimate interfacial abruptness of the layer-to-layer transition widths in the device structures prepared by this technology will challenge the MBE techniques in multilayer epitaxial growth applications

Advanced Inspection and Repair Welding Techniques for SCC Countermeasures

International Nuclear Information System (INIS)

Takagi, T.; Nishimoto, K.; Uchimoto, T.

2012-01-01

Feasibility studies of advanced inspection and repair welding techniques were conducted in the framework of the Nuclear and Industry Safety Agency of Japan (NISA) project on the enhancement of ageing management and maintenance of NPPs. In this paper, features of NDE methods investigated in the projects, main results of research activities and prospect of nickel based alloy weld inspection are discussed. We also make a review for the integrity and reliability evaluation techniques for repair welding of ageing plants which were intensively investigated in view of regulatory criteria, in NISA project. (author)

Time domain NMR evaluation of poly(vinyl alcohol) xerogels

Energy Technology Data Exchange (ETDEWEB)

Rodrigues, Elton Jorge da Rocha; Cavalcante, Maxwell de Paula; Tavares, Maria Ines Bruno, E-mail: mibt@ima.ufrj.br [Universidade Federal do Rio de Janeiro (IMA/UFRJ), Rio de Janeiro, RJ (Brazil). Centro de Tecnologia. Instituto de Macromoleculas Professora Eloisa Mano

2016-05-15

Poly(vinyl alcohol) (PVA)-based chemically cross-linked xerogels, both neat and loaded with nanoparticulate hydrophilic silica (SiO{sub 2}), were obtained and characterized mainly through time domain NMR experiments (TD-NMR). Fourier-transform infrared (FT-IR) and wide angle X-ray diffraction (WAXD) analyses were employed as secondary methods. TD-NMR, through the interpretation of the spin-lattice relaxation constant values and related information, showed both cross-linking and nanoparticle influences on PVA matrix. SiO{sub 2} does not interact chemically with the PVA chains, but has effect on its molecular mobility, as investigated via TD-NMR. Apparent energy of activation, spin-lattice time constant and size of spin domains in the sample have almost linear dependence with the degree of cross-linking of the PVA and are affected by the addition of SiO{sub 2}. These three parameters were derived from a single set of TD-NMR experiments, which demonstrates the versatility of the technique for characterization of inorganic-organic hybrid xerogels, an important class of materials. (author)

Study of kinetics of 2,3-diphosphoglycerate degradation by 31P-NMR technique in depleted human erythrocytes

International Nuclear Information System (INIS)

Ataullakhanov, F.I.; Vitvitskii, V.M.; Dubinskaya, E.I.; Dubinskii, V.Z.

1986-01-01

The kinetics of 2,3-diphosphoglycerate degradation in depleted human erythrocytes was studied by the high-resolution 31 P-NMR technique. A plateau was found on the kinetic curve in the first 1.5-2 h after the beginning of depletion. The mechanisms that may be responsible for the existence of such a plateau are discussed

NMR imaging studies of coal

Energy Technology Data Exchange (ETDEWEB)

Ma, Z.R.; Zhang, P.Z.; Ding, G.L.; Li, L.Y.; Ye, C.H. [University of Science and Technology, Beijing (China). Dept. of Chemistry

1996-06-01

The permeation transportation and swelling behavior of solvents into coal are investigated by NMR imaging using pyridine-d{sub 5} and acetone-d{sub 6}. Images of coal swollen with deuterated solvents illuminate proton distributions of mobile phases within the coal macromolecular networks. More information about the chemical and physical structure of coal can be obtained using NMR imaging techniques.

Structural investigations of substituted indolizine derivatives by NMR studies

International Nuclear Information System (INIS)

Furdui, Bianca; Dinica, Rodica; Demeunynck, Martine; Druta, Ioan

2008-01-01

Owing to the increasing importance of indolizine heterocycles in the field of biology and pharmacology we have synthesized and investigated the obtained heterocycles by NMR techniques. In order to investigate the substituent effects on the spectroscopic properties, a series of indolizine derivatives were studied by 1 H-NMR, 13 C-NMR and 2D NMR (GCOSY, GHMBC and GHMQC spectra). (authors)

Toxicological effects of cinnabar in rats by NMR-based metabolic profiling of urine and serum

International Nuclear Information System (INIS)

Wei Lai; Liao Peiqiu; Wu Huifeng; Li Xiaojing; Pei Fengkui; Li Weisheng; Wu Yijie

2008-01-01

Cinnabar, an important traditional Chinese mineral medicine, has been widely used as a Chinese patent medicine ingredient for sedative therapy. However, the pharmaceutical and toxicological effects of cinnabar, especially in the whole organism, were subjected to few investigations. In this study, an NMR-based metabolomics approach has been applied to investigate the toxicological effects of cinnabar after intragastrical administration (dosed at 0.5, 2 and 5 g/kg body weight) on male Wistar rats. Liver and kidney histopathology examinations and serum clinical chemistry analyses were also performed. The 1 H NMR spectra were analyzed using multivariate pattern recognition techniques to show the time- and dose-dependent biochemical variations induced by cinnabar. The metabolic signature of urinalysis from cinnabar-treated animals exhibited an increase in the levels of creatinine, acetate, acetoacetate, taurine, hippurate and phenylacetylglycine, together with a decrease in the levels of trimethyl-N-oxide, dimethylglycine and Kreb's cycle intermediates (citrate, 2-oxoglutarate and succinate). The metabolomics analyses of serum showed elevated concentrations of ketone bodies (3-D-hydroxybutyrate and acetoacetate), branched-chain amino acids (valine, leucine and isoleucine), choline and creatine as well as decreased glucose, lipids and lipoproteins from cinnabar-treated animals. These findings indicated cinnabar induced disturbance in energy metabolism, amino acid metabolism and gut microflora environment as well as slight injury in liver and kidney, which might indirectly result from cinnabar induced oxidative stress. This work illustrated the high reliability of NMR-based metabolomic approach on the study of the biochemical effects induced by traditional Chinese medicine

Lactose Binding Induces Opposing Dynamics Changes in Human Galectins Revealed by NMR-Based Hydrogen-Deuterium Exchange.

Science.gov (United States)

Chien, Chih-Ta Henry; Ho, Meng-Ru; Lin, Chung-Hung; Hsu, Shang-Te Danny

2017-08-16

Galectins are β-galactoside-binding proteins implicated in a myriad of biological functions. Despite their highly conserved carbohydrate binding motifs with essentially identical structures, their affinities for lactose, a common galectin inhibitor, vary significantly. Here, we aimed to examine the molecular basis of differential lactose affinities amongst galectins using solution-based techniques. Consistent dissociation constants of lactose binding were derived from nuclear magnetic resonance (NMR) spectroscopy, intrinsic tryptophan fluorescence, isothermal titration calorimetry and bio-layer interferometry for human galectin-1 (hGal1), galectin-7 (hGal7), and the N-terminal and C-terminal domains of galectin-8 (hGal8 NTD and hGal8 CTD , respectively). Furthermore, the dissociation rates of lactose binding were extracted from NMR lineshape analyses. Structural mapping of chemical shift perturbations revealed long-range perturbations upon lactose binding for hGal1 and hGal8 NTD . We further demonstrated using the NMR-based hydrogen-deuterium exchange (HDX) that lactose binding increases the exchange rates of residues located on the opposite side of the ligand-binding pocket for hGal1 and hGal8 NTD , indicative of allostery. Additionally, lactose binding induces significant stabilisation of hGal8 CTD across the entire domain. Our results suggested that lactose binding reduced the internal dynamics of hGal8 CTD on a very slow timescale (minutes and slower) at the expense of reduced binding affinity due to the unfavourable loss of conformational entropy.

Recent topics in NMR imaging and MRI

International Nuclear Information System (INIS)

Watanabe, Tokuko

2002-01-01

NMR and NMR imaging (MRI) are finding increasing use not only in the clinical and medical fields, but also in material, physicochemical, biological, geological, industrial and environmental applications. This short review is limited to two topics: new techniques and pulse sequences and their application to non-clinical fields that may have clinical application; and new trends in MR contrast agents. The former topic addresses pulse sequence and data analysis; dynamics such as diffusion, flow, velocity and velocimetry; chemometrics; pharmacological agents; and chemotherapy; the latter topic addresses contrast agents (CA) sensitive to biochemical activity; CA based on water exchange; molecular interactions and stability of CA; characteristics of emerging CA; superparamagnetic CA; and macromolecular CA. (author)

Polymeric proanthocyanidins 13C NMR studies of procyanidins

Science.gov (United States)

Lawrence J. Porter; Roger H. Newman; Lai Yeap Foo; Herbert Wong; Richard W. Hemingway

1982-01-01

Proanthocyanidin polymers have been shown to consist entirely of flavan-3-ol units by a combination of techniques including 13C n.m.r. spectroscopy. The 13C n.m.r. spectra of the polymers and related molecules are now considered in more detail. Prior to this study UC n.m.r. data has been published of procyanidins and...

Performance of the WeNMR CS-Rosetta3 web server in CASD-NMR

NARCIS (Netherlands)

Van Der Schot, Gijs; Bonvin, Alexandre M J J

We present here the performance of the WeNMR CS-Rosetta3 web server in CASD-NMR, the critical assessment of automated structure determination by NMR. The CS-Rosetta server uses only chemical shifts for structure prediction, in combination, when available, with a post-scoring procedure based on

Frontier of Advanced Accelerator Applications and Medical Treatments Using Nuclear Techniques. Abstract

International Nuclear Information System (INIS)

2015-01-01

To address the challenges of research-based practice, developing advanced accelerator applications, and medical treatments using nuclear tecniqoes, researchers from Rajamakala University of Technology Lanna, Office of Atoms for Peace, and Chiang Mai University have joined in hosting this conference. Nuclear medicine, amedical specialty, diagnoses and treats diseases in a safe and painless way. Nuclear techniques can determine medical information that may otherwise be unavailable, require surgery, or necessitate more expensive and invasive diagnostic tests. Advance in nuclear techniques also offer the potential to detect abnormalities at earlier stages, leasding to earlier treatment and a more successful prognosis.

Nuclear magnetic resonance (NMR) tomography

International Nuclear Information System (INIS)

Skalpe, I.O.

1984-01-01

A brief survey of the working principle of the NMR technique in diagnostical medicine is given. Its clinical usefulness for locating tumors, diagnosing various other diseases, such as some mental illnesses and multiple sclerosis, and its possibilities for studying biochemical processes in vivo are mentioned. The price of NMR image scanners and the problems of the strong magnetic field around the machines are mentioned

Chemical vs. electrochemical extraction of lithium from the Li-excess Li(1.10)Mn(1.90)O4 spinel followed by NMR and DRX techniques.

Science.gov (United States)

Martinez, S; Sobrados, I; Tonti, D; Amarilla, J M; Sanz, J

2014-02-21

Lithium extraction from the Li-excess Li1.10Mn1.90O4 spinel has been performed by chemical and electrochemical methods in aqueous and in organic media, respectively. De-lithiated samples have been investigated by XRD, SEM, TG, (7)Li and (1)H MAS-NMR techniques. The comparative study has allowed demonstrating that the intermediate de-intercalated samples prepared during the chemical extraction by acid titration are similar to those prepared by the electrochemical way in a non-aqueous electrolyte. LiMn2O4 based spinel with a tailored de-lithiation degree can be prepared as a single phase by controlling the pH used in chemical extraction. (7)Li MAS-NMR spectroscopy has been used to follow the influence of the manganese oxidation state on tetra and octahedral Li-signals detected in Li-extracted samples. The oxidation of Mn(III) ions goes parallel to the partial dissolution of the spinel, following Hunter's mechanism. Based on this mechanism, a generalized chemical reaction has been proposed to explain the formation of intermediate Li(+) de-intercalated samples during acid treatment in aqueous media. By the (1)H MAS NMR study, no evidence of Li-H topotactic exchange in the bulk of the acid treated material was found.

1H MAS NMR (magic-angle spinning nuclear magnetic resonance) techniques for the quantitative determination of hydrogen types in solid catalysts and supports.

Science.gov (United States)

Kennedy, Gordon J; Afeworki, Mobae; Calabro, David C; Chase, Clarence E; Smiley, Randolph J

2004-06-01

Distinct hydrogen species are present in important inorganic solids such as zeolites, silicoaluminophosphates (SAPOs), mesoporous materials, amorphous silicas, and aluminas. These H species include hydrogens associated with acidic sites such as Al(OH)Si, non-framework aluminum sites, silanols, and surface functionalities. Direct and quantitative methodology to identify, measure, and monitor these hydrogen species are key to monitoring catalyst activity, optimizing synthesis conditions, tracking post-synthesis structural modifications, and in the preparation of novel catalytic materials. Many workers have developed several techniques to address these issues, including 1H MAS NMR (magic-angle spinning nuclear magnetic resonance). 1H MAS NMR offers many potential advantages over other techniques, but care is needed in recognizing experimental limitations and developing sample handling and NMR methodology to obtain quantitatively reliable data. A simplified approach is described that permits vacuum dehydration of multiple samples simultaneously and directly in the MAS rotor without the need for epoxy, flame sealing, or extensive glovebox use. We have found that careful optimization of important NMR conditions, such as magnetic field homogeneity and magic angle setting are necessary to acquire quantitative, high-resolution spectra that accurately measure the concentrations of the different hydrogen species present. Details of this 1H MAS NMR methodology with representative applications to zeolites, SAPOs, M41S, and silicas as a function of synthesis conditions and post-synthesis treatments (i.e., steaming, thermal dehydroxylation, and functionalization) are presented.

Testing aspects of advanced coherent electron cooling technique

Energy Technology Data Exchange (ETDEWEB)

Litvinenko, V.; Jing, Y.; Pinayev, I.; Wang, G.; Samulyak, R.; Ratner, D.

2015-05-03

An advanced version of the Coherent-electron Cooling (CeC) based on the micro-bunching instability was proposed. This approach promises significant increase in the bandwidth of the CeC system and, therefore, significant shortening of cooling time in high-energy hadron colliders. In this paper we present our plans of simulating and testing the key aspects of this proposed technique using the set-up of the coherent-electron-cooling proof-of-principle experiment at BNL.

Advanced imaging techniques in pediatric body MRI

Energy Technology Data Exchange (ETDEWEB)

Courtier, Jesse [UCSF Benioff Children' s Hospital, Department of Radiology and Biomedical Imaging, San Francisco, CA (United States); Rao, Anil G. [Medical University of South Carolina, Department of Radiology, Charleston, SC (United States); Anupindi, Sudha A. [Children' s Hospital of Philadelphia, Department of Radiology, Philadelphia, PA (United States)

2017-05-15

While there are many challenges specific to pediatric abdomino-pelvic MRI, many recent advances are addressing these challenges. It is therefore essential for radiologists to be familiar with the latest advances in MR imaging. Laudable efforts have also recently been implemented in many centers to improve the overall experience of pediatric patients, including the use of dedicated radiology child life specialists, MRI video goggles, and improved MR suite environments. These efforts have allowed a larger number of children to be scanned while awake, with fewer studies being done under sedation or anesthesia; this has resulted in additional challenges from patient motion and difficulties with breath-holding and tolerating longer scan times. In this review, we highlight common challenges faced in imaging the pediatric abdomen and pelvis and discuss the application of the newest techniques to address these challenges. Additionally, we highlight the newest advances in quantified imaging techniques, specifically in MR liver iron quantification. The techniques described in this review are all commercially available and can be readily implemented. (orig.)

Biosynthetic origin of acetic acid using SNIF-NMR

International Nuclear Information System (INIS)

Boffo, Elisangela Fabiana; Ferreira, Antonio Gilberto

2006-01-01

The main purpose of this work is to describe the use of the technique Site-Specific Natural Isotopic Fractionation of hydrogen (SNIF-NMR), using 2 H and 1 H NMR spectroscopy, to investigate the biosynthetic origin of acetic acid in commercial samples of Brazilian vinegar. This method is based on the deuterium to hydrogen ratio at a specific position (methyl group) of acetic acid obtained by fermentation, through different biosynthetic mechanisms, which result in different isotopic ratios. We measured the isotopic ratio of vinegars obtained through C 3 , C 4 , and CAM biosynthetic mechanisms, blends of C 3 and C 4 (agrins) and synthetic acetic acid. (author)

Fundamentals of Protein NMR Spectroscopy

CERN Document Server

Rule, Gordon S

2006-01-01

NMR spectroscopy has proven to be a powerful technique to study the structure and dynamics of biological macromolecules. Fundamentals of Protein NMR Spectroscopy is a comprehensive textbook that guides the reader from a basic understanding of the phenomenological properties of magnetic resonance to the application and interpretation of modern multi-dimensional NMR experiments on 15N/13C-labeled proteins. Beginning with elementary quantum mechanics, a set of practical rules is presented and used to describe many commonly employed multi-dimensional, multi-nuclear NMR pulse sequences. A modular analysis of NMR pulse sequence building blocks also provides a basis for understanding and developing novel pulse programs. This text not only covers topics from chemical shift assignment to protein structure refinement, as well as the analysis of protein dynamics and chemical kinetics, but also provides a practical guide to many aspects of modern spectrometer hardware, sample preparation, experimental set-up, and data pr...

An Advanced Control Technique for Floating Offshore Wind Turbines Based on More Compact Barge Platforms

Directory of Open Access Journals (Sweden)

Joannes Olondriz

2018-05-01

Full Text Available Hydrodynamic Floating Offshore Wind Turbine (FOWT platform specifications are typically dominated by seaworthiness and maximum operating platform-pitch angle-related requirements. However, such specifications directly impact the challenge posed by an FOWT in terms of control design. The conventional FOWT systems are typically based on large, heavy floating platforms, which are less likely to suffer from the negative damping effect caused by the excessive coupling between blade-pitch control and platform-pitch motion. An advanced control technique is presented here to increase system stability for barge type platforms. Such a technique mitigates platform-pitch motions and improves the generator speed regulation, while maintaining blade-pitch activity and reducing blade and tower loads. The NREL’s 5MW + ITI Energy barge reference model is taken as a basis for this work. Furthermore, the capabilities of the proposed controller for performing with a more compact and less hydrodynamically stable barge platform is analysed, with encouraging results.

Advanced Morphological and Functional Magnetic Resonance Techniques in Glaucoma

Directory of Open Access Journals (Sweden)

Rodolfo Mastropasqua

2015-01-01

Full Text Available Glaucoma is a multifactorial disease that is the leading cause of irreversible blindness. Recent data documented that glaucoma is not limited to the retinal ganglion cells but that it also extends to the posterior visual pathway. The diagnosis is based on the presence of signs of glaucomatous optic neuropathy and consistent functional visual field alterations. Unfortunately these functional alterations often become evident when a significant amount of the nerve fibers that compose the optic nerve has been irreversibly lost. Advanced morphological and functional magnetic resonance (MR techniques (morphometry, diffusion tensor imaging, arterial spin labeling, and functional connectivity may provide a means for observing modifications induced by this fiber loss, within the optic nerve and the visual cortex, in an earlier stage. The aim of this systematic review was to determine if the use of these advanced MR techniques could offer the possibility of diagnosing glaucoma at an earlier stage than that currently possible.

75 FR 44015 - Certain Semiconductor Products Made by Advanced Lithography Techniques and Products Containing...

Science.gov (United States)

2010-07-27

... Advanced Lithography Techniques and Products Containing Same; Notice of Investigation AGENCY: U.S... violations of section 337 based upon the importation into the United States, the sale for importation, and the sale within the United States after importation of certain semiconductor products made by advanced...

Ischemic stroke progress evaluation by 31P NMR-based metabonomic of human serum

International Nuclear Information System (INIS)

Grandizoli, Caroline W.P.S.; Barison, Andersson; Lange, Marcos C.; Novak, Felipe T. M.; Campos, Francinete R.

2014-01-01

In this work, chemometric analyses over 31 P{ 1H } NMR (nuclear magnetic resonance) spectra of human blood serum permitted to discriminated ischemic stroke patients from health individuals due to changes in the chemical composition of phosphorus-containing compounds. These results indicate that 31 P NMR-based metabonomic allowed insights over the mechanism triggered by ischemic stroke. (author)

NMR spectroscopy study of agar-based polymers electrolytes

Energy Technology Data Exchange (ETDEWEB)

Mattos, R.I.; Tambelli, C.E. [Universidade de Sao Paulo (USP), Pirassununga, SP (Brazil). Fac. de Zootecnia e Engenharia de Alimentos; Raphael, E. [Universidade Federal de Sao Joao del-Rey (UFSJ), MG (Brazil). Dept. de Ciencias Naturais; Silva, I.D.A.; Magon, C.J.; Donoso, J.P. [Universidade de Sao Paulo (IFSC/USP), Sao Carlos, SP (Brazil). Inst. de Fisica

2012-07-01

Full text: This communication presents the results of preparation and characterization of transparent films obtained from agar and acetic acid. The films were characterized by electrochemical impedance spectroscopy (EIS) and nuclear magnetic resonance (NMR). The film formed by agar (Sigma Aldrich) was dispersed in water and kept under stirring and heating at 100 deg C. Next, glycerol, formaldehyde and different quantities of acetic acid (25 and 50 wt%) were added to this solution. The obtained solution was placed on a glass plate and left to dry for 48 hours in oven at 50 deg C to obtain the films, which were kept under vacuum before characterization. The ionic conductivity of the films display an Arrhenius behavior with activation energy E{sub a} = 78 (25 wt% of acetic acid) and E{sub a} = 87 kJ/mol (50 wt% of acetic acid). The conductivity values were 3:0 X 10{sup -6} and 1:2 X 10{sup -4} S/cm at room temperature and 4:4 X 10{sup -4} and 1:5 X 10{sup -3}S/cm at 70 deg C, for the 25 and 50 wt% of acetic acid respectively. To investigate the mechanism of protonic conduction in the polymer proton conductor proton NMR measurements were performed in the temperature range 200-370 K. The {sup 1}H-NMR results exhibit the qualitative feature associated with the proton mobility, namely the presence of well defined {sup 1}H spin-lattice relaxation maxima at 300 K. Activation energy of the order of 40 kJ/mol was obtained from the {sup 1}H-NMR line narrowing data. The ionic conductivity of the film combined with their transparency, flexibility, homogeneity and good adhesion to the glasses or metals indicate that agar-based SPEs are promising materials for used on optoelectronic applications. (author)

Performance of the WeNMR CS-Rosetta3 web server in CASD-NMR.

Science.gov (United States)

van der Schot, Gijs; Bonvin, Alexandre M J J

2015-08-01

We present here the performance of the WeNMR CS-Rosetta3 web server in CASD-NMR, the critical assessment of automated structure determination by NMR. The CS-Rosetta server uses only chemical shifts for structure prediction, in combination, when available, with a post-scoring procedure based on unassigned NOE lists (Huang et al. in J Am Chem Soc 127:1665-1674, 2005b, doi: 10.1021/ja047109h). We compare the original submissions using a previous version of the server based on Rosetta version 2.6 with recalculated targets using the new R3FP fragment picker for fragment selection and implementing a new annotation of prediction reliability (van der Schot et al. in J Biomol NMR 57:27-35, 2013, doi: 10.1007/s10858-013-9762-6), both implemented in the CS-Rosetta3 WeNMR server. In this second round of CASD-NMR, the WeNMR CS-Rosetta server has demonstrated a much better performance than in the first round since only converged targets were submitted. Further, recalculation of all CASD-NMR targets using the new version of the server demonstrates that our new annotation of prediction quality is giving reliable results. Predictions annotated as weak are often found to provide useful models, but only for a fraction of the sequence, and should therefore only be used with caution.

Characterization of new materials in chromatography and fuel cell development by modern NMR techniques; Charakterisierung neuer Materialien in der Chromatographie und Brennstoffzellen-Forschung mit Hilfe moderner NMR-Techniken

Energy Technology Data Exchange (ETDEWEB)

Schauff, S.

2007-12-28

directly observed using 1H HR-MAS NMR spectroscopy. Changing the mobile phase concentration and composition caused a shift of the broadened peak towards the narrow CH2 signal, resulting in the fusion of both. These effects were explained by two different theories, one of which substantiates with polarity differences, the other with the winding up of the C18 alkyl chains. Separating interactions were also investigated using the suspended-state STD HR-MAS NMR technique that unveiled the part of analyte molecule interacting with the chromatographic sorbent. Furthermore, the molecular recognition of a particulate and a monolithic MIP towards their respective template molecules was investigated using 1H STD HR-MAS NMR spectroscopy. The obtained data proved superiority of the respective MIP over the NIP, and definite knowledge of the interaction site at the analyte molecules could be gained. Differences between specific and non-specific binding could be observed. (orig.)

HPLC-NMR revisited: Using time-slice HPLC-SPE-NMR with database assisted dereplication

DEFF Research Database (Denmark)

Johansen, Kenneth; Wubshet, Sileshi Gizachew; Nyberg, Nils

2013-01-01

Time based trapping of chromatographically separated compounds on to solid-phase extraction cartridges (SPE) and subsequent elution to NMR-tubes was done to emulate the function of HPLC–NMR for dereplication purposes. Sufficient mass sensitivity was obtained by the use of a state-of-the-art HPLC......–SPE–NMR-system with a cryogenically cooled probe head, designed for 1.7 mm NMR-tubes. The resulting 1H NMR spectra (600 MHz) were evaluated against a database of previously acquired and prepared spectra. The in-house developed matching algorithm, based on partitioning of the spectra and allowing for changes in the chemical shifts......, is described and the code included as Supplementary Information. Two mixtures of natural products was used to test the approach; one extract of Carthamus oxyacantha (wild safflower) containing an array of spiro compounds and one extract of the endophytic fungus Penicillum namyslowski containing griseofulvin...

Revisiting 63Cu NMR evidence for charge order in superconducting La1.885Sr0.115CuO4

Science.gov (United States)

Imai, T.; Takahashi, S. K.; Arsenault, A.; Acton, A. W.; Lee, D.; He, W.; Lee, Y. S.; Fujita, M.

2017-12-01

The presence of charge and spin stripe order in the La2CuO4 -based family of superconductors continues to lead to new insight on the unusual ground-state properties of high-Tc cuprates. Soon after the discovery of charge stripe order at Tcharge≃65 K in Nd3 + co-doped La1.48Nd0.4Sr0.12CuO4 (Tc≃6 K) [Tranquada et al., Nature (London) 375, 561 (1995), 10.1038/375561a0], Hunt et al. demonstrated that La1.48Nd0.4Sr0.12CuO4 and superconducting La2 -xSrxCuO4 with x ˜1 /8 (Tc≃30 K) share nearly identical NMR anomalies near Tcharge of the former [Phys. Rev. Lett. 82, 4300 (1999), 10.1103/PhysRevLett.82.4300]. Their inevitable conclusion that La1.885Sr0.115CuO4 also undergoes charge order at a comparable temperature became controversial, because diffraction measurements at the time were unable to detect Bragg peaks associated with charge order. Recent advances in x-ray diffraction techniques finally led to definitive confirmations of the charge order Bragg peaks in La1.885Sr0.115CuO4 with an onset at as high as Tcharge≃80 K. Meanwhile, improved instrumental technology has enabled routine NMR measurements that were not feasible two decades ago. Motivated by these new developments, we revisit the charge order transition of a La1.885Sr0.115CuO4 single crystal based on 63Cu NMR techniques. We demonstrate that 63Cu NMR properties of the nuclear spin Iz=-1/2 to +1/2 central transition below Tcharge exhibit unprecedentedly strong dependence on the measurement time scale set by the separation time τ between the 90∘ and 180∘ radio-frequency pulses; a new kind of anomalous, very broad winglike 63Cu NMR signals gradually emerge below Tcharge only for extremely short τ ≲4 μ s , while the spectral weight INormal of the normal NMR signals is progressively wiped out. The NMR linewidth and relaxation rates depend strongly on τ below Tcharge, and their enhancement in the charge ordered state indicates that charge order turns on strong but inhomogeneous growth of Cu spin

Using Essential Oils to Teach Advanced-Level Organic Chemistry Separation Techniques and Spectroscopy

Science.gov (United States)

Bott, Tina M.; Wan, Hayley

2013-01-01

Students sometimes have difficulty grasping the importance of when and how basic distillation techniques, column chromatography, TLC, and basic spectroscopy (IR and NMR) can be used to identify unknown compounds within a mixture. This two-part experiment uses mixtures of pleasant-smelling, readily available terpenoid compounds as unknowns to…

Deuteron NMR and modelling in solid polymers

International Nuclear Information System (INIS)

Hirschinger, J.

1992-01-01

Deuteron NMR techniques are described and some recent applications to the study of rotational motions in solid polymers are reviewed. The information content and the domain of applicability of each technique are presented. Ultra-slow motions are studied in real time without any motional model consideration. For very fast motions, computer molecular dynamics simulations are shown to complement the NMR results. Experimental examples deal with the chain motion in the crystalline α-phase of poly(vinylidenefluoride) and nylon 6,6

Solid-state NMR basic principles and practice

CERN Document Server

Apperley, David C; Hodgkinson, Paul

2014-01-01

Nuclear Magnetic Resonance (NMR) has proved to be a uniquely powerful and versatile tool for analyzing and characterizing chemicals and materials of all kinds. This book focuses on the latest developments and applications for "solid-state" NMR, which has found new uses from archaeology to crystallography to biomaterials and pharmaceutical science research. The book will provide materials engineers, analytical chemists, and physicists, in and out of lab, a survey of the techniques and the essential tools of solid-state NMR, together with a practical guide on applications. In this concise introduction to the growing field of solid-state nuclear magnetic resonance spectroscopy The reader will find: * Basic NMR concepts for solids, including guidance on the spin-1/2 nuclei concept * Coverage of the quantum mechanics aspects of solid state NMR and an introduction to the concept of quadrupolar nuclei * An understanding relaxation, exchange and quantitation in NMR * An analysis and interpretation of NMR data, with e...

Exploring the limits to spatially resolved NMR

Energy Technology Data Exchange (ETDEWEB)

Gaedke, Achim; Nestle, Nikolaus [TU Darmstadt, Institute of Condensed Matter Physics (Germany)

2010-07-01

Recent advances in MRI have demonstrated resolutions down to 1 {mu}m. Magnetic resonance force microscopy has the potential to reach sensitivity for single nuclear spins. Given these numbers, in vivo imaging of single cells or even biomacromolecules may seem possible. However, for in vivo applications, there are fundamental differences in the contrast mechanisms compared to MRI at macroscopic scales as the length scale of of molecular self-diffusion exceeds that of the spatial resolution on the NMR time scale. Those effects - which are fundamentally different from the echo attenuation in field gradient NMR - even may lead to general limitations on the spatial resolution achievable in aqueous systems with high water content. In our contribution, we explore those effects on a model system in a high-resolution stray-field imaging setup. In addition to experimental results, simulations based on the Bloch-Torrey equation are presented.

Direct 13C NMR Detection in HPLC Hyphenation Mode

DEFF Research Database (Denmark)

Wubshet, Sileshi Gizachew; Johansen, Kenneth; Nyberg, Nils

2012-01-01

Solid phase extraction (SPE) was introduced as a crucial step in the HPLC-SPE-NMR technique to enable online analyte enrichment from which proton-detected NMR experiments on submicrogram amounts from complex mixtures were possible. However, the significance of direct-detected (13)C NMR experiments...... application of HPLC-SPE-NMR analysis using direct-detected (13)C NMR spectra. HPLC column loading, accumulative SPE trappings, and the effect of different elution solvents were evaluated and optimized. A column loading of approximately 600 mug of a prefractionated triterpenoid mixture, six trappings...

NMR imaging of soft tissue tumors

International Nuclear Information System (INIS)

Laval-Jeantet, M.; Tobolsk, F.; Delepine, N.; Delepine, G.; Roger, B.; Cabanis, E.A.

1986-01-01

Preliminary findings on NMR imaging of 30 soft tissue tumors demonstrated the indispensable value of this examination (particularly when a surface antenna is used) for preoperative investigation and diagnosis of tumoral recurrence when compared with other radiologic techniques. The possible potential of NMR imaging for characterization of tissues, apart from lipoma or liposarcoma, cannot be evaluated at the present time [fr

NMR screening in fragment-based drug design: a practical guide.

Science.gov (United States)

Kim, Hai-Young; Wyss, Daniel F

2015-01-01

Fragment-based drug design (FBDD) comprises both fragment-based screening (FBS) to find hits and elaboration of these hits to lead compounds. Typical fragment hits have lower molecular weight (FBDD since it identifies and localizes the binding site of weakly interacting hits on the target protein. Here we describe ligand-based NMR methods for hit identification from fragment libraries and for functional cross-validation of primary hits.

Test Concept for Advanced Oxidation Techniques

DEFF Research Database (Denmark)

Bennedsen, Lars Rønn; Søgaard, Erik Gydesen; Mortensen, Lars

advanced on-site oxidation tests. The remediation techniques included are electrochemical oxidation, photochemical/photocatalytic oxidation, ozone, hydrogen peroxide, permanganate, and persulfate among others. A versatile construction of the mobile test unit makes it possible to combine different...

Performance of the WeNMR CS-Rosetta3 web server in CASD-NMR

Energy Technology Data Exchange (ETDEWEB)

Schot, Gijs van der [Uppsala University, Laboratory of Molecular Biophysics, Department of Cell and Molecular Biology (Sweden); Bonvin, Alexandre M. J. J., E-mail: a.m.j.j.bonvin@uu.nl [Utrecht University, Faculty of Science – Chemistry, Bijvoet Center for Biomolecular Research (Netherlands)

2015-08-15

We present here the performance of the WeNMR CS-Rosetta3 web server in CASD-NMR, the critical assessment of automated structure determination by NMR. The CS-Rosetta server uses only chemical shifts for structure prediction, in combination, when available, with a post-scoring procedure based on unassigned NOE lists (Huang et al. in J Am Chem Soc 127:1665–1674, 2005b, doi: 10.1021/ja047109h 10.1021/ja047109h ). We compare the original submissions using a previous version of the server based on Rosetta version 2.6 with recalculated targets using the new R3FP fragment picker for fragment selection and implementing a new annotation of prediction reliability (van der Schot et al. in J Biomol NMR 57:27–35, 2013, doi: 10.1007/s10858-013-9762-6 10.1007/s10858-013-9762-6 ), both implemented in the CS-Rosetta3 WeNMR server. In this second round of CASD-NMR, the WeNMR CS-Rosetta server has demonstrated a much better performance than in the first round since only converged targets were submitted. Further, recalculation of all CASD-NMR targets using the new version of the server demonstrates that our new annotation of prediction quality is giving reliable results. Predictions annotated as weak are often found to provide useful models, but only for a fraction of the sequence, and should therefore only be used with caution.

Performance of the WeNMR CS-Rosetta3 web server in CASD-NMR

International Nuclear Information System (INIS)

Schot, Gijs van der; Bonvin, Alexandre M. J. J.

2015-01-01

We present here the performance of the WeNMR CS-Rosetta3 web server in CASD-NMR, the critical assessment of automated structure determination by NMR. The CS-Rosetta server uses only chemical shifts for structure prediction, in combination, when available, with a post-scoring procedure based on unassigned NOE lists (Huang et al. in J Am Chem Soc 127:1665–1674, 2005b, doi: 10.1021/ja047109h 10.1021/ja047109h ). We compare the original submissions using a previous version of the server based on Rosetta version 2.6 with recalculated targets using the new R3FP fragment picker for fragment selection and implementing a new annotation of prediction reliability (van der Schot et al. in J Biomol NMR 57:27–35, 2013, doi: 10.1007/s10858-013-9762-6 10.1007/s10858-013-9762-6 ), both implemented in the CS-Rosetta3 WeNMR server. In this second round of CASD-NMR, the WeNMR CS-Rosetta server has demonstrated a much better performance than in the first round since only converged targets were submitted. Further, recalculation of all CASD-NMR targets using the new version of the server demonstrates that our new annotation of prediction quality is giving reliable results. Predictions annotated as weak are often found to provide useful models, but only for a fraction of the sequence, and should therefore only be used with caution

NMR imaging of human atherosclerosis

International Nuclear Information System (INIS)

Toussaint, J.F.

1995-01-01

Diagnosis and prognosis of atherosclerosis can no longer be evaluated with morphological parameters only. A description of atherosclerotic plaque composition is necessary to study the mechanisms of plaque rupture, which depends on collagenous cap and lipid core thicknesses. NMR, as a biochemical imaging technique, allows visualization of these components using T1 contrast (mobile lipids), T2 contrast (cap vs. core), spin density (calcifications), diffusion imaging, 1H and 13C spectroscopy. Today, these imaging sequences allow to study in vitro the effects of interventional techniques such as angioplasty or atherectomy. Clinical investigations begin, which will attempt to develop in vivo microscopy and test the ability of NMR to predict plaque rupture. (author). 13 refs., 7 figs

Magic Angle Spinning NMR Structure Determination of Proteins from Pseudocontact Shifts

KAUST Repository

Li, Jianping

2013-06-05

Magic angle spinning solid-state NMR is a unique technique to study atomic-resolution structure of biomacromolecules which resist crystallization or are too large to study by solution NMR techniques. However, difficulties in obtaining sufficient number of long-range distance restraints using dipolar coupling based spectra hamper the process of structure determination of proteins in solid-state NMR. In this study it is shown that high-resolution structure of proteins in solid phase can be determined without the use of traditional dipolar-dipolar coupling based distance restraints by combining the measurements of pseudocontact shifts (PCSs) with Rosetta calculations. The PCSs were generated by chelating exogenous paramagnetic metal ions to a tag 4-mercaptomethyl-dipicolinic acid, which is covalently attached to different residue sites in a 56-residue immunoglobulin-binding domain of protein G (GB1). The long-range structural restraints with metal-nucleus distance of up to ∼20 Å are quantitatively extracted from experimentally observed PCSs, and these are in good agreement with the distances back-calculated using an X-ray structure model. Moreover, we demonstrate that using several paramagnetic ions with varied paramagnetic susceptibilities as well as the introduction of paramagnetic labels at different sites can dramatically increase the number of long-range restraints and cover different regions of the protein. The structure generated from solid-state NMR PCSs restraints combined with Rosetta calculations has 0.7 Å root-mean-square deviation relative to X-ray structure. © 2013 American Chemical Society.

Magic Angle Spinning NMR Structure Determination of Proteins from Pseudocontact Shifts

KAUST Repository

Li, Jianping; Pilla, Kala Bharath; Li, Qingfeng; Zhang, Zhengfeng; Su, Xuncheng; Huber, Thomas; Yang, Jun

2013-01-01

Magic angle spinning solid-state NMR is a unique technique to study atomic-resolution structure of biomacromolecules which resist crystallization or are too large to study by solution NMR techniques. However, difficulties in obtaining sufficient number of long-range distance restraints using dipolar coupling based spectra hamper the process of structure determination of proteins in solid-state NMR. In this study it is shown that high-resolution structure of proteins in solid phase can be determined without the use of traditional dipolar-dipolar coupling based distance restraints by combining the measurements of pseudocontact shifts (PCSs) with Rosetta calculations. The PCSs were generated by chelating exogenous paramagnetic metal ions to a tag 4-mercaptomethyl-dipicolinic acid, which is covalently attached to different residue sites in a 56-residue immunoglobulin-binding domain of protein G (GB1). The long-range structural restraints with metal-nucleus distance of up to ∼20 Å are quantitatively extracted from experimentally observed PCSs, and these are in good agreement with the distances back-calculated using an X-ray structure model. Moreover, we demonstrate that using several paramagnetic ions with varied paramagnetic susceptibilities as well as the introduction of paramagnetic labels at different sites can dramatically increase the number of long-range restraints and cover different regions of the protein. The structure generated from solid-state NMR PCSs restraints combined with Rosetta calculations has 0.7 Å root-mean-square deviation relative to X-ray structure. © 2013 American Chemical Society.

NMR studies of preimplantation embryo metabolism in human assisted reproductive techniques: a new biomarker for assessment of embryo implantation potential.

Science.gov (United States)

Pudakalakatti, Shivanand M; Uppangala, Shubhashree; D'Souza, Fiona; Kalthur, Guruprasad; Kumar, Pratap; Adiga, Satish Kumar; Atreya, Hanudatta S

2013-01-01

There has been growing interest in understanding energy metabolism in human embryos generated using assisted reproductive techniques (ART) for improving the overall success rate of the method. Using NMR spectroscopy as a noninvasive tool, we studied human embryo metabolism to identify specific biomarkers to assess the quality of embryos for their implantation potential. The study was based on estimation of pyruvate, lactate and alanine levels in the growth medium, ISM1, used in the culture of embryos. An NMR study involving 127 embryos from 48 couples revealed that embryos transferred on Day 3 (after 72 h in vitro culture) with successful implantation (pregnancy) exhibited significantly (p < 10(-5) ) lower pyruvate/alanine ratios compared to those that failed to implant. Lactate levels in media were similar for all embryos. This implies that in addition to lactate production, successfully implanted embryos use pyruvate to produce alanine and other cellular functions. While pyruvate and alanine individually have been used as biomarkers, the present study highlights the potential of combining them to provide a single parameter that correlates strongly with implantation potential. Copyright © 2012 John Wiley & Sons, Ltd.

The stereochemistry of the condensation product of salicylaldehyde and n-butylbarbituric acid by NMR techniques

International Nuclear Information System (INIS)

Cruz, Elizabete R.; Villar, J. Daniel Figueroa

1995-01-01

Since the discovery of the 5-deazaflavin cofactor (coenzyme F 420 ) as a naturally occurring compound, a great attention has been focused on several iso steric flavin analogues. One of the simplest approaches towards the synthesis of oxadeazaflavin, compound which the nitrogen at the N-10 position of 5-deazaflavin is replaced by oxygen, is the direct condensation between barbituric acid and salicylaldehyde. In this paper, the use of some NMR techniques so as to determine the stereochemistry of the preformed isomer has been described and a possible mechanism for this isomerization discussed

Integrative NMR for biomolecular research

International Nuclear Information System (INIS)

Lee, Woonghee; Cornilescu, Gabriel; Dashti, Hesam; Eghbalnia, Hamid R.; Tonelli, Marco; Westler, William M.; Butcher, Samuel E.; Henzler-Wildman, Katherine A.; Markley, John L.

2016-01-01

NMR spectroscopy is a powerful technique for determining structural and functional features of biomolecules in physiological solution as well as for observing their intermolecular interactions in real-time. However, complex steps associated with its practice have made the approach daunting for non-specialists. We introduce an NMR platform that makes biomolecular NMR spectroscopy much more accessible by integrating tools, databases, web services, and video tutorials that can be launched by simple installation of NMRFAM software packages or using a cross-platform virtual machine that can be run on any standard laptop or desktop computer. The software package can be downloaded freely from the NMRFAM software download page ( http://pine.nmrfam.wisc.edu/download-packages.html http://pine.nmrfam.wisc.edu/download_packages.html ), and detailed instructions are available from the Integrative NMR Video Tutorial page ( http://pine.nmrfam.wisc.edu/integrative.html http://pine.nmrfam.wisc.edu/integrative.html ).

Integrative NMR for biomolecular research

Energy Technology Data Exchange (ETDEWEB)

Lee, Woonghee, E-mail: whlee@nmrfam.wisc.edu; Cornilescu, Gabriel; Dashti, Hesam; Eghbalnia, Hamid R.; Tonelli, Marco; Westler, William M.; Butcher, Samuel E.; Henzler-Wildman, Katherine A.; Markley, John L., E-mail: markley@nmrfam.wisc.edu [University of Wisconsin-Madison, National Magnetic Resonance Facility at Madison and Biochemistry Department (United States)

2016-04-15

NMR spectroscopy is a powerful technique for determining structural and functional features of biomolecules in physiological solution as well as for observing their intermolecular interactions in real-time. However, complex steps associated with its practice have made the approach daunting for non-specialists. We introduce an NMR platform that makes biomolecular NMR spectroscopy much more accessible by integrating tools, databases, web services, and video tutorials that can be launched by simple installation of NMRFAM software packages or using a cross-platform virtual machine that can be run on any standard laptop or desktop computer. The software package can be downloaded freely from the NMRFAM software download page ( http://pine.nmrfam.wisc.edu/download-packages.html http://pine.nmrfam.wisc.edu/download{sub p}ackages.html ), and detailed instructions are available from the Integrative NMR Video Tutorial page ( http://pine.nmrfam.wisc.edu/integrative.html http://pine.nmrfam.wisc.edu/integrative.html ).

Automatic NMR field-frequency lock-pulsed phase locked loop approach.

Science.gov (United States)

Kan, S; Gonord, P; Fan, M; Sauzade, M; Courtieu, J

1978-06-01

A self-contained deuterium frequency-field lock scheme for a high-resolution NMR spectrometer is described. It is based on phase locked loop techniques in which the free induction decay signal behaves as a voltage-controlled oscillator. By pulsing the spins at an offset frequency of a few hundred hertz and using a digital phase-frequency discriminator this method not only eliminates the usual phase, rf power, offset adjustments needed in conventional lock systems but also possesses the automatic pull-in characteristics that dispense with the use of field sweeps to locate the NMR line prior to closure of the lock loop.

Probing Spin Crossover in a Solution by Paramagnetic NMR Spectroscopy.

Science.gov (United States)

Pavlov, Alexander A; Denisov, Gleb L; Kiskin, Mikhail A; Nelyubina, Yulia V; Novikov, Valentin V

2017-12-18

Spin transitions in spin-crossover compounds are now routinely studied in the solid state by magnetometry; however, only a few methods exist for studies in solution. The currently used Evans method, which relies on NMR spectroscopy to measure the magnetic susceptibility, requires the availability of a very pure sample of the paramagnetic compound and its exact concentration. To overcome these limitations, we propose an alternative NMR-based technique for evaluating spin-state populations by only using the chemical shifts of a spin-crossover compound; those can be routinely obtained for a solution that contains unknown impurities and paramagnetic admixtures or is contaminated otherwise.

High-resolution, high-sensitivity NMR of nano-litre anisotropic samples by coil spinning

Energy Technology Data Exchange (ETDEWEB)

Sakellariou, D [CEA Saclay, DSM, DRECAM, SCM, Lab Struct and Dynam Resonance Magnet, CNRS URA 331, F-91191 Gif Sur Yvette, (France); Le Goff, G; Jacquinot, J F [CEA Saclay, DSM, DRECAM, SPEC: Serv Phys Etat Condense, CNRS URA 2464, F-91191 Gif Sur Yvette, (France)

2007-07-01

Nuclear magnetic resonance (NMR) can probe the local structure and dynamic properties of liquids and solids, making it one of the most powerful and versatile analytical methods available today. However, its intrinsically low sensitivity precludes NMR analysis of very small samples - as frequently used when studying isotopically labelled biological molecules or advanced materials, or as preferred when conducting high-throughput screening of biological samples or 'lab-on-a-chip' studies. The sensitivity of NMR has been improved by using static micro-coils, alternative detection schemes and pre-polarization approaches. But these strategies cannot be easily used in NMR experiments involving the fast sample spinning essential for obtaining well-resolved spectra from non-liquid samples. Here we demonstrate that inductive coupling allows wireless transmission of radio-frequency pulses and the reception of NMR signals under fast spinning of both detector coil and sample. This enables NMR measurements characterized by an optimal filling factor, very high radio-frequency field amplitudes and enhanced sensitivity that increases with decreasing sample volume. Signals obtained for nano-litre-sized samples of organic powders and biological tissue increase by almost one order of magnitude (or, equivalently, are acquired two orders of magnitude faster), compared to standard NMR measurements. Our approach also offers optimal sensitivity when studying samples that need to be confined inside multiple safety barriers, such as radioactive materials. In principle, the co-rotation of a micrometer-sized detector coil with the sample and the use of inductive coupling (techniques that are at the heart of our method) should enable highly sensitive NMR measurements on any mass-limited sample that requires fast mechanical rotation to obtain well-resolved spectra. The method is easy to implement on a commercial NMR set-up and exhibits improved performance with miniaturization, and we

Devices, materials, and processes for nano-electronics: characterization with advanced X-ray techniques using lab-based and synchrotron radiation sources

International Nuclear Information System (INIS)

Zschech, E.; Wyon, C.; Murray, C.E.; Schneider, G.

2011-01-01

Future nano-electronics manufacturing at extraordinary length scales, new device structures, and advanced materials will provide challenges to process development and engineering but also to process control and physical failure analysis. Advanced X-ray techniques, using lab systems and synchrotron radiation sources, will play a key role for the characterization of thin films, nano-structures, surfaces, and interfaces. The development of advanced X-ray techniques and tools will reduce risk and time for the introduction of new technologies. Eventually, time-to-market for new products will be reduced by the timely implementation of the best techniques for process development and process control. The development and use of advanced methods at synchrotron radiation sources will be increasingly important, particularly for research and development in the field of advanced processes and new materials but also for the development of new X-ray components and procedures. The application of advanced X-ray techniques, in-line, in out-of-fab analytical labs and at synchrotron radiation sources, for research, development, and manufacturing in the nano-electronics industry is reviewed. The focus of this paper is on the study of nano-scale device and on-chip interconnect materials, and materials for 3D IC integration as well. (authors)

Fast 2D NMR Spectroscopy for In vivo Monitoring of Bacterial Metabolism in Complex Mixtures

Directory of Open Access Journals (Sweden)

Rupashree Dass

2017-07-01

Full Text Available The biological toolbox is full of techniques developed originally for analytical chemistry. Among them, spectroscopic experiments are very important source of atomic-level structural information. Nuclear magnetic resonance (NMR spectroscopy, although very advanced in chemical and biophysical applications, has been used in microbiology only in a limited manner. So far, mostly one-dimensional 1H experiments have been reported in studies of bacterial metabolism monitored in situ. However, low spectral resolution and limited information on molecular topology limits the usability of these methods. These problems are particularly evident in the case of complex mixtures, where spectral peaks originating from many compounds overlap and make the interpretation of changes in a spectrum difficult or even impossible. Often a suite of two-dimensional (2D NMR experiments is used to improve resolution and extract structural information from internuclear correlations. However, for dynamically changing sample, like bacterial culture, the time-consuming sampling of so-called indirect time dimensions in 2D experiments is inefficient. Here, we propose the technique known from analytical chemistry and structural biology of proteins, i.e., time-resolved non-uniform sampling. The method allows application of 2D (and multi-D experiments in the case of quickly varying samples. The indirect dimension here is sparsely sampled resulting in significant reduction of experimental time. Compared to conventional approach based on a series of 1D measurements, this method provides extraordinary resolution and is a real-time approach to process monitoring. In this study, we demonstrate the usability of the method on a sample of Escherichia coli culture affected by ampicillin and on a sample of Propionibacterium acnes, an acne causing bacterium, mixed with a dose of face tonic, which is a complicated, multi-component mixture providing complex NMR spectrum. Through our experiments

NMR Analysis of Some Pentacycloundecanedione Derivatives

African Journals Online (AJOL)

NJD

Although many authors have commented on the difficulty of ... coming these former difficulties. Cookson's dione 19,10 .... and 2.58 ppm) is the common factor and the positions of H-2. (2.94 ppm) .... Owing to advances in NMR technology, the.

NMR-based metabonomic analysis of the hepatotoxicity induced by combined exposure to PCBs and TCDD in rats

International Nuclear Information System (INIS)

Lu Chunfeng; Wang Yimei; Sheng Zhiguo; Liu Gang; Fu Ze; Zhao Jing; Zhao Jun; Yan Xianzhong; Zhu Benzhan; Peng Shuangqing

2010-01-01

A metabonomic approach using 1 H NMR spectroscopy was adopted to investigate the metabonomic pattern of rat urine after oral administration of environmental endocrine disruptors (EDs) polychlorinated biphenyls (PCBs) and 2,3,7,8-tetrachlorodibenzo- p-dioxin (TCDD) alone or in combination and to explore the possible hepatotoxic mechanisms of combined exposure to PCBs and TCDD. 1 H NMR spectra of urines collected 24 h before and after exposure were analyzed via pattern recognition by using principal component analysis (PCA). Serum biochemistry and liver histopathology indicated significant hepatotoxicity in the rats of the combined group. The PCA scores plots of urinary 1 H NMR data showed that all the treatment groups could be easily distinguished from the control group, so could the PCBs or TCDD group and the combined group. The loadings plots of the PCA revealed remarkable increases in the levels of lactate, glucose, taurine, creatine, and 2-hydroxy-isovaleric acid and reductions in the levels of 2-oxoglutarate, citrate, succinate, hippurate, and trimethylamine-N-oxide in rat urine after exposure. These changes were more striking in the combined group. The changed metabolites may be considered possible biomarker for the hepatotoxicity. The present study demonstrates that combined exposure to PCBs and TCDD induced significant hepatotoxicity in rats, and mitochondrial dysfunction and fatty acid metabolism perturbations might contribute to the hepatotoxicity. There was good conformity between changes in the urine metabonomic pattern and those in serum biochemistry and liver histopathology. These results showed that the NMR-based metabonomic approach may provide a promising technique for the evaluation of the combined toxicity of EDs.

NMR-based metabolomics for identification of α-amylase inhibitors in rowan berries (Sorbus spp.)

DEFF Research Database (Denmark)

Broholm, Sofie L.; Gramsbergen, Simone; Nyberg, Nils

Type 2 diabetes is a metabolic disorder estimated to affect millions of people all over the world.1 One way of reducing diabetes-related complications is to control postprandial glucose.2 Inhibition of the carbohydrate digestive enzyme α-amylase is a therapeutic target for maintaining low blood g...... a 1H-NMR method suitable for NMR-based metabolomics...

Diffraction based overlay and image based overlay on production flow for advanced technology node

Science.gov (United States)

Blancquaert, Yoann; Dezauzier, Christophe

2013-04-01

One of the main challenges for lithography step is the overlay control. For the advanced technology node like 28nm and 14nm, the overlay budget becomes very tight. Two overlay techniques compete in our advanced semiconductor manufacturing: the Diffraction based Overlay (DBO) with the YieldStar S200 (ASML) and the Image Based Overlay (IBO) with ARCHER (KLA). In this paper we will compare these two methods through 3 critical production layers: Poly Gate, Contact and first metal layer. We will show the overlay results of the 2 techniques, explore the accuracy and compare the total measurement uncertainty (TMU) for the standard overlay targets of both techniques. We will see also the response and impact for the Image Based Overlay and Diffraction Based Overlay techniques through a process change like an additional Hardmask TEOS layer on the front-end stack. The importance of the target design is approached; we will propose more adapted design for image based targets. Finally we will present embedded targets in the 14 FDSOI with first results.

Advanced structural equation modeling issues and techniques

CERN Document Server

Marcoulides, George A

2013-01-01

By focusing primarily on the application of structural equation modeling (SEM) techniques in example cases and situations, this book provides an understanding and working knowledge of advanced SEM techniques with a minimum of mathematical derivations. The book was written for a broad audience crossing many disciplines, assumes an understanding of graduate level multivariate statistics, including an introduction to SEM.

Advanced Equalization Techniques for Digital Coherent Optical Receivers

DEFF Research Database (Denmark)

Arlunno, Valeria

approach based on joint encoding and equalization technique, known as Turbo Equalization (TE). This scheme is demonstrated to be powerful in transmission impairments mitigation for high order modulations formats, such as 16 Quadrature Amplitude Modulation (QAM), considered a key technology for high speed...... a lower complexity convolutional code compared to state of the art reports. Furthermore, in order to fulfill the strict constrains of spectral efficiency, this thesis shows the application of digital adaptive equalizer for reconfigurable and Ultra Dense Wavelength Division Multiplexing (U......-over-Fiber (RoF) transmission system for a stand alone case and mixed modulation mixed bit rates transmission scheme. In conclusion, this PhD thesis demonstrates the flexibility, upgrade-ability and robustness offered by rising advanced digital signal processing techniques, for future high-speed, high...

A guide to the identification of metabolites in NMR-based metabonomics/metabolomics experiments.

Science.gov (United States)

Dona, Anthony C; Kyriakides, Michael; Scott, Flora; Shephard, Elizabeth A; Varshavi, Dorsa; Veselkov, Kirill; Everett, Jeremy R

2016-01-01

Metabonomics/metabolomics is an important science for the understanding of biological systems and the prediction of their behaviour, through the profiling of metabolites. Two technologies are routinely used in order to analyse metabolite profiles in biological fluids: nuclear magnetic resonance (NMR) spectroscopy and mass spectrometry (MS), the latter typically with hyphenation to a chromatography system such as liquid chromatography (LC), in a configuration known as LC-MS. With both NMR and MS-based detection technologies, the identification of the metabolites in the biological sample remains a significant obstacle and bottleneck. This article provides guidance on methods for metabolite identification in biological fluids using NMR spectroscopy, and is illustrated with examples from recent studies on mice.

A guide to the identification of metabolites in NMR-based metabonomics/metabolomics experiments

Directory of Open Access Journals (Sweden)

Anthony C. Dona

2016-01-01

Full Text Available Metabonomics/metabolomics is an important science for the understanding of biological systems and the prediction of their behaviour, through the profiling of metabolites. Two technologies are routinely used in order to analyse metabolite profiles in biological fluids: nuclear magnetic resonance (NMR spectroscopy and mass spectrometry (MS, the latter typically with hyphenation to a chromatography system such as liquid chromatography (LC, in a configuration known as LC–MS. With both NMR and MS-based detection technologies, the identification of the metabolites in the biological sample remains a significant obstacle and bottleneck. This article provides guidance on methods for metabolite identification in biological fluids using NMR spectroscopy, and is illustrated with examples from recent studies on mice.

Quantification of organic acids in beer by nuclear magnetic resonance (NMR)-based methods

International Nuclear Information System (INIS)

Rodrigues, J.E.A.; Erny, G.L.; Barros, A.S.; Esteves, V.I.; Brandao, T.; Ferreira, A.A.; Cabrita, E.; Gil, A.M.

2010-01-01

The organic acids present in beer provide important information on the product's quality and history, determining organoleptic properties and being useful indicators of fermentation performance. NMR spectroscopy may be used for rapid quantification of organic acids in beer and different NMR-based methodologies are hereby compared for the six main acids found in beer (acetic, citric, lactic, malic, pyruvic and succinic). The use of partial least squares (PLS) regression enables faster quantification, compared to traditional integration methods, and the performance of PLS models built using different reference methods (capillary electrophoresis (CE), both with direct and indirect UV detection, and enzymatic essays) was investigated. The best multivariate models were obtained using CE/indirect detection and enzymatic essays as reference and their response was compared with NMR integration, either using an internal reference or an electrical reference signal (Electronic REference To access In vivo Concentrations, ERETIC). NMR integration results generally agree with those obtained by PLS, with some overestimation for malic and pyruvic acids, probably due to peak overlap and subsequent integral errors, and an apparent relative underestimation for citric acid. Overall, these results make the PLS-NMR method an interesting choice for organic acid quantification in beer.

Quantification of organic acids in beer by nuclear magnetic resonance (NMR)-based methods

Energy Technology Data Exchange (ETDEWEB)

Rodrigues, J.E.A. [CICECO-Department of Chemistry, University of Aveiro, Campus de Santiago, 3810-193 Aveiro (Portugal); Erny, G.L. [CESAM - Department of Chemistry, University of Aveiro, Campus de Santiago, 3810-193 Aveiro (Portugal); Barros, A.S. [QOPNAA-Department of Chemistry, University of Aveiro, Campus de Santiago, 3810-193 Aveiro (Portugal); Esteves, V.I. [CESAM - Department of Chemistry, University of Aveiro, Campus de Santiago, 3810-193 Aveiro (Portugal); Brandao, T.; Ferreira, A.A. [UNICER, Bebidas de Portugal, Leca do Balio, 4466-955 S. Mamede de Infesta (Portugal); Cabrita, E. [Department of Chemistry, New University of Lisbon, 2825-114 Caparica (Portugal); Gil, A.M., E-mail: agil@ua.pt [CICECO-Department of Chemistry, University of Aveiro, Campus de Santiago, 3810-193 Aveiro (Portugal)

2010-08-03

The organic acids present in beer provide important information on the product's quality and history, determining organoleptic properties and being useful indicators of fermentation performance. NMR spectroscopy may be used for rapid quantification of organic acids in beer and different NMR-based methodologies are hereby compared for the six main acids found in beer (acetic, citric, lactic, malic, pyruvic and succinic). The use of partial least squares (PLS) regression enables faster quantification, compared to traditional integration methods, and the performance of PLS models built using different reference methods (capillary electrophoresis (CE), both with direct and indirect UV detection, and enzymatic essays) was investigated. The best multivariate models were obtained using CE/indirect detection and enzymatic essays as reference and their response was compared with NMR integration, either using an internal reference or an electrical reference signal (Electronic REference To access In vivo Concentrations, ERETIC). NMR integration results generally agree with those obtained by PLS, with some overestimation for malic and pyruvic acids, probably due to peak overlap and subsequent integral errors, and an apparent relative underestimation for citric acid. Overall, these results make the PLS-NMR method an interesting choice for organic acid quantification in beer.

Studies of metal-biomolecule systems in liquids with beta-detected NMR

CERN Document Server

Walczak, Michal

2017-01-01

My internship took place within a small research team funded via the European Research Council (ERC Starting Grant: Beta-Drop NMR) at ISOLDE. It was devoted to laser spin-polarization and beta-detected NMR techniques and their future applications in chemistry and biology. I was involved in the design and tests of the beta-NMR spectrometer which will be used in the upcoming experiments. In this way I have been exposed to many topics in physics (atomic and nuclear physics), experimental techniques (vacuum technology, lasers, beta detectors, electronics, DAQ software), as well as chemistry and biology (NMR on metal ions, metal ion binding to biomolecules, quantum chemistry calculations).

Selected topics in solution-phase biomolecular NMR spectroscopy

Science.gov (United States)

Kay, Lewis E.; Frydman, Lucio

2017-05-01

Solution bio-NMR spectroscopy continues to enjoy a preeminent role as an important tool in elucidating the structure and dynamics of a range of important biomolecules and in relating these to function. Equally impressive is how NMR continues to 'reinvent' itself through the efforts of many brilliant practitioners who ask increasingly demanding and increasingly biologically relevant questions. The ability to manipulate spin Hamiltonians - almost at will - to dissect the information of interest contributes to the success of the endeavor and ensures that the NMR technology will be well poised to contribute to as yet unknown frontiers in the future. As a tribute to the versatility of solution NMR in biomolecular studies and to the continued rapid advances in the field we present a Virtual Special Issue (VSI) that includes over 40 articles on various aspects of solution-state biomolecular NMR that have been published in the Journal of Magnetic Resonance in the past 7 years. These, in total, help celebrate the achievements of this vibrant field.

Proton NMR studies of functionalized nanoparticles in aqueous environments

Science.gov (United States)

Tataurova, Yulia Nikolaevna

in high-resolution NMR spectra. This technique is selective for protons on the surface organic functional groups due to their motional averaging in solution. In this study, 1H solution NMR spectroscopy was used to investigate the interface of the organic functional groups in D2O. The pKa for these functional groups covalently bound to the surface of nanoparticles was determined using an NMR-pH titration method based on the variation in the proton chemical shift for the alkyl group protons closest to the amine group with pH. The adsorption of toxic contaminants (chromate and arsenate anions) on the surface of functionalized silicalite-1 and mesoporous silica nanoparticles has been studied by 1H solution NMR spectroscopy. With this method, the surface bound contaminants are detected. The analysis of the intensity and position of these peaks allows quantitative assessment of the relative amounts of functional groups with adsorbed metal ions. These results demonstrate the sensitivity of solution NMR spectroscopy to the electronic environment and structure of the surface functional groups on porous nanomaterials.

Microcomputer utilization for comparison of 1H-NMR spectra with data base standards

International Nuclear Information System (INIS)

Vale Rodrigues, G. do; Nagem, T.J.

1989-01-01

A new computacional technique for the storage of spectrometric data of natural products listed in the literature and its comparison with data of new compounds isolated as natural products is described here. The programs allow a correlation of two spectra by inverting one relative to the other. The programs again permit the comparison of two NMR spectra in different frequencies. (author) [pt

Development and applications of quantitative NMR spectroscopy

International Nuclear Information System (INIS)

Yamazaki, Taichi

2016-01-01

Recently, quantitative NMR spectroscopy has attracted attention as an analytical method which can easily secure traceability to SI unit system, and discussions about its accuracy and inaccuracy are also started. This paper focuses on the literatures on the advancement of quantitative NMR spectroscopy reported between 2009 and 2016, and introduces both NMR measurement conditions and actual analysis cases in quantitative NMR. The quantitative NMR spectroscopy using an internal reference method enables accurate quantitative analysis with a quick and versatile way in general, and it is possible to obtain the precision sufficiently applicable to the evaluation of pure substances and standard solutions. Since the external reference method can easily prevent contamination to samples and the collection of samples, there are many reported cases related to the quantitative analysis of biologically related samples and highly scarce natural products in which NMR spectra are complicated. In the precision of quantitative NMR spectroscopy, the internal reference method is superior. As the quantitative NMR spectroscopy widely spreads, discussions are also progressing on how to utilize this analytical method as the official methods in various countries around the world. In Japan, this method is listed in the Pharmacopoeia and Japanese Standard of Food Additives, and it is also used as the official method for purity evaluation. In the future, this method will be expected to spread as the general-purpose analysis method that can ensure traceability to SI unit system. (A.O.)

1H NMR-based metabolomics of time-dependent responses of Eisenia fetida to sub-lethal phenanthrene exposure

International Nuclear Information System (INIS)

Lankadurai, Brian P.; Wolfe, David M.; Simpson, Andre J.; Simpson, Myrna J.

2011-01-01

1 H NMR-based metabolomics was used to examine the response of the earthworm Eisenia fetida after exposure to sub-lethal concentrations of phenanthrene over time. Earthworms were exposed to 0.025 mg/cm 2 of phenanthrene (1/64th of the LC 50 ) via contact tests over four days. Earthworm tissues were extracted using a mixture of chloroform, methanol and water, resulting in polar and non-polar fractions that were analyzed by 1 H NMR after one, two, three and four days. NMR-based metabolomic analyses revealed heightened E. fetida responses with longer phenanthrene exposure times. Amino acids alanine and glutamate, the sugar maltose, the lipids cholesterol and phosphatidylcholine emerged as potential indicators of phenanthrene exposure. The conversion of succinate to fumarate in the Krebs cycle was also interrupted by phenanthrene. Therefore, this study shows that NMR-based metabolomics is a powerful tool for elucidating time-dependent relationships in addition to the mode of toxicity of phenanthrene in earthworm exposure studies. - Highlights: → NMR-based earthworm metabolomic analysis of the mode of action of phenanthrene is presented. → The earthworm species E. fetida were exposed to sub-lethal phenanthrene concentrations. → Both polar and non-polar metabolites of E. fetida tissue extracts were analyzed by 1 H NMR. → Longer phenanthrene exposure times resulted in heightened earthworm responses. → An interruption of the Krebs cycle was also observed due to phenanthrene exposure. - 1 H NMR metabolomics is used to determine the relationship between phenanthrene exposure and the metabolic response of the earthworm E. fetida over time and also to elucidate the phenanthrene mode of toxicity.

Thermometry of hot spot using NMR for hyperthermia

International Nuclear Information System (INIS)

Amemiya, Yoshifumi; Kamimura, Yoshitsugu

1983-01-01

Lately noticed hyperthermia in cancer therapy requires non-invasive measurement of the temperature at the warmed site in the deep portion of human body. Nuclear magnetic relaxation time of NMR is also usable for cancer diagnosis. For coordination of these two techniques, it was judged suitable to measure temperature by NMR so that cancer diagnosis and treatment and evaluation of therapeutic effect might be incorporated into one system. This report dealt with concrete procedures of measuring the temperature of deep portions by NMR. Computations revealed that the coefficient of temperature of the thermal equilibrium magnetization was useful, that magnetic field focusing was the most effective imaging technique and that temperature rise in areas about 2 cm in radius could be measured without large errors. (Chiba, N.)

Ischemic stroke progress evaluation by {sup 31}P NMR-based metabonomic of human serum

Energy Technology Data Exchange (ETDEWEB)

Grandizoli, Caroline W.P.S.; Barison, Andersson, E-mail: andernmr@ufpr.br [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Departamento de Quimica. Centro de RMN; Lange, Marcos C.; Novak, Felipe T. M. [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Hospital de Clínicas. Divisao de Neurologia; Campos, Francinete R. [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Departmento de Farmacia

2014-07-01

In this work, chemometric analyses over {sup 31}P{"1"H} NMR (nuclear magnetic resonance) spectra of human blood serum permitted to discriminated ischemic stroke patients from health individuals due to changes in the chemical composition of phosphorus-containing compounds. These results indicate that {sup 31}P NMR-based metabonomic allowed insights over the mechanism triggered by ischemic stroke. (author)

Use of NMR as an online sensor in industrial processes

International Nuclear Information System (INIS)

Andrade, Fabiana Diuk de

2012-01-01

Nuclear magnetic resonance (NMR) is one of the most versatile analytical techniques for chemical, biochemical and medical applications. Despite this great success, NMR is seldom used as a tool in industrial applications. The first application of NMR in flowing samples was published in 1951. However, only in the last ten years Flow NMR has gained momentum and new and potential applications have been proposed. In this review we present the historical evolution of flow or online NMR spectroscopy and imaging, and current developments for use in the automation of industrial processes. (author)

Advances in Proteomic Techniques for Cytokine Analysis: Focus on Melanoma Research

Directory of Open Access Journals (Sweden)

Helena Kupcova Skalnikova

2017-12-01

Full Text Available Melanoma is a skin cancer with permanently increasing incidence and resistance to therapies in advanced stages. Reports of spontaneous regression and tumour infiltration with T-lymphocytes makes melanoma candidate for immunotherapies. Cytokines are key factors regulating immune response and intercellular communication in tumour microenvironment. Cytokines may be used in therapy of melanoma to modulate immune response. Cytokines also possess diagnostic and prognostic potential and cytokine production may reflect effects of immunotherapies. The purpose of this review is to give an overview of recent advances in proteomic techniques for the detection and quantification of cytokines in melanoma research. Approaches covered span from mass spectrometry to immunoassays for single molecule detection (ELISA, western blot, multiplex assays (chemiluminescent, bead-based (Luminex and planar antibody arrays, ultrasensitive techniques (Singulex, Simoa, immuno-PCR, proximity ligation/extension assay, immunomagnetic reduction assay, to analyses of single cells producing cytokines (ELISpot, flow cytometry, mass cytometry and emerging techniques for single cell secretomics. Although this review is focused mainly on cancer and particularly melanoma, the discussed techniques are in general applicable to broad research field of biology and medicine, including stem cells, development, aging, immunology and intercellular communication.

Advances in 27Al MAS NMR studies of geopolymers

Czech Academy of Sciences Publication Activity Database

Brus, Jiří; Abbrent, Sabina; Kobera, Libor; Urbanová, Martina; Cuba, P.

2016-01-01

Roč. 88, č. 2016 (2016), s. 79-147 ISSN 0066-4103 R&D Projects: GA ČR(CZ) GA13-24155S; GA MŠk(CZ) LO1507 Institutional support: RVO:61389013 Keywords : geopolymers * aluminosilicates * solid-state NMR Subject RIV: CD - Macromolecular Chemistry Impact factor: 2.600, year: 2016

C-13 NMR spectroscopy of plasma reduces interference of hypertriglyceridemia in the H-1 NMR detection of malignancy

International Nuclear Information System (INIS)

Fossell, E.T.; Hall, F.M.; McDonagh, J.

1991-01-01

The authors have previously described the application of water-suppressed proton nuclear magnetic resonance (H-1 NMR) spectroscopy of plasma for detection of malignancy. Subsequently, hypertriglyceridemia has been identified as a source of false positive results. Here is described a confirmatory, adjunctive technique -analysis of the carbon-13 (C-13) NMR spectrum of plasma- which also identifies the presence of malignancy but is not sensitive to the plasma triglyceride level. Blinded plasma samples from 480 normal donors and 208 patients scheduled for breast biopsy were analyzed by water-suppressed H-1 and C-13 NMR spectroscopy. Triglyceride levels were also measured. Among the normal donors, there were 38 individuals with hypertriglyceridemia of whom 18 had results consistent with malignancy by H-1 NMR spectroscopy. However, the C-13 technique reduced the apparent H-1 false positive rate from 7.0 to 0.6 percent. Similarly, in the breast biopsy cohort, C-13 reduced the false positive rate from 2.8 to 0.9 percent. Furthermore, the accuracy of the combined H-1/C-13 test in this blinded study was greater than 96 percent in 208 patients studied. (author). 27 refs.; 5 figs.; 4 tabs

Error characterization and quantum control benchmarking in liquid state NMR using quantum information processing techniques

Science.gov (United States)

Laforest, Martin

Quantum information processing has been the subject of countless discoveries since the early 1990's. It is believed to be the way of the future for computation: using quantum systems permits one to perform computation exponentially faster than on a regular classical computer. Unfortunately, quantum systems that not isolated do not behave well. They tend to lose their quantum nature due to the presence of the environment. If key information is known about the noise present in the system, methods such as quantum error correction have been developed in order to reduce the errors introduced by the environment during a given quantum computation. In order to harness the quantum world and implement the theoretical ideas of quantum information processing and quantum error correction, it is imperative to understand and quantify the noise present in the quantum processor and benchmark the quality of the control over the qubits. Usual techniques to estimate the noise or the control are based on quantum process tomography (QPT), which, unfortunately, demands an exponential amount of resources. This thesis presents work towards the characterization of noisy processes in an efficient manner. The protocols are developed from a purely abstract setting with no system-dependent variables. To circumvent the exponential nature of quantum process tomography, three different efficient protocols are proposed and experimentally verified. The first protocol uses the idea of quantum error correction to extract relevant parameters about a given noise model, namely the correlation between the dephasing of two qubits. Following that is a protocol using randomization and symmetrization to extract the probability that a given number of qubits are simultaneously corrupted in a quantum memory, regardless of the specifics of the error and which qubits are affected. Finally, a last protocol, still using randomization ideas, is developed to estimate the average fidelity per computational gates for

On advanced estimation techniques for exoplanet detection and characterization using ground-based coronagraphs

Science.gov (United States)

Lawson, Peter R.; Poyneer, Lisa; Barrett, Harrison; Frazin, Richard; Caucci, Luca; Devaney, Nicholas; Furenlid, Lars; Gładysz, Szymon; Guyon, Olivier; Krist, John; Maire, Jérôme; Marois, Christian; Mawet, Dimitri; Mouillet, David; Mugnier, Laurent; Pearson, Iain; Perrin, Marshall; Pueyo, Laurent; Savransky, Dmitry

2012-07-01

The direct imaging of planets around nearby stars is exceedingly difficult. Only about 14 exoplanets have been imaged to date that have masses less than 13 times that of Jupiter. The next generation of planet-finding coronagraphs, including VLT-SPHERE, the Gemini Planet Imager, Palomar P1640, and Subaru HiCIAO have predicted contrast performance of roughly a thousand times less than would be needed to detect Earth-like planets. In this paper we review the state of the art in exoplanet imaging, most notably the method of Locally Optimized Combination of Images (LOCI), and we investigate the potential of improving the detectability of faint exoplanets through the use of advanced statistical methods based on the concepts of the ideal observer and the Hotelling observer. We propose a formal comparison of techniques using a blind data challenge with an evaluation of performance using the Receiver Operating Characteristic (ROC) and Localization ROC (LROC) curves. We place particular emphasis on the understanding and modeling of realistic sources of measurement noise in ground-based AO-corrected coronagraphs. The work reported in this paper is the result of interactions between the co-authors during a week-long workshop on exoplanet imaging that was held in Squaw Valley, California, in March of 2012.

Automated Solid Phase Extraction (SPE) LC/NMR Applied to the Structural Analysis of Extractable Compounds from a Pharmaceutical Packaging Material of Construction.

Science.gov (United States)

Norwood, Daniel L; Mullis, James O; Davis, Mark; Pennino, Scott; Egert, Thomas; Gonnella, Nina C

2013-01-01

The structural analysis (i.e., identification) of organic chemical entities leached into drug product formulations has traditionally been accomplished with techniques involving the combination of chromatography with mass spectrometry. These include gas chromatography/mass spectrometry (GC/MS) for volatile and semi-volatile compounds, and various forms of liquid chromatography/mass spectrometry (LC/MS or HPLC/MS) for semi-volatile and relatively non-volatile compounds. GC/MS and LC/MS techniques are complementary for structural analysis of leachables and potentially leachable organic compounds produced via laboratory extraction of pharmaceutical container closure/delivery system components and corresponding materials of construction. Both hyphenated analytical techniques possess the separating capability, compound specific detection attributes, and sensitivity required to effectively analyze complex mixtures of trace level organic compounds. However, hyphenated techniques based on mass spectrometry are limited by the inability to determine complete bond connectivity, the inability to distinguish between many types of structural isomers, and the inability to unambiguously determine aromatic substitution patterns. Nuclear magnetic resonance spectroscopy (NMR) does not have these limitations; hence it can serve as a complement to mass spectrometry. However, NMR technology is inherently insensitive and its ability to interface with chromatography has been historically challenging. This article describes the application of NMR coupled with liquid chromatography and automated solid phase extraction (SPE-LC/NMR) to the structural analysis of extractable organic compounds from a pharmaceutical packaging material of construction. The SPE-LC/NMR technology combined with micro-cryoprobe technology afforded the sensitivity and sample mass required for full structure elucidation. Optimization of the SPE-LC/NMR analytical method was achieved using a series of model compounds

NMR studies of cerebral metabolism in vivo

International Nuclear Information System (INIS)

Prichard, J.W.

1986-01-01

The nature and extent of the potential synergism between PET and NMR methods is not yet well appreciated in the biomedical community. The long-range interest of medical neurobiology will be well served by efforts of PET and NMR scientists to follow each others' work so that opportunities for productive interchange can be efficiently exploited. Appreciation of the synergism by the rest of the biomedical community will follow naturally. PET is said by the people doing it to be still in its infancy, for they are more concerned with advancing their discipline than with admiring its already impressive achievements. On the scale of the same developmental metaphor, many NMR methods for studying the living human brain are still in utero. The best way to provide the reader a sense of the current status and future course of NMR research in medical neurobiology is by discussion of published in vivo studies. Such a discussion, adapted from another article is what follows

Isotope labeling for NMR studies of macromolecular structure and interactions

International Nuclear Information System (INIS)

Wright, P.E.

1994-01-01

Implementation of biosynthetic methods for uniform or specific isotope labeling of proteins, coupled with the recent development of powerful heteronuclear multidimensional NMR methods, has led to a dramatic increase in the size and complexity of macromolecular systems that are now amenable to NMR structural analysis. In recent years, a new technology has emerged that combines uniform 13 C, 15 N labeling with heteronuclear multidimensional NMR methods to allow NMR structural studies of systems approaching 25 to 30 kDa in molecular weight. In addition, with the introduction of specific 13 C and 15 N labels into ligands, meaningful NMR studies of complexes of even higher molecular weight have become feasible. These advances usher in a new era in which the earlier, rather stringent molecular weight limitations have been greatly surpassed and NMR can begin to address many central biological problems that involve macromolecular structure, dynamics, and interactions

Isotope labeling for NMR studies of macromolecular structure and interactions

Energy Technology Data Exchange (ETDEWEB)

Wright, P.E. [Scripps Research Institute, La Jolla, CA (United States)

1994-12-01

Implementation of biosynthetic methods for uniform or specific isotope labeling of proteins, coupled with the recent development of powerful heteronuclear multidimensional NMR methods, has led to a dramatic increase in the size and complexity of macromolecular systems that are now amenable to NMR structural analysis. In recent years, a new technology has emerged that combines uniform {sup 13}C, {sup 15}N labeling with heteronuclear multidimensional NMR methods to allow NMR structural studies of systems approaching 25 to 30 kDa in molecular weight. In addition, with the introduction of specific {sup 13}C and {sup 15}N labels into ligands, meaningful NMR studies of complexes of even higher molecular weight have become feasible. These advances usher in a new era in which the earlier, rather stringent molecular weight limitations have been greatly surpassed and NMR can begin to address many central biological problems that involve macromolecular structure, dynamics, and interactions.

The stereochemistry of the condensation product of salicylaldehyde and n-butylbarbituric acid by NMR techniques

Energy Technology Data Exchange (ETDEWEB)

Cruz, Elizabete R.; Villar, J. Daniel Figueroa [Instituto Militar de Engenharia (IME), Rio de Janeiro, RJ (Brazil). Dept. de Quimica

1995-12-31

Since the discovery of the 5-deazaflavin cofactor (coenzyme F{sub 420}) as a naturally occurring compound, a great attention has been focused on several iso steric flavin analogues. One of the simplest approaches towards the synthesis of oxadeazaflavin, compound which the nitrogen at the N-10 position of 5-deazaflavin is replaced by oxygen, is the direct condensation between barbituric acid and salicylaldehyde. In this paper, the use of some NMR techniques so as to determine the stereochemistry of the preformed isomer has been described and a possible mechanism for this isomerization discussed 12 refs., 2 figs., 1 tab.

A fragment separator at LBL for beta-NMR experiment

International Nuclear Information System (INIS)

Matsuta, K.; Ozawa, A.; Nojiri, Y.; Minamisono, T.; Fukuda, M.; Kitagawa, A.; Ohtsubo, T.; Momota, S.; Fukuda, S.; Matsuo, Y.; Takechi, H.; Minami, I.; Sugimoto, K.; Tanihata, I.; Omata, K.; Alonso, J.R.; Krebs, G.F.; Symons, T.J.M.

1992-03-01

The Beam 44 fragment separator was built at the Bevalac of LBL for NMR studies of beta emitting nuclei. 37 K, 39 Ca, and 43 Ti fragments originating from 40 Ca and 46 Ti primary beams were separated by the separator for NMR studies on these nuclei. Nuclear spin polarization was created in 39 Ca and 43 Ti using the tilted foil technique (TFT), and the magnetic moment of 43 Ti was deduced. Fragment polarization was measured for 37 K and 39 Ca emitted to finite deflection angles. The Beam 44 fragment separator in combination with a proper polarization technique, such as TFT or fragment polarization, has been very effective for such NMR studies

Skull base tumours part I: Imaging technique, anatomy and anterior skull base tumours

Energy Technology Data Exchange (ETDEWEB)

Borges, Alexandra [Instituto Portugues de Oncologia Francisco Gentil, Centro de Lisboa, Servico de Radiologia, Rua Professor Lima Basto, 1093 Lisboa Codex (Portugal)], E-mail: borgesalexandra@clix.pt

2008-06-15

Advances in cross-sectional imaging, surgical technique and adjuvant treatment have largely contributed to ameliorate the prognosis, lessen the morbidity and mortality of patients with skull base tumours and to the growing medical investment in the management of these patients. Because clinical assessment of the skull base is limited, cross-sectional imaging became indispensable in the diagnosis, treatment planning and follow-up of patients with suspected skull base pathology and the radiologist is increasingly responsible for the fate of these patients. This review will focus on the advances in imaging technique; contribution to patient's management and on the imaging features of the most common tumours affecting the anterior skull base. Emphasis is given to a systematic approach to skull base pathology based upon an anatomic division taking into account the major tissue constituents in each skull base compartment. The most relevant information that should be conveyed to surgeons and radiation oncologists involved in patient's management will be discussed.

Skull base tumours part I: Imaging technique, anatomy and anterior skull base tumours

International Nuclear Information System (INIS)

Borges, Alexandra

2008-01-01

Advances in cross-sectional imaging, surgical technique and adjuvant treatment have largely contributed to ameliorate the prognosis, lessen the morbidity and mortality of patients with skull base tumours and to the growing medical investment in the management of these patients. Because clinical assessment of the skull base is limited, cross-sectional imaging became indispensable in the diagnosis, treatment planning and follow-up of patients with suspected skull base pathology and the radiologist is increasingly responsible for the fate of these patients. This review will focus on the advances in imaging technique; contribution to patient's management and on the imaging features of the most common tumours affecting the anterior skull base. Emphasis is given to a systematic approach to skull base pathology based upon an anatomic division taking into account the major tissue constituents in each skull base compartment. The most relevant information that should be conveyed to surgeons and radiation oncologists involved in patient's management will be discussed

Direct Comparison of 19F qNMR and 1H qNMR by Characterizing Atorvastatin Calcium Content

Directory of Open Access Journals (Sweden)

Yang Liu

2016-01-01

Full Text Available Quantitative nuclear magnetic resonance (qNMR is a powerful tool in measuring drug content because of its high speed, sensitivity, and precision. Most of the reports were based on proton qNMR (1H qNMR and only a few fluorine qNMR (19F qNMR were reported. No research has been conducted to directly compare the advantage and disadvantage between these two methods. In the present study, both 19F and 1H qNMR were performed to characterize the content of atorvastatin calcium with the same internal standard. Linearity, precision, and results from two methods were compared. Results showed that 19F qNMR has similar precision and sensitivity to 1H qNMR. Both methods generate similar results compared to mass balance method. Major advantage from 19F qNMR is that the analyte signal is with less or no interference from impurities. 19F qNMR is an excellent approach to quantify fluorine-containing analytes.

A metal-ion NMR investigation of the antibiotic facilitated transport of monovalent cations through the walls of phospholipid vesicles. II. Sulfur-33 NMR

International Nuclear Information System (INIS)

Buster, D.C.

1988-01-01

A technique has been developed to investigate the antibiotic facilitated transmembrane transport of monovalent cations using 23 Na and 7 Li Nuclear Magnetic Resonance spectroscopy. The initial portion of this thesis outlines the production and characterization of a model lipid system amenable to the NMR detection of cation transport. Large unilamellar vesicles (LUV) have been prepared from a 4:1 mixture of phosphatidylcholine and phosphatidylglycerol. The presence of the anionic chemical shift reagent dysprosium (III) tripolyphosphate, either inside or outside of the vesicles, allows for the spectroscopic separation of the NMR resonances arising from the inter- and extravesicular cation pools. The cation transporting properties of the channel-forming pentadecapeptide, gramicidin D, have been studied using the NMR technique

Reducing acquisition times in multidimensional NMR with a time-optimized Fourier encoding algorithm

Energy Technology Data Exchange (ETDEWEB)

Zhang, Zhiyong [Department of Chemical Physics, Weizmann Institute of Science, Rehovot 76100 (Israel); Department of Electronic Science, Fujian Provincial Key Laboratory of Plasma and Magnetic Resonance, Xiamen University, Xiamen, Fujian 361005 (China); Smith, Pieter E. S.; Frydman, Lucio, E-mail: lucio.frydman@weizmann.ac.il [Department of Chemical Physics, Weizmann Institute of Science, Rehovot 76100 (Israel)

2014-11-21

Speeding up the acquisition of multidimensional nuclear magnetic resonance (NMR) spectra is an important topic in contemporary NMR, with central roles in high-throughput investigations and analyses of marginally stable samples. A variety of fast NMR techniques have been developed, including methods based on non-uniform sampling and Hadamard encoding, that overcome the long sampling times inherent to schemes based on fast-Fourier-transform (FFT) methods. Here, we explore the potential of an alternative fast acquisition method that leverages a priori knowledge, to tailor polychromatic pulses and customized time delays for an efficient Fourier encoding of the indirect domain of an NMR experiment. By porting the encoding of the indirect-domain to the excitation process, this strategy avoids potential artifacts associated with non-uniform sampling schemes and uses a minimum number of scans equal to the number of resonances present in the indirect dimension. An added convenience is afforded by the fact that a usual 2D FFT can be used to process the generated data. Acquisitions of 2D heteronuclear correlation NMR spectra on quinine and on the anti-inflammatory drug isobutyl propionic phenolic acid illustrate the new method's performance. This method can be readily automated to deal with complex samples such as those occurring in metabolomics, in in-cell as well as in in vivo NMR applications, where speed and temporal stability are often primary concerns.

Reducing acquisition times in multidimensional NMR with a time-optimized Fourier encoding algorithm

International Nuclear Information System (INIS)

Zhang, Zhiyong; Smith, Pieter E. S.; Frydman, Lucio

2014-01-01

Speeding up the acquisition of multidimensional nuclear magnetic resonance (NMR) spectra is an important topic in contemporary NMR, with central roles in high-throughput investigations and analyses of marginally stable samples. A variety of fast NMR techniques have been developed, including methods based on non-uniform sampling and Hadamard encoding, that overcome the long sampling times inherent to schemes based on fast-Fourier-transform (FFT) methods. Here, we explore the potential of an alternative fast acquisition method that leverages a priori knowledge, to tailor polychromatic pulses and customized time delays for an efficient Fourier encoding of the indirect domain of an NMR experiment. By porting the encoding of the indirect-domain to the excitation process, this strategy avoids potential artifacts associated with non-uniform sampling schemes and uses a minimum number of scans equal to the number of resonances present in the indirect dimension. An added convenience is afforded by the fact that a usual 2D FFT can be used to process the generated data. Acquisitions of 2D heteronuclear correlation NMR spectra on quinine and on the anti-inflammatory drug isobutyl propionic phenolic acid illustrate the new method's performance. This method can be readily automated to deal with complex samples such as those occurring in metabolomics, in in-cell as well as in in vivo NMR applications, where speed and temporal stability are often primary concerns

Influence of Freezing and Storage Procedure on Human Urine Samples in NMR-Based Metabolomics

OpenAIRE

Rist, Manuela; Muhle-Goll, Claudia; Görling, Benjamin; Bub, Achim; Heissler, Stefan; Watzl, Bernhard; Luy, Burkhard

2013-01-01

It is consensus in the metabolomics community that standardized protocols should be followed for sample handling, storage and analysis, as it is of utmost importance to maintain constant measurement conditions to identify subtle biological differences. The aim of this work, therefore, was to systematically investigate the influence of freezing procedures and storage temperatures and their effect on NMR spectra as a potentially disturbing aspect for NMR-based metabolomics studies. Urine sample...

Nanodisc-Targeted STD NMR Spectroscopy Reveals Atomic Details of Ligand Binding to Lipid Environments.

Science.gov (United States)

Muñoz-García, Juan C; Inacio Dos Reis, Rosana; Taylor, Richard J; Henry, Alistair J; Watts, Anthony

2018-05-18

Saturation transfer difference (STD) NMR spectroscopy is one of the most popular ligand-based NMR techniques for the study of protein-ligand interactions. This is due to its robustness and the fact that it is focused on the signals of the ligand, without any need for NMR information on the macromolecular target. This technique is most commonly applied to systems involving different types of ligands (e.g., small organic molecules, carbohydrates or lipids) and a protein as the target, in which the latter is selectively saturated. However, only a few examples have been reported where membrane mimetics are the macromolecular binding partners. Here, we have employed STD NMR spectroscopy to investigate the interactions of the neurotransmitter dopamine with mimetics of lipid bilayers, such as nanodiscs, by saturation of the latter. In particular, the interactions between dopamine and model lipid nanodiscs formed either from charged or zwitterionic lipids have been resolved at the atomic level. The results, in agreement with previous isothermal titration calorimetry studies, show that dopamine preferentially binds to negatively charged model membranes, but also provide detailed atomic insights into the mode of interaction of dopamine with membrane mimetics. Our findings provide relevant structural information for the design of lipid-based drug carriers of dopamine and its structural analogues and are of general applicability to other systems. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

First NMR Experiments in the Hybrid, 40T and beyond: A challenge to traditional NMR instrumentation

Science.gov (United States)

Reyes, Arneil P.

2001-03-01

The recent commissioning of the continuous 45T hybrid magnet at NHMFL has opened new horizon for science but carried with it new challenges that forced NMR spectroscopists to reevaluate the traditional approach to NMR instrumentation. Very recently, a world record frequency at 1.5GHz has been achieved, signaling the new era of NMR probe designs that may someday blur the distinction between the classic NMR and millimeter-wave spectroscopies. No longer can we ignore stray capacitances and exposed leads in the terrain where every millimeter of cable counts. The challenge brought about by ever increasing fields and consequently, frequency, requirements has stimulated ingenuity among scientists. This is eased by accelerated growth in RF communications and computing technologies that made available advanced devices with more speed, power, bandwidth, noise immunity, flexibility, and complexity in small space at very low costs. Utilization of these devices have been paramount consideration in cutting-edge designs at NHMFL for Condensed Matter NMR and will be described in this talk. I will also discuss a number of first >33T NMR experiments to date utilizing the strength of the field to expose, as well as to induce occurrence of, new physical phenomena in condensed matter and which resulted in better understanding of the physics of materials. This work has been a result of continuing collaboration with P. L Kuhns, W. G. Moulton, W. P. Halperin (NU), and W. G. Clark (UCLA). The NHMFL is supported through the National Science Foundation and the State of Florida.

Stripline-based microfluidic devices for high-resolution NMR spectroscopy

NARCIS (Netherlands)

Bart, J.

2009-01-01

A novel route towards microchip integrated NMR analysis was studied. For NMR analysis of mass-limited samples, research has focussed for decennia on microsolenoidal or planar helical detection coils on microfluidic substrates. Since these approaches suffer from static field distortion resulting in

Multiple acquisition of magic angle spinning solid-state NMR experiments using one receiver: Application to microcrystalline and membrane protein preparations

Science.gov (United States)

Gopinath, T.; Veglia, Gianluigi

2015-04-01

Solid-state NMR spectroscopy of proteins is a notoriously low-throughput technique. Relatively low-sensitivity and poor resolution of protein samples require long acquisition times for multidimensional NMR experiments. To speed up data acquisition, we developed a family of experiments called Polarization Optimized Experiments (POE), in which we utilized the orphan spin operators that are discarded in classical multidimensional NMR experiments, recovering them to allow simultaneous acquisition of multiple 2D and 3D experiments, all while using conventional probes with spectrometers equipped with one receiver. POE allow the concatenation of multiple 2D or 3D pulse sequences into a single experiment, thus potentially combining all of the aforementioned advances, boosting the capability of ssNMR spectrometers at least two-fold without the addition of any hardware. In this perspective, we describe the first generation of POE, such as dual acquisition MAS (or DUMAS) methods, and then illustrate the evolution of these experiments into MEIOSIS, a method that enables the simultaneous acquisition of multiple 2D and 3D spectra. Using these new pulse schemes for the solid-state NMR investigation of biopolymers makes it possible to obtain sequential resonance assignments, as well as distance restraints, in about half the experimental time. While designed for acquisition of heteronuclei, these new experiments can be easily implemented for proton detection and coupled with other recent advancements, such as dynamic nuclear polarization (DNP), to improve signal to noise. Finally, we illustrate the application of these methods to microcrystalline protein preparations as well as single and multi-span membrane proteins reconstituted in lipid membranes.

Application of Solution NMR Spectroscopy to Study Protein Dynamics

Directory of Open Access Journals (Sweden)

Christoph Göbl

2012-03-01

Full Text Available Recent advances in spectroscopic methods allow the identification of minute fluctuations in a protein structure. These dynamic properties have been identified as keys to some biological processes. The consequences of this structural flexibility can be far‑reaching and they add a new dimension to the structure-function relationship of biomolecules. Nuclear Magnetic Resonance (NMR spectroscopy allows the study of structure as well as dynamics of biomolecules in a very broad range of timescales at atomic level. A number of new NMR methods have been developed recently to allow the measurements of time scales and spatial fluctuations, which in turn provide the thermodynamics associated with the biological processes. Since NMR parameters reflect ensemble measurements, structural ensemble approaches in analyzing NMR data have also been developed. These new methods in some instances can even highlight previously hidden conformational features of the biomolecules. In this review we describe several solution NMR methods to study protein dynamics and discuss their impact on important biological processes.

Automatic 1H-NMR Screening of Fatty Acid Composition in Edible Oils

Directory of Open Access Journals (Sweden)

David Castejón

2016-02-01

Full Text Available In this work, we introduce an NMR-based screening method for the fatty acid composition analysis of edible oils. We describe the evaluation and optimization needed for the automated analysis of vegetable oils by low-field NMR to obtain the fatty acid composition (FAC. To achieve this, two scripts, which automatically analyze and interpret the spectral data, were developed. The objective of this work was to drive forward the automated analysis of the FAC by NMR. Due to the fact that this protocol can be carried out at low field and that the complete process from sample preparation to printing the report only takes about 3 min, this approach is promising to become a fundamental technique for high-throughput screening. To demonstrate the applicability of this method, the fatty acid composition of extra virgin olive oils from various Spanish olive varieties (arbequina, cornicabra, hojiblanca, manzanilla, and picual was determined by 1H-NMR spectroscopy according to this protocol.

{sup 1}H NMR-based metabolomics of time-dependent responses of Eisenia fetida to sub-lethal phenanthrene exposure

Energy Technology Data Exchange (ETDEWEB)

Lankadurai, Brian P.; Wolfe, David M.; Simpson, Andre J. [Department of Chemistry, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4 Canada (Canada); Simpson, Myrna J., E-mail: myrna.simpson@utoronto.ca [Department of Chemistry, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4 Canada (Canada)

2011-10-15

{sup 1}H NMR-based metabolomics was used to examine the response of the earthworm Eisenia fetida after exposure to sub-lethal concentrations of phenanthrene over time. Earthworms were exposed to 0.025 mg/cm{sup 2} of phenanthrene (1/64th of the LC{sub 50}) via contact tests over four days. Earthworm tissues were extracted using a mixture of chloroform, methanol and water, resulting in polar and non-polar fractions that were analyzed by {sup 1}H NMR after one, two, three and four days. NMR-based metabolomic analyses revealed heightened E. fetida responses with longer phenanthrene exposure times. Amino acids alanine and glutamate, the sugar maltose, the lipids cholesterol and phosphatidylcholine emerged as potential indicators of phenanthrene exposure. The conversion of succinate to fumarate in the Krebs cycle was also interrupted by phenanthrene. Therefore, this study shows that NMR-based metabolomics is a powerful tool for elucidating time-dependent relationships in addition to the mode of toxicity of phenanthrene in earthworm exposure studies. - Highlights: > NMR-based earthworm metabolomic analysis of the mode of action of phenanthrene is presented. > The earthworm species E. fetida were exposed to sub-lethal phenanthrene concentrations. > Both polar and non-polar metabolites of E. fetida tissue extracts were analyzed by {sup 1}H NMR. > Longer phenanthrene exposure times resulted in heightened earthworm responses. > An interruption of the Krebs cycle was also observed due to phenanthrene exposure. - {sup 1}H NMR metabolomics is used to determine the relationship between phenanthrene exposure and the metabolic response of the earthworm E. fetida over time and also to elucidate the phenanthrene mode of toxicity.

Teaching advanced wound closure techniques using cattle digits.

Science.gov (United States)

Khalil, Philipe N; Kanz, Karl-Georg; Siebeck, Matthias; Mutschler, Wolf

2011-03-01

To evaluate a model used to impart advanced wound closure skills because available models do not meet the necessary requirements to a substantial degree. Seventy-one residents were asked to evaluate a 75-minute-long skills course using cadaveric cattle digits to learn Z-plasty, V-Y-plasty, and oval-shaped rotational flaps. A short film and the course instructor demonstrated each technique first. A Likert rating scale ranging from 1 to 6 was used for questions in the survey given to the residents. There was strong agreement among residents (1.65 ± 1.17 years of experience) that advanced wound closure training courses are necessary (5.73 ± 0.73), which corresponded to the residents' low level of knowledge and self-assessment of practical skills and present experience (2.84 ± 1.01). The course was evaluated with high acceptance, even though it was found to be demanding for the trainees (5.84 ± 0.40). This might also be related to the high rating of the model itself, which was found to be a suitable method for teaching advanced wound closure techniques (5.50 ± 0.71) that was easily comprehensible (5.73 ± 0.53). Skills training courses for young trainees are warranted to impart advanced wound closure techniques. The curriculum using cattle digits presented here is recommended. The authors have indicated no significant interest with commercial supporters. © 2011 by the American Society for Dermatologic Surgery, Inc.

(S)Pinning down protein interactions by NMR

DEFF Research Database (Denmark)

Teilum, Kaare; Kunze, Micha Ben Achim; Erlendsson, Simon

2017-01-01

Protein molecules are highly diverse communication platforms and their interaction repertoire stretches from atoms over small molecules such as sugars and lipids to macromolecules. An important route to understanding molecular communication is to quantitatively describe their interactions...... all types of protein reactions, which can span orders of magnitudes in affinities, reaction rates and lifetimes of states. As the more versatile technique, solution NMR spectroscopy offers a remarkable catalogue of methods that can be successfully applied to the quantitative as well as qualitative...... descriptions of protein interactions. In this review we provide an easy-access approach to NMR for the non-NMR specialist and describe how and when solution state NMR spectroscopy is the method of choice for addressing protein ligand interaction. We describe very briefly the theoretical background...

Proceedings of the symposium on advanced measurement techniques and instrumentation: abstract book

International Nuclear Information System (INIS)

Kale, Y.B.; Kushwaha, M.; Somkuwar, S.P.; Ajayakumar, S.; Sampathkumar, R.

2011-01-01

In order to consolidate the existing knowledge base and further to focus on the future directions of the field of advanced measurement techniques and instrumentation, Bhabha Atomic Research Centre has organized a three-day symposium on 'Advanced Measurement Techniques and Instrumentation' at Multi Purpose Hall, Training School Hostel, Anushaktinagar, Mumbai during February 02-04, 2011. The symposium is aimed at providing a forum to discuss the emerging trends and challenges ahead in the important area of measurement science and technology. This is a unique symposium, which brings together scientists and engineers from all disciplines and provides them a platform for close interaction to exchange ideas, methodologies and expertise, which is extremely important for synergic growth of this field. The symposium consists of 27 talks, which include keynote address, plenary and invited talks, and 63 contributory papers. The abstracts of these papers are brought to you in this volume. Readers may observe that the scientific programme of the symposium covers a wide ranging issues including advanced scientific concepts in measurements, instrumentation strategies, mathematical techniques and development of devices for applications in fundamental physics, astrophysics, fusion plasmas, nuclear reactors, accelerators, environment, chemical and biological sciences, and national security. Papers relevant to INIS are indexed separately

Principles of high resolution NMR in solids

CERN Document Server

Mehring, Michael

1983-01-01

The field of Nuclear Magnetic Resonance (NMR) has developed at a fascinating pace during the last decade. It always has been an extremely valuable tool to the organic chemist by supplying molecular "finger print" spectra at the atomic level. Unfortunately the high resolution achievable in liquid solutions could not be obtained in solids and physicists and physical chemists had to live with unresolved lines open to a wealth of curve fitting procedures and a vast amount of speculations. High resolution NMR in solids seemed to be a paradoxon. Broad structure­ less lines are usually encountered when dealing with NMR in solids. Only with the recent advent of mUltiple pulse, magic angle, cross-polarization, two-dimen­ sional and multiple-quantum spectroscopy and other techniques during the last decade it became possible to resolve finer details of nuclear spin interactions in solids. I have felt that graduate students, researchers and others beginning to get involved with these techniques needed a book which trea...

Comparative NMR investigation of the Re-based borides

Science.gov (United States)

Lue, C. S.; Tao, Y. F.; Su, T. H.

2008-07-01

We report a systematic study of the rhenium-based borides, ReB2 , Re7B3 , and Re3B , by means of the B11 nuclear magnetic resonance (NMR) spectroscopy. While Re7B3 and Re3B are superconductors, ReB2 exhibits no superconducting signature but is of current interest due to its superhard mechanical property. Since the major focus of this investigation is their electronic characteristics in the normal states, we performed the measurements at temperatures between 77 and 295 K. For Re7B3 and Re3B , s -character electrons were found to be responsible for the observed B11 NMR Knight shift and spin-lattice relaxation rate (1/T1) . From T1 analysis, we thus deduce the partial Bs Fermi-level density of states (DOS) of both borides. On the other hand, the relaxation rate of ReB2 is mainly associated with p electrons, similar to the cases of OsB2 and RuB2 . In addition, the extracted B2p Fermi-level DOS is in good agreement with the theoretical prediction from band-structure calculations.

A neutron-X-ray, NMR and calorimetric study of glassy Probucol synthesized using containerless techniques

International Nuclear Information System (INIS)

Weber, J.K.R.; Benmore, C.J.; Tailor, A.N.; Tumber, S.K.; Neuefeind, J.; Cherry, B.; Yarger, J.L.; Mou, Q.; Weber, W.; Byrn, S.R.

2013-01-01

Highlights: • Acoustic levitation was used to make phase-pure glassy forms of pharmaceutical compounds. • Neutrons, X-rays and NMR were used to characterize the glasses. • The glass comprised of slightly distorted molecules packed in a random network. • Potential for new drug synthesis routes is discussed. - Abstract: Acoustic levitation was used to trap 1–3 mm diameter drops of Probucol and other pharmaceutical materials in containerless conditions. Samples were studied in situ using X-ray diffraction and ex situ using neutron diffraction, NMR and DSC techniques. The materials were brought into non-equilibrium states by supersaturating solutions or by supercooling melts. The glass transition and crystallization temperatures of glassy Probucol were 29 ± 1 and 71 ± 1 °C respectively. The glassy form was stable with a shelf life of at least 8 months. A neutron/X-ray difference function of the glass showed that while molecular sub-groups remain rigid, many of the hydrogen correlations observed in the crystal become smeared out in the disordered material. The glass is principally comprised of slightly distorted Form I Probucol molecules with disordered packing rather than large changes in the individual molecular structure. Avoiding surface contact-induced nucleation provided access to highly non-equilibrium phases and enabled synthesis of phase-pure glasses

A neutron-X-ray, NMR and calorimetric study of glassy Probucol synthesized using containerless techniques

Energy Technology Data Exchange (ETDEWEB)

Weber, J.K.R., E-mail: rweber@anl.gov [Materials Development, Inc., Arlington Heights, IL 60004 (United States); Argonne National Laboratory, Argonne, IL 60439 (United States); Benmore, C.J. [Argonne National Laboratory, Argonne, IL 60439 (United States); Department of Physics, Arizona State University, AZ 85287 (United States); Tailor, A.N.; Tumber, S.K. [Materials Development, Inc., Arlington Heights, IL 60004 (United States); Neuefeind, J. [Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States); Cherry, B. [Magnetic Resonance Research Center, Arizona State University, AZ 85287 (United States); Department of Chemistry and Biochemistry, Arizona State University, AZ 85287 (United States); Yarger, J.L. [Department of Physics, Arizona State University, AZ 85287 (United States); Magnetic Resonance Research Center, Arizona State University, AZ 85287 (United States); Department of Chemistry and Biochemistry, Arizona State University, AZ 85287 (United States); Mou, Q. [Magnetic Resonance Research Center, Arizona State University, AZ 85287 (United States); Department of Chemistry and Biochemistry, Arizona State University, AZ 85287 (United States); Weber, W. [Department of Physics, Arizona State University, AZ 85287 (United States); Department of Chemistry and Biochemistry, Arizona State University, AZ 85287 (United States); Byrn, S.R. [Department of Industrial and Physical Pharmacy, Purdue University, IN 47907 (United States)

2013-10-16

Highlights: • Acoustic levitation was used to make phase-pure glassy forms of pharmaceutical compounds. • Neutrons, X-rays and NMR were used to characterize the glasses. • The glass comprised of slightly distorted molecules packed in a random network. • Potential for new drug synthesis routes is discussed. - Abstract: Acoustic levitation was used to trap 1–3 mm diameter drops of Probucol and other pharmaceutical materials in containerless conditions. Samples were studied in situ using X-ray diffraction and ex situ using neutron diffraction, NMR and DSC techniques. The materials were brought into non-equilibrium states by supersaturating solutions or by supercooling melts. The glass transition and crystallization temperatures of glassy Probucol were 29 ± 1 and 71 ± 1 °C respectively. The glassy form was stable with a shelf life of at least 8 months. A neutron/X-ray difference function of the glass showed that while molecular sub-groups remain rigid, many of the hydrogen correlations observed in the crystal become smeared out in the disordered material. The glass is principally comprised of slightly distorted Form I Probucol molecules with disordered packing rather than large changes in the individual molecular structure. Avoiding surface contact-induced nucleation provided access to highly non-equilibrium phases and enabled synthesis of phase-pure glasses.

Quartz Crystal Temperature Sensor for MAS NMR

Science.gov (United States)

Simon, Gerald

1997-10-01

Quartz crystal temperature sensors (QCTS) were tested for the first time as wireless thermometers in NMR MAS rotors utilizing the NMR RF technique itself for exiting and receiving electro-mechanical quartz resonances. This new tool in MAS NMR has a high sensitivity, linearity, and precision. When compared to the frequently used calibration of the variable temperature in the NMR system by a solid state NMR chemical shift thermometer (CST), such as lead nitrate, QCTS shows a number of advantages. It is an inert thermometer in close contact with solid samples operating parallel to the NMR experiment. QCTS can be manufactured for any frequency to be near a NMR frequency of interest (typically 1 to 2 MHz below or above). Due to the strong response of the crystal, signal detection is possible without changing the tuning of the MAS probe. The NMR signal is not influenced due to the relative sharp crystal resonance, restricted excitation by finite pulses, high probeQvalues, and commonly used audio filters. The quadratic dependence of the temperature increase on spinning speed is the same for the QCTS and for the CST lead nitrate and is discussed in terms of frictional heat in accordance with the literature about lead nitrate and with the results of a simple rotor speed jump experiment with differently radial located lead nitrate in the rotor.

Global host metabolic response to Plasmodium vivax infection: a 1H NMR based urinary metabonomic study

Directory of Open Access Journals (Sweden)

Sengupta Arjun

2011-12-01

Full Text Available Abstract Background Plasmodium vivax is responsible for the majority of malarial infection in the Indian subcontinent. This species of the parasite is generally believed to cause a relatively benign form of the disease. However, recent reports from different parts of the world indicate that vivax malaria can also have severe manifestation. Host response to the parasite invasion is thought to be an important factor in determining the severity of manifestation. In this paper, attempt was made to determine the host metabolic response associated with P. vivax infection by means of NMR spectroscopy-based metabonomic techniques in an attempt to better understand the disease pathology. Methods NMR spectroscopy of urine samples from P. vivax-infected patients, healthy individuals and non-malarial fever patients were carried out followed by multivariate statistical analysis. Two data analysis techniques were employed, namely, Principal Component Analysis [PCA] and Orthogonal Projection to Latent Structure Discriminant Analysis [OPLS-DA]. Several NMR signals from the urinary metabolites were further selected for univariate comparison among the classes. Results The urine metabolic profiles of P. vivax-infected patients were distinct from those of healthy individuals as well as of non-malarial fever patients. A highly predictive model was constructed from urine profile of malarial and non-malarial fever patients. Several metabolites were found to be varying significantly across these cohorts. Urinary ornithine seems to have the potential to be used as biomarkers of vivax malaria. An increasing trend in pipecolic acid was also observed. The results suggest impairment in the functioning of liver as well as impairment in urea cycle. Conclusions The results open up a possibility of non-invasive analysis and diagnosis of P. vivax using urine metabolic profile. Distinct variations in certain metabolites were recorded, and amongst these, ornithine may have the

Thin film characterisation by advanced X-ray diffraction techniques

International Nuclear Information System (INIS)

Cappuccio, G.; Terranova, M.L.

1996-09-01

The Fifth School on X-ray diffraction from polycrystalline materials was devoted to thin film characterization by advanced X-ray diffraction techniques. Twenty contributions are contained in this volume; all twenty are recorded in the INIS Database. X-ray diffraction is known to be a powerful analytical tool for characterizing materials and understanding their structural features. The aim of these articles is to illustrate the fundamental contribution of modern diffraction techniques (grazing incidence, surface analysis, standing waves, etc.) to the characterization of thin and ultra-thin films, which have become important in many advanced technologies

Final Report: Characterization of Hydrogen Adsorption in Carbon-Based Materials by NMR

International Nuclear Information System (INIS)

Wu, Yue; Kleinhammes, Alfred

2011-01-01

In support of DOE/EERE's Fuel Cell Technologies Program Hydrogen Sorption Center of Excellence (HSCoE), UNC conducted Nuclear Magnetic Resonance (NMR) measurements that contributed spectroscopic information as well as quantitative analysis of adsorption processes. While NMR based Langmuir isotherms produce reliable H2 capacity measurements, the most astute contribution to the center is provided by information on dihydrogen adsorption on the scale of nanometers, including the molecular dynamics of hydrogen in micropores, and the diffusion of dihydrogen between macro and micro pores. A new method to assess the pore width using H2 as probe of the pore geometry was developed and is based on the variation of the observed chemical shift of adsorbed dihydrogen as function of H2 pressure. Adsorbents designed and synthesized by the Center were assessed for their H2 capacity, the binding energy of the adsorption site, their pore structure and their ability to release H2. Feedback to the materials groups was provided to improve the materials properties. To enable in situ NMR measurements as a function of H2 pressure and temperature, a unique, specialized NMR system was designed and built. Pressure can be varied between 10-4 and 107 Pa while the temperature can be controlled between 77K and room temperature. In addition to the 1H investigation of the H2 adsorption process, NMR was implemented to measure the atomic content of substituted elements, e.g. boron in boron substituted graphitic material as well as to determine the local environment and symmetry of these substituted nuclei. The primary findings by UNC are the following: (1) Boron substituted for carbon in graphitic material in the planar BC3 configuration enhances the binding energy for adsorbed hydrogen; (2) Arrested kinetics of H2 was observed below 130K in the same boron substituted carbon samples that combine enhanced binding energy with micropore structure; (3) Hydrogen storage material made from activated PEEK

Final Report: Characterization of Hydrogen Adsorption in Carbon-Based Materials by NMR

Energy Technology Data Exchange (ETDEWEB)

Wu, Yue; Kleinhammes, Alfred

2011-07-11

In support of DOE/EERE's Fuel Cell Technologies Program Hydrogen Sorption Center of Excellence (HSCoE), UNC conducted Nuclear Magnetic Resonance (NMR) measurements that contributed spectroscopic information as well as quantitative analysis of adsorption processes. While NMR based Langmuir isotherms produce reliable H2 capacity measurements, the most astute contribution to the center is provided by information on dihydrogen adsorption on the scale of nanometers, including the molecular dynamics of hydrogen in micropores, and the diffusion of dihydrogen between macro and micro pores. A new method to assess the pore width using H2 as probe of the pore geometry was developed and is based on the variation of the observed chemical shift of adsorbed dihydrogen as function of H2 pressure. Adsorbents designed and synthesized by the Center were assessed for their H2 capacity, the binding energy of the adsorption site, their pore structure and their ability to release H2. Feedback to the materials groups was provided to improve the materials’ properties. To enable in situ NMR measurements as a function of H2 pressure and temperature, a unique, specialized NMR system was designed and built. Pressure can be varied between 10-4 and 107 Pa while the temperature can be controlled between 77K and room temperature. In addition to the 1H investigation of the H2 adsorption process, NMR was implemented to measure the atomic content of substituted elements, e.g. boron in boron substituted graphitic material as well as to determine the local environment and symmetry of these substituted nuclei. The primary findings by UNC are the following: • Boron substituted for carbon in graphitic material in the planar BC3 configuration enhances the binding energy for adsorbed hydrogen. • Arrested kinetics of H2 was observed below 130K in the same boron substituted carbon samples that combine enhanced binding energy with micropore structure. • Hydrogen storage material made from

Image restoration from non-uniform magnetic field influence for direct Fourier NMR imaging

International Nuclear Information System (INIS)

Sekihara, K.; Kuroda, M.; Kohno, H.

1984-01-01

A new technique is proposed for NMR image restoration from the influence of main magnetic field non-uniformities. This technique is applicable to direct Fourier NMR imaging. The mathematical basis and details of this technique are fully described. Modification to include image restoration from non-linear field gradient influence is also presented. Computer simulation demonstrates the effectiveness of this technique for both Fourier zeugmatography and spin-warp imaging. (author)

WaVPeak: Picking NMR peaks through wavelet-based smoothing and volume-based filtering

KAUST Repository

Liu, Zhi; Abbas, Ahmed; Jing, Bing-Yi; Gao, Xin

2012-01-01

Motivation: Nuclear magnetic resonance (NMR) has been widely used as a powerful tool to determine the 3D structures of proteins in vivo. However, the post-spectra processing stage of NMR structure determination usually involves a tremendous amount

The fluorescence properties and NMR analysis of protopine and allocryptopine

International Nuclear Information System (INIS)

Kubala, Martin; Vacek, Jan; Popa, Igor; Janovska, Marika; Kosina, Pavel; Ulrichova, Jitka; Travnicek, Zdenek; Simanek, Vilim

2011-01-01

The fluorescence properties of protopine and allocryptopine in aqueous and organic environments are described for the first time. The fluorescence of alkaloids and their pH-dependent interconversion to cationic forms (transannular interaction) were studied using steady-state and time-resolved fluorescence techniques. For the analysis of tricyclic base and cis/trans tetracyclic cations of the alkaloids, NMR and X-ray crystallography were used. - Highlights: → We describe fundamental fluorescence characteristics of alkaloids protopine and allocryptopine. → We analyzed the pH-dependent transitions and cis/trans isomerization. → These two alkaloids can be better distinguished by their fluorescence decay characteristics. → The fluorescence parameters are related to the NMR and crystallographic structural data.

Impact of advanced MRI techniques for the diagnosis of dementia: comparison with PET

DEFF Research Database (Denmark)

Steffensen, Elena; Prakash, Vineet; Vestergård, Karsten

Introduction: The use of high magnetic fields in combination with fast algorithms for computer-based postprocessing has moved advanced MRI techniques into clinical practice. MRI provides in analogy with PET physiological information in addition to more traditional morphological images. Evaluation...... with suspected Alzheimer's disease (AD); 4 with suspected frontotemporal dementia (FTD), and 2 were found normal. Mean FA and ADC values in cingulum and in CC for the patient group compared with controls are presented in Table 1. ADC values in CC were higher comparing with controls and higher for patients...... with suspected FTD than for patients with suspected AD. Conclusion: CBF measurements and characteristics obtained by advanced MRI techniques have a potential to facilitate early diagnosis and understanding of dementia....

A Toolbox of Solid-State NMR Experiments for the Characterization of Soft Organic Nanomaterials

KAUST Repository

Straasø, Lasse Arnt

2016-02-02

Determining how organic molecules self-assemble into a solid material is a challenging and demanding task if a single crystal of the material cannot be produced. Solid-state NMR spectroscopy offers access to such molecular details via an appropriate selection of techniques. This report gives a selected overview of 1D and 2D solid-state NMR techniques for elucidating the structure of soft organic solids. We focus on how the solid-state NMR techniques are designed from the perspective of the different nuclear interactions, using average Hamiltonian theory and product operators. We also introduce recent methods for quantification and reduction of experimental artifacts. Finally, we highlight how the solid-state NMR techniques can be applied to soft organic materials by reviewing recent applications to semicrystalline polymers, π-conjugated polymers, natural silk, and graphene-related materials.

A Toolbox of Solid-State NMR Experiments for the Characterization of Soft Organic Nanomaterials

KAUST Repository

Straasø , Lasse Arnt; Saleem, Qasim; Hansen, Michael Ryan

2016-01-01

Determining how organic molecules self-assemble into a solid material is a challenging and demanding task if a single crystal of the material cannot be produced. Solid-state NMR spectroscopy offers access to such molecular details via an appropriate selection of techniques. This report gives a selected overview of 1D and 2D solid-state NMR techniques for elucidating the structure of soft organic solids. We focus on how the solid-state NMR techniques are designed from the perspective of the different nuclear interactions, using average Hamiltonian theory and product operators. We also introduce recent methods for quantification and reduction of experimental artifacts. Finally, we highlight how the solid-state NMR techniques can be applied to soft organic materials by reviewing recent applications to semicrystalline polymers, π-conjugated polymers, natural silk, and graphene-related materials.

Workshop on High-Field NMR and Biological Applications

Science.gov (United States)

Scientists at the Pacific Northwest Laboratory have been working toward the establishment of a new Molecular Science Research Center (MSRC). The primary scientific thrust of this new research center is in the areas of theoretical chemistry, chemical dynamics, surface and interfacial science, and studies on the structure and interactions of biological macromolecules. The MSRC will provide important new capabilities for studies on the structure of biological macromolecules. The MSRC program includes several types of advanced spectroscopic techniques for molecular structure analysis, and a theory and modeling laboratory for molecular mechanics/dynamics calculations and graphics. It is the goal to closely integrate experimental and theoretical studies on macromolecular structure, and to join these research efforts with those of the molecular biological programs to provide new insights into the structure/function relationships of biological macromolecules. One of the areas of structural biology on which initial efforts in the MSRC will be focused is the application of high field, 2-D NMR to the study of biological macromolecules. First, there is interest in obtaining 3-D structural information on large proteins and oligonucleotides. Second, one of the primary objectives is to closely link theoretical approaches to molecular structure analysis with the results obtained in experimental research using NMR and other spectroscopies.

New Computational Approaches for NMR-based Drug Design: A Protocol for Ligand Docking to Flexible Target Sites

International Nuclear Information System (INIS)

Gracia, Luis; Speidel, Joshua A.; Weinstein, Harel

2006-01-01

NMR-based drug design has met with some success in the last decade, as illustrated in numerous instances by Fesik's ''ligand screening by NMR'' approach. Ongoing efforts to generalize this success have led us to the development of a new paradigm in which quantitative computational approaches are being integrated with NMR derived data and biological assays. The key component of this work is the inclusion of the intrinsic dynamic quality of NMR structures in theoretical models and its use in docking. A new computational protocol is introduced here, designed to dock small molecule ligands to flexible proteins derived from NMR structures. The algorithm makes use of a combination of simulated annealing monte carlo simulations (SA/MC) and a mean field potential informed by the NMR data. The new protocol is illustrated in the context of an ongoing project aimed at developing new selective inhibitors for the PCAF bromodomains that interact with HIV Tat

Characterization of nylon 6/poly(propylene oxide) polymeric mixture by combined NMR techniques

International Nuclear Information System (INIS)

Costa, Dilma Alves; Oliveira, Clara Marize F.; Tavares, Maria Ines B.

1995-01-01

Polymeric mixtures aim to improve physical or chemical properties of materials. This mixtures can be compatible or not. The compatibility between polymers determine changes of properties. This work has presented a detailed study where nylon 6 and poly(propylene oxide) mixture was analysed by 13 C NMR in the solid state, and NMR spectra were shown and explained. The molecular mobility as well as the compatibility have been observed and discussed

Advances in stable isotope assisted labeling strategies with information science.

Science.gov (United States)

Kigawa, Takanori

2017-08-15

Stable-isotope (SI) labeling of proteins is an essential technique to investigate their structures, interactions or dynamics by nuclear magnetic resonance (NMR) spectroscopy. The assignment of the main-chain signals, which is the fundamental first step in these analyses, is usually achieved by a sequential assignment method based on triple resonance experiments. Independently of the triple resonance experiment-based sequential assignment, amino acid-selective SI labeling is beneficial for discriminating the amino acid type of each signal; therefore, it is especially useful for the signal assignment of difficult targets. Various combinatorial selective labeling schemes have been developed as more sophisticated labeling strategies. In these strategies, amino acids are represented by combinations of SI labeled samples, rather than simply assigning one amino acid to one SI labeled sample as in the case of conventional amino acid-selective labeling. These strategies have proven to be useful for NMR analyses of difficult proteins, such as those in large complex systems, in living cells, attached or integrated into membranes, or with poor solubility. In this review, recent advances in stable isotope assisted labeling strategies will be discussed. Copyright © 2017 Elsevier Inc. All rights reserved.

Fundamentals and advanced techniques in derivatives hedging

CERN Document Server

Bouchard, Bruno

2016-01-01

This book covers the theory of derivatives pricing and hedging as well as techniques used in mathematical finance. The authors use a top-down approach, starting with fundamentals before moving to applications, and present theoretical developments alongside various exercises, providing many examples of practical interest. A large spectrum of concepts and mathematical tools that are usually found in separate monographs are presented here. In addition to the no-arbitrage theory in full generality, this book also explores models and practical hedging and pricing issues. Fundamentals and Advanced Techniques in Derivatives Hedging further introduces advanced methods in probability and analysis, including Malliavin calculus and the theory of viscosity solutions, as well as the recent theory of stochastic targets and its use in risk management, making it the first textbook covering this topic. Graduate students in applied mathematics with an understanding of probability theory and stochastic calculus will find this b...

NMR of geophysical drill cores with a mobile Halbach scanner

International Nuclear Information System (INIS)

Talnishnikh, E.

2007-01-01

This thesis is devoted to a mobile NMR with an improved Halbach scanner. This is a lightweight tube-shaped magnet with sensitive volume larger and a homogeneity of the magnetic field higher than the previous prototype version. The improved Halbach scanner is used for analysis of water-saturated drill cores and plugs with diameters up to 60 mm. To provide the analysis, the standard 1D technique with the CPMG sequence as well as 2D correlation experiments were successfully applied and adapted to study properties of fluid-saturated sediments. Afterwards the Halbach scanner was calibrated to fast non-destructive measurements of porosity, relaxation time distributions, and estimation of permeability. These properties can be calculated directly from the NMR data using the developed methodology. Any independent measurements of these properties with other methods are not needed. One of the main results of this work is the development of a new NMR on-line core scanner for measurements of porosity in long cylindrical and semi cylindrical drill cores. Also dedicated software was written to operate the NMR on-line core scanner. The physical background of this work is the study of the diffusion influence on transverse relaxation. The diffusion effect in the presence of internal gradients in porous media was probed by 1D and 2D experiments. The transverse relaxation time distributions obtained from 1D and from 2D experiments are comparable but different in fine details. Two new methodologies were developed based on the results of this study. First is the methodology quantifying the influence of diffusion in the internal gradients of water-saturated sediments on transverse relaxation from 2D correlation experiments. The second one is the correction of the permeability estimation from the NMR data taking in account the influence of the diffusion. Furthermore, PFG NMR technique was used to study restricted diffusion in the same kind of samples. Preliminary results are reported

NMR of geophysical drill cores with a mobile Halbach scanner

Energy Technology Data Exchange (ETDEWEB)

Talnishnikh, E.

2007-08-21

This thesis is devoted to a mobile NMR with an improved Halbach scanner. This is a lightweight tube-shaped magnet with sensitive volume larger and a homogeneity of the magnetic field higher than the previous prototype version. The improved Halbach scanner is used for analysis of water-saturated drill cores and plugs with diameters up to 60 mm. To provide the analysis, the standard 1D technique with the CPMG sequence as well as 2D correlation experiments were successfully applied and adapted to study properties of fluid-saturated sediments. Afterwards the Halbach scanner was calibrated to fast non-destructive measurements of porosity, relaxation time distributions, and estimation of permeability. These properties can be calculated directly from the NMR data using the developed methodology. Any independent measurements of these properties with other methods are not needed. One of the main results of this work is the development of a new NMR on-line core scanner for measurements of porosity in long cylindrical and semi cylindrical drill cores. Also dedicated software was written to operate the NMR on-line core scanner. The physical background of this work is the study of the diffusion influence on transverse relaxation. The diffusion effect in the presence of internal gradients in porous media was probed by 1D and 2D experiments. The transverse relaxation time distributions obtained from 1D and from 2D experiments are comparable but different in fine details. Two new methodologies were developed based on the results of this study. First is the methodology quantifying the influence of diffusion in the internal gradients of water-saturated sediments on transverse relaxation from 2D correlation experiments. The second one is the correction of the permeability estimation from the NMR data taking in account the influence of the diffusion. Furthermore, PFG NMR technique was used to study restricted diffusion in the same kind of samples. Preliminary results are reported

Solid state multinuclear NMR. A versatile tool for studying the reactivity of solid systems

Energy Technology Data Exchange (ETDEWEB)

MacKenzie, Kenneth J.D. [MacDiarmid Institute for Advanced Materials and Nanotechnology, Victoria University of Wellington, P.O. Box 600, Wellington (New Zealand)

2004-08-31

Traditionally, X-ray powder diffraction has been a favoured method for studying chemical reactions in the solid state, but the increasing importance of energy-efficient synthesis methods for solids (e.g. sol-gel synthesis, mechanochemical synthesis) has led to the need for an analytical method not dependent on long-range structural periodicity. Multinuclear solid state nuclear magnetic resonance (NMR) represents a technique which is equally applicable to amorphous or crystalline solids, and is now used in increasing numbers of solid state studies.This paper briefly outlines the principles and practical details of this powerful technique and gives examples of its use in solid-state chemistry, particularly in very recent studies of mechanochemical synthesis of advanced sialon ceramics. The temperature at which these technically important silicon aluminium oxynitride compounds are formed can be significantly lowered by high-energy grinding of their components to produce X-ray amorphous precursors. Solid-state NMR has been used to provide detailed information which could not have been obtained by any other means about the chemical environment of the Si and Al atoms in these amorphous precursors, and the various atomic movements undergone as they crystallise to the final product.

Using an Interactive Web-Based Learning NMR Spectroscopy as a Means to Improve Problem Solving Skills for Undergraduates

International Nuclear Information System (INIS)

Supasorn, Saksri; Vibuljun, Sunantha; Panijpan, Bhinyo; Rajviroongit, Shuleewan

2005-10-01

An Interactive Web-Based Learning NMR Spectroscopy course is developed to improve and facilitate student ' s learning as well as achievement of learning objectives in the concepts of multiplicity, chemical shift, and problem solving. This web-based learning course is emphasized on NMR problem solving, therefore, the concepts of multiplicity and chemical shift, basic concepts for practice problem solving, are also emphasized. Most of animations and pictures in this web-based learning are new created and simplified to explain processes and principles in NMR spectroscopy. With meaningful animations and pictures, simplified English language used, step-by-step problem solving, and interactive test, it can be self-learning web site and best on the student ' s convenience

A software framework for analysing solid-state MAS NMR data

International Nuclear Information System (INIS)

Stevens, Tim J.; Fogh, Rasmus H.; Boucher, Wayne; Higman, Victoria A.; Eisenmenger, Frank; Bardiaux, Benjamin; Rossum, Barth-Jan van; Oschkinat, Hartmut; Laue, Ernest D.

2011-01-01

Solid-state magic-angle-spinning (MAS) NMR of proteins has undergone many rapid methodological developments in recent years, enabling detailed studies of protein structure, function and dynamics. Software development, however, has not kept pace with these advances and data analysis is mostly performed using tools developed for solution NMR which do not directly address solid-state specific issues. Here we present additions to the CcpNmr Analysis software package which enable easier identification of spinning side bands, straightforward analysis of double quantum spectra, automatic consideration of non-uniform labelling schemes, as well as extension of other existing features to the needs of solid-state MAS data. To underpin this, we have updated and extended the CCPN data model and experiment descriptions to include transfer types and nomenclature appropriate for solid-state NMR experiments, as well as a set of experiment prototypes covering the experiments commonly employed by solid-sate MAS protein NMR spectroscopists. This work not only improves solid-state MAS NMR data analysis but provides a platform for anyone who uses the CCPN data model for programming, data transfer, or data archival involving solid-state MAS NMR data.

NMRNet: A deep learning approach to automated peak picking of protein NMR spectra.

Science.gov (United States)

Klukowski, Piotr; Augoff, Michal; Zieba, Maciej; Drwal, Maciej; Gonczarek, Adam; Walczak, Michal J

2018-03-14

Automated selection of signals in protein NMR spectra, known as peak picking, has been studied for over 20 years, nevertheless existing peak picking methods are still largely deficient. Accurate and precise automated peak picking would accelerate the structure calculation, and analysis of dynamics and interactions of macromolecules. Recent advancement in handling big data, together with an outburst of machine learning techniques, offer an opportunity to tackle the peak picking problem substantially faster than manual picking and on par with human accuracy. In particular, deep learning has proven to systematically achieve human-level performance in various recognition tasks, and thus emerges as an ideal tool to address automated identification of NMR signals. We have applied a convolutional neural network for visual analysis of multidimensional NMR spectra. A comprehensive test on 31 manually-annotated spectra has demonstrated top-tier average precision (AP) of 0.9596, 0.9058 and 0.8271 for backbone, side-chain and NOESY spectra, respectively. Furthermore, a combination of extracted peak lists with automated assignment routine, FLYA, outperformed other methods, including the manual one, and led to correct resonance assignment at the levels of 90.40%, 89.90% and 90.20% for three benchmark proteins. The proposed model is a part of a Dumpling software (platform for protein NMR data analysis), and is available at https://dumpling.bio/. michaljerzywalczak@gmail.compiotr.klukowski@pwr.edu.pl. Supplementary data are available at Bioinformatics online.

Carbon-13 NMR of flavinoids

International Nuclear Information System (INIS)

Agrawal, P.K.

1989-01-01

The present book has been written with the objective of introducing the organic chemists with the conceptual and experimental basis required for interpretation of 13 C NMR spectra of a flavonoid and to a discussion of general usefulness of the technique in solving flavonoid structural problem. After a brief general introduction to the essential aspects of flavonoids and 13 C NMR spectroscopy, considerable emphasis has been placed in chapter 2 on the various experimental methods and the interpretation of spectral details which enable individual resonance lines to be associated with the appropriate carbons in a molecule. The whole bulk of the literature, published on 13 C NMR of flavonoids in the major journals upto 1986 alongwith some recent references of 1987 has been classified in several categories such as: flavonoids, isflavonoids, other flavonoids, flavonoid glycosides, chalconoids and flavanoids. Each category constitutes a chapter. Finally the last chapter is devoted largely to a discussion for the differentiation of various categories and subcategories of flavonoids and for the establishment of aromatic substitution pattern in these compounds. It should be emphasized that the book is a data book and only concerned with the actual analysis of 13 C NMR spectra, thus a reasonable familiarity with basic instrumentation of 13 C NMR and general pattern of nuclear chemical shifts has been assumed. (author). refs.; figs.; tabs

NMR and domain wall mobility in intermetallic compounds

International Nuclear Information System (INIS)

Guimaraes, A.P.; Sampaio, L.C.; Cunha, S.F.; Alves, K.M.B.

1991-01-01

The technique of pulsed NMR can be used to study the distribution of hyperfine fields in a magnetic matrix. The dynamics of the domain walls are relevant to the generation of NMR signals. In the present study on the (R x Y 1-x ) Fe 2 intermetallic compounds, the reduction in the signals is associated to increased propagation fields. This indicates that a smaller domain wall mobility is at the origin of these effects. NMR spectra in this system show the importance of direct and indirect (i.e., mediated by Fe atoms) terms in the transferred hyperfine field. (author)

NATO Advanced Research Workshop on Thin Film Growth Techniques for Low-Dimensional Structures

CERN Document Server

Parkin, S; Dobson, P; Neave, J; Arrott, A

1987-01-01

This work represents the account of a NATO Advanced Research Workshop on "Thin Film Growth Techniques for Low Dimensional Structures", held at the University of Sussex, Brighton, England from 15-19 Sept. 1986. The objective of the workshop was to review the problems of the growth and characterisation of thin semiconductor and metal layers. Recent advances in deposition techniques have made it possible to design new material which is based on ultra-thin layers and this is now posing challenges for scientists, technologists and engineers in the assessment and utilisation of such new material. Molecular beam epitaxy (MBE) has become well established as a method for growing thin single crystal layers of semiconductors. Until recently, MBE was confined to the growth of III-V compounds and alloys, but now it is being used for group IV semiconductors and II-VI compounds. Examples of such work are given in this volume. MBE has one major advantage over other crystal growth techniques in that the structure of the growi...

Determination of the intracellular pH of intact erythrocytes by 1H NMR spectroscopy

International Nuclear Information System (INIS)

Rabenstein, D.L.; Isab, A.A.

1982-01-01

A method is described for determining the intracellular pH of intact erythrocytes by 1 H NMR. The determination is based on the pH dependence of the chemical shifts of resonances for carbon-bounded protons of an indicator molecule (imidazole) in intact cells. The imidazole is introduced into the erythrocytes by incubation in an isotonic saline solution of the indicator. The pH dependence of the chemical shifts of the imidazole resonances is calibrated from 1 H NMR spectra of the imidazole-containing red cell lysates whose pH is varied by the addition of acid or base and measured directly with a pH electrode. To reduce in intensity or eliminate the much more intense envelope of resonances from the hemoglobin, the 1 H NMR measurements are made by either the spin-echo Fourier transform technique or by the transfer-or-saturation by cross-relaxation method

Proton NMR studies on Megaphaera elsdenii flavodoxin : structure elucidation by 2D-NMR and implications

NARCIS (Netherlands)

Mierlo, van C.

1990-01-01

¹H NMR techniques have been applied for a thorough study of the uncrystallizable Megasphaera elsdenii flavodoxin in its three redox states. The aim of the research project described in this thesis was to obtain answers regarding questions

An NMR log echo data de-noising method based on the wavelet packet threshold algorithm

International Nuclear Information System (INIS)

Meng, Xiangning; Xie, Ranhong; Li, Changxi; Hu, Falong; Li, Chaoliu; Zhou, Cancan

2015-01-01

To improve the de-noising effects of low signal-to-noise ratio (SNR) nuclear magnetic resonance (NMR) log echo data, this paper applies the wavelet packet threshold algorithm to the data. The principle of the algorithm is elaborated in detail. By comparing the properties of a series of wavelet packet bases and the relevance between them and the NMR log echo train signal, ‘sym7’ is found to be the optimal wavelet packet basis of the wavelet packet threshold algorithm to de-noise the NMR log echo train signal. A new method is presented to determine the optimal wavelet packet decomposition scale; this is within the scope of its maximum, using the modulus maxima and the Shannon entropy minimum standards to determine the global and local optimal wavelet packet decomposition scales, respectively. The results of applying the method to the simulated and actual NMR log echo data indicate that compared with the wavelet threshold algorithm, the wavelet packet threshold algorithm, which shows higher decomposition accuracy and better de-noising effect, is much more suitable for de-noising low SNR–NMR log echo data. (paper)

Structure determination of helical filaments by solid-state NMR spectroscopy

Science.gov (United States)

Ahmed, Mumdooh; Spehr, Johannes; König, Renate; Lünsdorf, Heinrich; Rand, Ulfert; Lührs, Thorsten; Ritter, Christiane

2016-01-01

The controlled formation of filamentous protein complexes plays a crucial role in many biological systems and represents an emerging paradigm in signal transduction. The mitochondrial antiviral signaling protein (MAVS) is a central signal transduction hub in innate immunity that is activated by a receptor-induced conversion into helical superstructures (filaments) assembled from its globular caspase activation and recruitment domain. Solid-state NMR (ssNMR) spectroscopy has become one of the most powerful techniques for atomic resolution structures of protein fibrils. However, for helical filaments, the determination of the correct symmetry parameters has remained a significant hurdle for any structural technique and could thus far not be precisely derived from ssNMR data. Here, we solved the atomic resolution structure of helical MAVSCARD filaments exclusively from ssNMR data. We present a generally applicable approach that systematically explores the helical symmetry space by efficient modeling of the helical structure restrained by interprotomer ssNMR distance restraints. Together with classical automated NMR structure calculation, this allowed us to faithfully determine the symmetry that defines the entire assembly. To validate our structure, we probed the protomer arrangement by solvent paramagnetic resonance enhancement, analysis of chemical shift differences relative to the solution NMR structure of the monomer, and mutagenesis. We provide detailed information on the atomic contacts that determine filament stability and describe mechanistic details on the formation of signaling-competent MAVS filaments from inactive monomers. PMID:26733681

Tritiation methods and tritium NMR spectroscopy

International Nuclear Information System (INIS)

Jaiswal, D.K.; Morimoto, H.; Salijoughian, M.; Williams, P.G.

1991-09-01

We have used a simple process for the production of highly tritiated water and characterized the product species by 1 H and 3 H NMR spectroscopy. The water is readily manipulated and used in subsequent reactions either as T 2 O, CH 3 COOT or CF 3 COOT. Development of tritiated diimide has progressed to the point where cis-hydrogenated products at 1-20 Ci/mmole S.A. are possible. Tri-n-butyl tin tritide has been produced at >95% tritium content and well characterized by multinuclear NMR techniques. 27 refs., 3 figs

Isobutylene Dimerization: A Discovery-Based Exploration of Mechanism and Regioselectivity by NMR Spectroscopy and Molecular Modeling

Science.gov (United States)

Schuster, Mariah L.; Peterson, Karl P.; Stoffregen, Stacey A.

2018-01-01

This two-period undergraduate laboratory experiment involves the synthesis of a mixture of isomeric unknowns, isolation of the mixture by means of distillation, and characterization of the two products primarily by NMR spectroscopy (1D and 2D) supported with IR spectroscopy and GC-MS techniques. Subsequent calculation and examination of the…

Pathogenesis-based treatments in primary Sjogren's syndrome using artificial intelligence and advanced machine learning techniques: a systematic literature review.

Science.gov (United States)

Foulquier, Nathan; Redou, Pascal; Le Gal, Christophe; Rouvière, Bénédicte; Pers, Jacques-Olivier; Saraux, Alain

2018-05-17

Big data analysis has become a common way to extract information from complex and large datasets among most scientific domains. This approach is now used to study large cohorts of patients in medicine. This work is a review of publications that have used artificial intelligence and advanced machine learning techniques to study physio pathogenesis-based treatments in pSS. A systematic literature review retrieved all articles reporting on the use of advanced statistical analysis applied to the study of systemic autoimmune diseases (SADs) over the last decade. An automatic bibliography screening method has been developed to perform this task. The program called BIBOT was designed to fetch and analyze articles from the pubmed database using a list of keywords and Natural Language Processing approaches. The evolution of trends in statistical approaches, sizes of cohorts and number of publications over this period were also computed in the process. In all, 44077 abstracts were screened and 1017 publications were analyzed. The mean number of selected articles was 101.0 (S.D. 19.16) by year, but increased significantly over the time (from 74 articles in 2008 to 138 in 2017). Among them only 12 focused on pSS but none of them emphasized on the aspect of pathogenesis-based treatments. To conclude, medicine progressively enters the era of big data analysis and artificial intelligence, but these approaches are not yet used to describe pSS-specific pathogenesis-based treatment. Nevertheless, large multicentre studies are investigating this aspect with advanced algorithmic tools on large cohorts of SADs patients.

Efficient design of multituned transmission line NMR probes: the electrical engineering approach.

Science.gov (United States)

Frydel, J A; Krzystyniak, M; Pienkowski, D; Pietrzak, M; de Sousa Amadeu, N; Ratajczyk, T; Idzik, K; Gutmann, T; Tietze, D; Voigt, S; Fenn, A; Limbach, H H; Buntkowsky, G

2011-01-01

Transmission line-based multi-channel solid state NMR probes have many advantages regarding the cost of construction, number of RF-channels, and achievable RF-power levels. Nevertheless, these probes are only rarely employed in solid state-NMR-labs, mainly owing to the difficult experimental determination of the necessary RF-parameters. Here, the efficient design of multi-channel solid state MAS-NMR probes employing transmission line theory and modern techniques of electrical engineering is presented. As technical realization a five-channel ((1)H, (31)P, (13)C, (2)H and (15)N) probe for operation at 7 Tesla is described. This very cost efficient design goal is a multi port single coil transmission line probe based on the design developed by Schaefer and McKay. The electrical performance of the probe is determined by measuring of Scattering matrix parameters (S-parameters) in particular input/output ports. These parameters are compared to the calculated parameters of the design employing the S-matrix formalism. It is shown that the S-matrix formalism provides an excellent tool for examination of transmission line probes and thus the tool for a rational design of these probes. On the other hand, the resulting design provides excellent electrical performance. From a point of view of Nuclear Magnetic Resonance (NMR), calibration spectra of particular ports (channels) are of great importance. The estimation of the π/2 pulses length for all five NMR channels is presented. Copyright © 2011 Elsevier Inc. All rights reserved.

Advanced neuroimaging techniques for the term newborn with encephalopathy.

Science.gov (United States)

Chau, Vann; Poskitt, Kenneth John; Miller, Steven Paul

2009-03-01

Neonatal encephalopathy is associated with a high risk of morbidity and mortality in the neonatal period and of long-term neurodevelopmental disability in survivors. Advanced magnetic resonance techniques now play a major role in the clinical care of newborns with encephalopathy and in research addressing this important condition. From conventional magnetic resonance imaging, typical patterns of injury have been defined in neonatal encephalopathy. When applied in contemporary cohorts of newborns with encephalopathy, the patterns of brain injury on magnetic resonance imaging distinguish risk factors, clinical presentation, and risk of abnormal outcome. Advanced magnetic resonance techniques such as magnetic resonance spectroscopy, diffusion-weighted imaging, and diffusion tensor imaging provide novel perspectives on neonatal brain metabolism, microstructure, and connectivity. With the application of these imaging tools, it is increasingly apparent that brain injury commonly occurs at or near the time of birth and evolves over the first weeks of life. These observations have complemented findings from trials of emerging strategies of brain protection, such as hypothermia. Application of these advanced magnetic resonance techniques may enable the earliest possible identification of newborns at risk of neurodevelopmental impairment, thereby ensuring appropriate follow-up with rehabilitation and psychoeducational resources.

ECG gated NMR-CT for cardiovascular diseases

International Nuclear Information System (INIS)

Nishikawa, J.; Machida, K.; Iio, M.; Yoshimoto, N.; Sugimoto, T.; Kawaguchi, H.; Mano, H.

1984-01-01

The authors applied NMR-CT to cardiac study with ECG gated technique to evaluate the left ventricular (LV) function and compared it with cardiovascular nuclear medicine study (NM). The NMR-CT machine has resistive air-core magnet with 0.15 Tesla. The saturation recovery image or inversion recovery image were obtained as 256 x 256 matrix and 15 mm in thickness. The study population was ten patients who were evaluated both by NMR image and by NM performed within one week interval. The heart muscle was able to be visualized without any contrast material nor radioisotopes in inversion recovery images, whereas saturation recovery images failed to separate heart muscle from blood pool. The wall motions of LV in both methods were well correlated except for inferior wall. The values of ejection fraction in NMR image were moderately low, but two modalities showed satisfactory correlation (r=0.85). The region of myocardial infarction was revealed as wall thinning and/or wall motion abnormality. It is still preliminary to draw a conclusion, however, it can be said that in the evaluation of LV function, method by NMR might be of equal value to those of NM. It can be certain that eventually gated NMR-CT will become more effective method for various aspects of cardiovascular evaluation

In situ NMR and electrochemical quartz crystal microbalance techniques reveal the structure of the electrical double layer in supercapacitors

Science.gov (United States)

Griffin, John M.; Forse, Alexander C.; Tsai, Wan-Yu; Taberna, Pierre-Louis; Simon, Patrice; Grey, Clare P.

2015-08-01

Supercapacitors store charge through the electrosorption of ions on microporous electrodes. Despite major efforts to understand this phenomenon, a molecular-level picture of the electrical double layer in working devices is still lacking as few techniques can selectively observe the ionic species at the electrode/electrolyte interface. Here, we use in situ NMR to directly quantify the populations of anionic and cationic species within a working microporous carbon supercapacitor electrode. Our results show that charge storage mechanisms are different for positively and negatively polarized electrodes for the electrolyte tetraethylphosphonium tetrafluoroborate in acetonitrile; for positive polarization charging proceeds by exchange of the cations for anions, whereas for negative polarization, cation adsorption dominates. In situ electrochemical quartz crystal microbalance measurements support the NMR results and indicate that adsorbed ions are only partially solvated. These results provide new molecular-level insight, with the methodology offering exciting possibilities for the study of pore/ion size, desolvation and other effects on charge storage in supercapacitors.

Clinical application and evaluation of the diagnostic significance of NMR-tomography

International Nuclear Information System (INIS)

Bielke, G.; Higer, P.

1987-01-01

Aim of the project was the clinical application and evaluation of the diagnostic significance of NMR-tomography. About 3 000 patients have been examined especially with diseases of the brain. In 75% of all cases pathological findings could be detected. A subgroup of these patients was used for comprehensive studies with regard to tissue characterization based on the calculation of relaxation time parameters. With methods of image processing and classification techniques we tried to get a clear correlation between combined NMR-parameters and human tissue types. The results show that this procedure is able to improve the detectibility and the association to finding groups and tumorgradings in certain cases. (orig./ECB) With 134 refs., 17 tabs., 86 figs [de

(1)H NMR-based metabonomics revealed protective effect of Naodesheng bioactive extract on ischemic stroke rats.

Science.gov (United States)

Luo, Lan; Zhen, Lifeng; Xu, Yatao; Yang, Yongxia; Feng, Suxiang; Wang, Shumei; Liang, Shengwang

2016-06-20

Stroke is a leading cause of death and disability in the world. However, current therapies are limited. Naodesheng, a widely used traditional Chinese medicine prescription, has shown a good clinical curative effect on ischemic stroke. Also, Naodesheng has been suggested to have neuroprotective effect on focal cerebral ischemia rats, but the underlying molecular mechanism remains unclear. The present study was designed to evaluate the effect of Naodesheng bioactive extract on the metabolic changes in brain tissue, plasma and urine induced by cerebral ischemia perfusion injury, and explore the possible metabolic mechanisms by using a (1)H NMR-based metabonomics approach. A middle cerebral artery occlusion rat model was established and confirmed by the experiments of neurobehavioral abnormality evaluation, brain tissue TTC staining and pathological examination. The metabolic changes in brain tissue, plasma and urine were then assessed by a (1)H NMR technique combined with multivariate statistical analysis method. These NMR data showed that cerebral ischemia reperfusion induced great metabolic disorders in brain tissue, plasma and urine metabolisms. However, Naodesheng bioactive extract could reverse most of the imbalanced metabolites. Meanwhile, it was found that both the medium and high dosages of Naodesheng bioactive extract were more effective on the metabolic changes than the low dosage, consistent with histopathological assessments. These results revealed that Naodesheng had protective effect on ischemic stroke rats and the underlying mechanisms involved multiple metabolic pathways, including energy metabolism, amino acid metabolism, oxidative stress and inflammatory injury. The present study could provide evidence that metabonomics revealed its capacity to evaluate the holistic efficacy of traditional Chinese medicine and explore the underlying mechanisms. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

LipSpin: A New Bioinformatics Tool for Quantitative 1H NMR Lipid Profiling.

Science.gov (United States)

Barrilero, Rubén; Gil, Miriam; Amigó, Núria; Dias, Cintia B; Wood, Lisa G; Garg, Manohar L; Ribalta, Josep; Heras, Mercedes; Vinaixa, Maria; Correig, Xavier

2018-02-06

The structural similarity among lipid species and the low sensitivity and spectral resolution of nuclear magnetic resonance (NMR) have traditionally hampered the routine use of 1 H NMR lipid profiling of complex biological samples in metabolomics, which remains mostly manual and lacks freely available bioinformatics tools. However, 1 H NMR lipid profiling provides fast quantitative screening of major lipid classes (fatty acids, glycerolipids, phospholipids, and sterols) and some individual species and has been used in several clinical and nutritional studies, leading to improved risk prediction models. In this Article, we present LipSpin, a free and open-source bioinformatics tool for quantitative 1 H NMR lipid profiling. LipSpin implements a constrained line shape fitting algorithm based on voigt profiles and spectral templates from spectra of lipid standards, which automates the analysis of severely overlapped spectral regions and lipid signals with complex coupling patterns. LipSpin provides the most detailed quantification of fatty acid families and choline phospholipids in serum lipid samples by 1 H NMR to date. Moreover, analytical and clinical results using LipSpin quantifications conform with other techniques commonly used for lipid analysis.

Mapping of unfolding states of integral helical membrane proteins by GPS-NMR and scattering techniques

DEFF Research Database (Denmark)

Calcutta, Antonello; Jessen, Christian M; Behrens, Manja Annette

2012-01-01

induced by unfolding of an integral membrane protein, namely TFE-induced unfolding of KcsA solubilized by the n-dodecyl ß-d-maltoside (DDM) surfactant is investigated by the recently introduced GPS-NMR (Global Protein folding State mapping by multivariate NMR) (Malmendal et al., PlosONE 5, e10262 (2010......)) along with dynamic light scattering (DLS) and small-angle X-ray scattering (SAXS). GPS-NMR is used as a tool for fast analysis of the protein unfolding processes upon external perturbation, and DLS and SAXS are used for further structural characterization of the unfolding states. The combination allows...

Nuclear techniques in the development of advanced ceramic technologies

International Nuclear Information System (INIS)

Axe, J.D.; Hewat, A.W.; Maier, J.; Margaca, F.M.A.; Rauch, H.

1999-01-01

The importance of research, development and application of advanced materials is well understood by all developed and most developing countries. Amongst advanced materials, ceramics play a prominent role due to their specific chemical and physical properties. According to performance and importance, advanced ceramics can be classified as structural ceramics (mechanical function) and the so-called functional ceramics. In the latter class of materials, special electrical, chemical, thermal, magnetic and optical properties are of interest. The most valuable materials are multifunctional, for example, when structural ceramics combine beneficial mechanical properties with thermal and chemical sensitivity. Multifunctionality is characteristic of many composite materials (organic/inorganic composite). Additionally, properties of material can be changed by reducing its dimension (thin films, nanocrystalline ceramics). Nuclear techniques, found important applications in research and development of advanced ceramics. The use of neutron techniques has increased dramatically in recent years due to the development of advanced neutron sources, instrumentation and improved data analysis. Typical neutron techniques are neutron diffraction, neutron radiography, small angle neutron scattering and very small angle neutron scattering. Neutrons can penetrate deeply into most materials thus sampling their bulk properties. In determination of the crystal structure of HTSC, YBa 2 Cu 2 O 7 , XRD located the heavy metal atoms, but failed in finding many of the oxygen atoms, while the neutron diffraction located all atoms equally well in the crystal structure. Neutron diffraction is also unique for the determination of the magnetic structure of materials since the neutrons themselves have a magnetic moment. Application of small angle neutron scattering for the determination of the size of hydrocarbon aggregates within the zeolite channels is illustrated. (author)

Deuterium and lithium-6 MAS NMR studies of manganese oxide electrode materials

Science.gov (United States)

Paik, Younkee

Electrolytic manganese dioxide (EMD) is used world wide as the cathode materials in both lithium and alkaline primary (non-rechargeable) batteries. We have developed deuterium and lithium MAS NMR techniques to study EMD and related manganese oxides and hydroxides, where diffraction techniques are of limited value due to a highly defective nature of the structures. Deuterons in EMD, manganite, groutite, and deuterium-intercalated pyrolusite and ramsdellite were detected by NMR, for the first time, and their locations and motions in the structures were analyzed by applying variable temperature NMR techniques. Discharge mechanisms of EMD in alkaline (aqueous) electrolytes were studied, in conjunction with step potential electrochemical spectroscopic (SPECS) method, and five distinctive discharge processes were proposed. EMD is usually heat-treated at about 300--400°C to remove water to be used in lithium batteries. Details of the effects of heat-treatment, such as structural and compositional changes as a function of heat-treatment temperature, were studied by a combination of MAS NMR, XRD, and thermogravimetric analysis. Lithium local environments in heat-treated EMD (HEMD) that were discharged in lithium cells, were described in terms of related environments found in model compounds pyrolusite and ramsdellite where specific Li + sites were detected by MAS NMR and the hyperfine shift scale method of Grey et al. Acid-leaching of Li2MnO3 represents an approach for synthesizing new or modified manganese oxide electrode materials for lithium rechargeable batteries. Progressive removal of lithium from specific crystallographic sites, followed by a gradual change of the crystal structure, was monitored by a combination of NMR and XRD techniques.

Photochemical Degradation of the Anticancer Drug Bortezomib by V-UV/UV (185/254 nm) Investigated by (1)H NMR Fingerprinting: A Way to Follow Aromaticity Evolution.

Science.gov (United States)

Martignac, Marion; Balayssac, Stéphane; Gilard, Véronique; Benoit-Marquié, Florence

2015-06-18

We have investigated the removal of bortezomib, an anticancer drug prescribed in multiple myeloma, using the photochemical advanced oxidation process of V-UV/UV (185/254 nm). We used two complementary analytical techniques to follow the removal rate of bortezomib. Nuclear magnetic resonance (NMR) is a nonselective method requiring no prior knowledge of the structures of the byproducts and permits us to provide a spectral signature (fingerprinting approach). This untargeted method provides clues to the molecular structure changes and information on the degradation of the parent drug during the irradiation process. This holistic NMR approach could provide information for monitoring aromaticity evolution. We use liquid chromatography, coupled with high-resolution mass spectrometry (LC-MS), to correlate results obtained by (1)H NMR and for accurate identification of the byproducts, in order to understand the mechanistic degradation pathways of bortezomib. The results show that primary byproducts come from photoassisted deboronation of bortezomib at 254 nm. A secondary byproduct of pyrazinecarboxamide was also identified. We obtained a reliable correlation between these two analytical techniques.

Mini-review: novel non-destructivein situbiofilm characterization techniques in membrane systems

KAUST Repository

Valladares Linares, Rodrigo; Fortunato, Luca; Farhat, Nadia; Bucs, Szilard; Staal, M.; Fridjonsson, E.O.; Johns, M.L.; Vrouwenvelder, Johannes S.; Leiknes, TorOve

2016-01-01

Membrane systems are commonly used in the water industry to produce potable water and for advanced wastewater treatment. One of the major drawbacks of membrane systems is biofilm formation (biofouling), which results in an unacceptable decline in membrane performance. Three novel in situ biofouling characterization techniques were assessed: (i) optical coherence tomography (OCT), (ii) planar optodes, and (iii) nuclear magnetic resonance (NMR). The first two techniques were assessed using a biofilm grown on the surface of nanofiltration (NF) membranes using a transparent membrane fouling simulator that accurately simulates spiral wound modules, modified for in situ biofilm imaging. For the NMR study, a spiral wound reverse osmosis membrane module was used. Results show that these techniques can provide information to reconstruct the biofilm accurately, either with 2-D (OCT, planar optodes and NMR), or 3-D (OCT and NMR) scans. These non-destructive tools can elucidate the interaction of hydrodynamics and mass transport on biofilm accumulation in membrane systems. Oxygen distribution in the biofilm can be mapped and linked to water flow and substrate characteristics; insights on the effect of crossflow velocity, flow stagnation, and feed spacer presence can be obtained, and in situ information on biofilm structure, thickness, and spatial distribution can be quantitatively assessed. The combination of these novel non-destructive in situ biofilm characterization techniques can provide real-time observation of biofilm formation at the mesoscale. The information obtained with these tools could potentially be used for further improvement in the design of membrane systems and operational parameters to reduce impact of biofouling on membrane performance. © 2016 Balaban Desalination Publications. All rights reserved.

Mini-review: novel non-destructivein situbiofilm characterization techniques in membrane systems

KAUST Repository

Valladares Linares, R.

2016-05-12

Membrane systems are commonly used in the water industry to produce potable water and for advanced wastewater treatment. One of the major drawbacks of membrane systems is biofilm formation (biofouling), which results in an unacceptable decline in membrane performance. Three novel in situ biofouling characterization techniques were assessed: (i) optical coherence tomography (OCT), (ii) planar optodes, and (iii) nuclear magnetic resonance (NMR). The first two techniques were assessed using a biofilm grown on the surface of nanofiltration (NF) membranes using a transparent membrane fouling simulator that accurately simulates spiral wound modules, modified for in situ biofilm imaging. For the NMR study, a spiral wound reverse osmosis membrane module was used. Results show that these techniques can provide information to reconstruct the biofilm accurately, either with 2-D (OCT, planar optodes and NMR), or 3-D (OCT and NMR) scans. These non-destructive tools can elucidate the interaction of hydrodynamics and mass transport on biofilm accumulation in membrane systems. Oxygen distribution in the biofilm can be mapped and linked to water flow and substrate characteristics; insights on the effect of crossflow velocity, flow stagnation, and feed spacer presence can be obtained, and in situ information on biofilm structure, thickness, and spatial distribution can be quantitatively assessed. The combination of these novel non-destructive in situ biofilm characterization techniques can provide real-time observation of biofilm formation at the mesoscale. The information obtained with these tools could potentially be used for further improvement in the design of membrane systems and operational parameters to reduce impact of biofouling on membrane performance. © 2016 Balaban Desalination Publications. All rights reserved.

Functional Group and Structural Characterization of Unmodified and Functionalized Lignin by Titration, Elemental Analysis, 1H NMR and FTIR Techniques

Directory of Open Access Journals (Sweden)

Ramin Bairami Habashi

2017-11-01

Full Text Available Lignin is the second most abundant polymer in the world after cellulose. Therefore, characterization of the structure and functional groups of lignin in order to assess its potential applications in various technical fields has become a necessity. One of the major problems related to the characterization of lignin is the lack of well-defined protocols and standards. In this paper, systematic studies have been done to characterize the structure and functional groups of lignin quantitatively using different techniques such as elemental analysis, titration and 1H NMR and FTIR techniques. Lignin as a black liquor was obtained from Choka Paper Factory and it was purified before any test. The lignin was reacted with α-bromoisobutyryl bromide to calculate the number of hydroxyl and methoxyl moles. Using 1H NMR spectroscopic method on α-bromoisobutyrylated lignin (BiBL in the presence of a given amount of N,N-dimethylformamide (DMF as an internal standard, the number of moles of hydroxyl and methoxyl groups per gram of lignin was found to be 6.44 mmol/g and 6.64 mmol/g, respectively. Using aqueous titration, the number of moles of phenolic hydroxyl groups and carboxyl groups of the lignin were calculated as 3.13 mmol/g and 2.84 mmol/g, respectively. The findings obtained by 1H NMR and elemental analysis indicated to phenyl propane unit of the lignin with C9 structural formula as C9 HAl 3.84HAr2.19S0.2O0.8(OH1.38(OCH31.42. Due to poor solubility of the lignin in tetrahydrofuran (THF, acetylated lignin was used in the GPC analysis, by which number-average molecular weight  of the lignin was calculated as 992 g/mol.

Advanced condition monitoring techniques and plant life extension studies at EBR-2

International Nuclear Information System (INIS)

Singer, R.M.; Gross, K.C.; Perry, W.H.; King, R.W.

1991-01-01

Numerous advanced techniques have been evaluated and tested at EBR-2 as part of a plant-life extension program for detection of degradation and other abnormalities in plant systems. Two techniques have been determined to be of considerable assistance in planning for the extended-life operation of EBR-2. The first, a computer-based pattern-recognition system (System State Analyzer or SSA) is used for surveillance of the primary system instrumentation, primary sodium pumps and plant heat balances. This surveillance has indicated that the SSA can detect instrumentation degradation and system performance degradation over varying time intervals and can be used to provide derived signal values to replace signals from failed sensors. The second technique, also a computer-based pattern-recognition system (Sequential Probability Ratio Test or SPRT) is used to validate signals and to detect incipient failures in sensors and components or systems. It is being used on the failed fuel detection system and is experimentally used on the primary coolant pumps. Both techniques are described and experience with their operation presented

Modelling the acid/base 1H NMR chemical shift limits of metabolites in human urine.

Science.gov (United States)

Tredwell, Gregory D; Bundy, Jacob G; De Iorio, Maria; Ebbels, Timothy M D

2016-01-01

Despite the use of buffering agents the 1 H NMR spectra of biofluid samples in metabolic profiling investigations typically suffer from extensive peak frequency shifting between spectra. These chemical shift changes are mainly due to differences in pH and divalent metal ion concentrations between the samples. This frequency shifting results in a correspondence problem: it can be hard to register the same peak as belonging to the same molecule across multiple samples. The problem is especially acute for urine, which can have a wide range of ionic concentrations between different samples. To investigate the acid, base and metal ion dependent 1 H NMR chemical shift variations and limits of the main metabolites in a complex biological mixture. Urine samples from five different individuals were collected and pooled, and pre-treated with Chelex-100 ion exchange resin. Urine samples were either treated with either HCl or NaOH, or were supplemented with various concentrations of CaCl 2 , MgCl 2 , NaCl or KCl, and their 1 H NMR spectra were acquired. Nonlinear fitting was used to derive acid dissociation constants and acid and base chemical shift limits for peaks from 33 identified metabolites. Peak pH titration curves for a further 65 unidentified peaks were also obtained for future reference. Furthermore, the peak variations induced by the main metal ions present in urine, Na + , K + , Ca 2+ and Mg 2+ , were also measured. These data will be a valuable resource for 1 H NMR metabolite profiling experiments and for the development of automated metabolite alignment and identification algorithms for 1 H NMR spectra.

Condensed Matter NMR under Extreme Conditions: Challenges and Opportunities

Science.gov (United States)

Reyes, Arneil

2006-11-01

Advances in resistive magnet and power supply technology have made available extremely high magnetic fields suitable for condensed matter broadline NMR experiments. This capability expands the available phase space for investigating a wide variety of materials using magnetic resonance; utilizing the strength of the field to expose or induce new physical phenomena resulting in better understanding of the physics. Continuous fields up to 45T in NHMFL Hybrid magnet have brought new challenges in designing NMR instrumentation. Field strengths and sample space limitations put constraints on RF pulse power, tuning range, bandwidth, and temperature control. The inclusion of other capabilities, including high pressure, optics, and sample rotation requires intricate probe design and construction, while extremely low milliKelvin temperatures are desired in order to explore energy scales where thermal fluctuations are suppressed. Optimization of these devices has been of paramount consideration in NHMFL Condensed Matter NMR user program. Science achieved at high fields, the new initiatives to develop resistively-detected NMR in 2D electron gas and similar systems, and the current new generation Series-Connected Hybrid magnets for NMR work will be discussed. The NHMFL is supported by the National Science Foundation and the State of Florida.

De novo fragment-based design of inhibitors of DXS guided by spin-diffusion-based NMR spectroscopy

NARCIS (Netherlands)

Masini, T.; Pilger, J.; Kroezen, B. S.; Illarionov, B.; Lottmann, P.; Fischer, M.; Griesinger, C.; Hirsch, A. K. H.

We applied for the first time an innovative ligand-based NMR methodology (STI) to a medicinal-chemistry project aimed at the development of inhibitors for the enzyme 1-deoxy-D-xylulose-5-phosphate synthase (DXS). DXS is the first enzyme of the 2C-methyl-D-erythritol-4-phosphate (MEP) pathway,

Functional studies using NMR

International Nuclear Information System (INIS)

McCready, V.R.; Leach, M.; Ell, P.J.

1987-01-01

This volume is based on a series of lectures delivered at a one-day teaching symposium on functional and metabolic aspects of NMR measurements held at the Middlesex Hospital Medical School on 1st September 1985 as a part of the European Nuclear Medicine Society Congress. Currently the major emphasis in medical NMR in vivo is on its potential to image and display abnormalities in conventional radiological images, providing increased contrast between normal and abnormal tissue, improved definition of vasculature, and possibly an increased potential for differential diagnosis. Although these areas are undeniably of major importance, it is probable that NMR will continue to complement conventional measurement methods. The major potential benefits to be derived from in vivo NMR measurements are likely to arise from its use as an instrument for functional and metabolic studies in both clinical research and in the everyday management of patients. It is to this area that this volume is directed

Parental Attitudes Toward Advanced Behavior Guidance Techniques Used in Pediatric Dentistry.

Science.gov (United States)

Patel, Monica; McTigue, Dennis J; Thikkurissy, Sarat; Fields, Henry W

2016-01-01

To re-examine parental attitudes toward advanced behavior management techniques in pediatric dentistry and determine whether cost, urgency, and amount of treatment influence parental preferences. Parents viewed previously validated videotaped clinical vignettes of four advanced behavior guidance techniques: (1) passive immobilization; (2) active immobilization; (3) general anesthesia; and (4) oral sedation. The study was conducted in a children's hospital dental clinic and a suburban private pediatric dentistry office. Parents rated overall acceptance of the techniques, and acceptance under specified conditions using an anchored visual analogue scale. One hundred five parents completed the survey; 55 from the children's hospital and 50 from private practice. Oral sedation was rated as the most acceptable technique, followed by general anesthesia, active immobilization, and passive immobilization. As urgency, convenience, and previous experience increased, parental acceptance of the technique increased. As cost of treatment increased, parental acceptance decreased. Ratings between the children's hospital group and private practice group differed, as did the demographic variables of insurance, income, and race. The hierarchy of parental acceptance of advanced behavior guidance techniques is changing with increasing approval of pharmacological management and decreasing approval of physical management. The health care delivery system, urgency, convenience, previous experience, and cost all influence parental acceptance.

Principles and techniques in the design of ADMS+. [advanced data-base management system

Science.gov (United States)

Roussopoulos, Nick; Kang, Hyunchul

1986-01-01

'ADMS+/-' is an advanced data base management system whose architecture integrates the ADSM+ mainframe data base system with a large number of work station data base systems, designated ADMS-; no communications exist between these work stations. The use of this system radically decreases the response time of locally processed queries, since the work station runs in a single-user mode, and no dynamic security checking is required for the downloaded portion of the data base. The deferred update strategy used reduces overhead due to update synchronization in message traffic.

Advanced inspection and repair techniques for primary side components

International Nuclear Information System (INIS)

Elm, Ralph

1998-01-01

The availability of nuclear power plant mainly depends on the components of the Nuclear Steam Supply System (NSSS) such as reactor pressure vessel, core internals and steam generators. The last decade has been characterized by intensive inspection and repair work on PWR steam generators. In the future, it can be expected, that the inspection of the reactor pressure vessel and the inspection and repair of its internals, in both PWR and BWR will be one of the challenges for the nuclear community. Due to this challenge, new, advanced inspection and repair techniques for the vital primary side components have been developed and applied, taking into account such issues as: use of reliable and fast inspection methods, repair of affected components instead of costly replacement, reduction of outage time compared to conventional methods, minimized radiation exposure, acceptable costs. This paper reflects on advanced inspection and repair techniques such as: Baffle Former Bolt inspection and replacement, Barrel Former Bolt inspection and replacement, Mechanized UT and visual inspection of reactor pressure vessels, Steam Generator repair by advanced sleeving technology. The techniques described have been successfully applied in nuclear power plants and improved the operation performance of the components and the NPP. (author). 6 figs

Burnout prediction using advance image analysis coal characterization techniques

Energy Technology Data Exchange (ETDEWEB)

Edward Lester; Dave Watts; Michael Cloke [University of Nottingham, Nottingham (United Kingdom). School of Chemical Environmental and Mining Engineering

2003-07-01

The link between petrographic composition and burnout has been investigated previously by the authors. However, these predictions were based on 'bulk' properties of the coal, including the proportion of each maceral or the reflectance of the macerals in the whole sample. Combustion studies relating burnout with microlithotype analysis, or similar, remain less common partly because the technique is more complex than maceral analysis. Despite this, it is likely that any burnout prediction based on petrographic characteristics will become more accurate if it includes information about the maceral associations and the size of each particle. Chars from 13 coals, 106-125 micron size fractions, were prepared using a Drop Tube Furnace (DTF) at 1300{degree}C and 200 millisecond and 1% Oxygen. These chars were then refired in the DTF at 1300{degree}C 5% oxygen and residence times of 200, 400 and 600 milliseconds. The progressive burnout of each char was compared with the characteristics of the initial coals. This paper presents an extension of previous studies in that it relates combustion behaviour to coals that have been characterized on a particle by particle basis using advanced image analysis techniques. 13 refs., 7 figs.

1H NMR-based spectroscopy detects metabolic alterations in serum of patients with early-stage ulcerative colitis

International Nuclear Information System (INIS)

Zhang, Ying; Lin, Lianjie; Xu, Yanbin; Lin, Yan; Jin, Yu; Zheng, Changqing

2013-01-01

Highlights: •Twenty ulcerative colitis patients and nineteen healthy controls were enrolled. •Increased 3-hydroxybutyrate, glucose, phenylalanine, and decreased lipid were found. •We report early stage diagnosis of ulcerative colitis using NMR-based metabolomics. -- Abstract: Ulcerative colitis (UC) has seriously impaired the health of citizens. Accurate diagnosis of UC at an early stage is crucial to improve the efficiency of treatment and prognosis. In this study, proton nuclear magnetic resonance ( 1 H NMR)-based metabolomic analysis was performed on serum samples collected from active UC patients (n = 20) and healthy controls (n = 19), respectively. The obtained spectral profiles were subjected to multivariate data analysis. Our results showed that consistent metabolic alterations were present between the two groups. Compared to healthy controls, UC patients displayed increased 3-hydroxybutyrate, β-glucose, α-glucose, and phenylalanine, but decreased lipid in serum. These findings highlight the possibilities of NMR-based metabolomics as a non-invasive diagnostic tool for UC

FoodPro: A Web-Based Tool for Evaluating Covariance and Correlation NMR Spectra Associated with Food Processes

Directory of Open Access Journals (Sweden)

Eisuke Chikayama

2016-10-01

Full Text Available Foods from agriculture and fishery products are processed using various technologies. Molecular mixture analysis during food processing has the potential to help us understand the molecular mechanisms involved, thus enabling better cooking of the analyzed foods. To date, there has been no web-based tool focusing on accumulating Nuclear Magnetic Resonance (NMR spectra from various types of food processing. Therefore, we have developed a novel web-based tool, FoodPro, that includes a food NMR spectrum database and computes covariance and correlation spectra to tasting and hardness. As a result, FoodPro has accumulated 236 aqueous (extracted in D2O and 131 hydrophobic (extracted in CDCl3 experimental bench-top 60-MHz NMR spectra, 1753 tastings scored by volunteers, and 139 hardness measurements recorded by a penetrometer, all placed into a core database. The database content was roughly classified into fish and vegetable groups from the viewpoint of different spectrum patterns. FoodPro can query a user food NMR spectrum, search similar NMR spectra with a specified similarity threshold, and then compute estimated tasting and hardness, covariance, and correlation spectra to tasting and hardness. Querying fish spectra exemplified specific covariance spectra to tasting and hardness, giving positive covariance for tasting at 1.31 ppm for lactate and 3.47 ppm for glucose and a positive covariance for hardness at 3.26 ppm for trimethylamine N-oxide.

FoodPro: A Web-Based Tool for Evaluating Covariance and Correlation NMR Spectra Associated with Food Processes.

Science.gov (United States)

Chikayama, Eisuke; Yamashina, Ryo; Komatsu, Keiko; Tsuboi, Yuuri; Sakata, Kenji; Kikuchi, Jun; Sekiyama, Yasuyo

2016-10-19

Foods from agriculture and fishery products are processed using various technologies. Molecular mixture analysis during food processing has the potential to help us understand the molecular mechanisms involved, thus enabling better cooking of the analyzed foods. To date, there has been no web-based tool focusing on accumulating Nuclear Magnetic Resonance (NMR) spectra from various types of food processing. Therefore, we have developed a novel web-based tool, FoodPro, that includes a food NMR spectrum database and computes covariance and correlation spectra to tasting and hardness. As a result, FoodPro has accumulated 236 aqueous (extracted in D₂O) and 131 hydrophobic (extracted in CDCl₃) experimental bench-top 60-MHz NMR spectra, 1753 tastings scored by volunteers, and 139 hardness measurements recorded by a penetrometer, all placed into a core database. The database content was roughly classified into fish and vegetable groups from the viewpoint of different spectrum patterns. FoodPro can query a user food NMR spectrum, search similar NMR spectra with a specified similarity threshold, and then compute estimated tasting and hardness, covariance, and correlation spectra to tasting and hardness. Querying fish spectra exemplified specific covariance spectra to tasting and hardness, giving positive covariance for tasting at 1.31 ppm for lactate and 3.47 ppm for glucose and a positive covariance for hardness at 3.26 ppm for trimethylamine N -oxide.

A novel tridentate Schiff base dioxo-molybdenum(VI) complex: synthesis, experimental and theoretical studies on its crystal structure, FTIR, UV-visible, ¹H NMR and ¹³C NMR spectra.

Science.gov (United States)

Saheb, Vahid; Sheikhshoaie, Iran; Stoeckli-Evans, Helen

2012-09-01

A new dioxo-molybdenum(VI) complex [MoO(2)(L)(H(2)O)] has been synthesized, using 5-methoxy 2-[(2-hydroxypropylimino)methyl]phenol as tridentate ONO donor Schiff base ligand (H(2)L) and MoO(2)(acac)(2). The yellow crystals of the compound are used for single-crystal X-ray analysis and measuring Fourier Transform Infrared (FTIR), UV-visible, (1)H NMR and (13)C NMR spectra. Electronic structure calculations at the B3LYP and PW91PW91 levels of theory are performed to optimize the molecular geometry and to calculate the UV-visible, FTIR, (1)H NMR and (13)C NMR spectra of the compound. Vibrational assignments and analysis of the fundamental modes of the compound are performed. Time-dependent density functional theory (TDDFT) method is used to calculate the electronic transitions of the complex. All theoretical methods can well reproduce the structure of the compound. The (1)H NMR shielding tensors computed at the B3LYP/DGDZVP level of theory is in agreement with experimental (1)H NMR spectra. However, the (13)C NMR shielding tensors computed at the B3LYP level, employing a combined basis set of DGDZVP for Mo and 6-31+G(2df,p) for other atoms, are in better agreement with experimental (13)C NMR spectra. The electronic transitions calculated at the B3LYP/DGDZVP level by using TD-DFT method is in accordance with the observed UV-visible spectrum of the compound. Copyright © 2012 Elsevier B.V. All rights reserved.

Experimental solid state NMR of gas hydrates : problems and solutions

Energy Technology Data Exchange (ETDEWEB)

Moudrakovski, I.; Lu, H.; Ripmeester, J. [National Research Council of Canada, Ottawa, ON (Canada). Steacie Inst. for Molecular Sciences; Kumar, R.; Susilo, R. [British Columbia Univ., Vancouver, BC (Canada). Dept. of Chemical and Biological Engineering; Luzi, M. [GeoForschungsZentrum Potsdam, Potsdam (Germany)

2008-07-01

Solid State NMR is a suitable spectroscopic technique for hydrate research for several reasons, including its capability to distinguish between different structural types of hydrates, its quantitative nature and potential for both in-situ and time resolved experiments. This study illustrated the applications of solid state NMR for compositional and structural studies of clathrate hydrates, with particular emphasis on experimental techniques and potential ways to overcome technical difficulties. In order to use the method to its full capacity, some instrumental developments are needed to adapt it to the specific experimental requirements of hydrate studies, such as very low temperatures and high pressures. This presentation discussed the quantification of the Carbon-13 spectra with examples from natural and synthetic hydrates prepared from multi-component mixtures of hydrocarbons. The main approach used for the first two examples was Carbon-13 NMR with Magic Angle Spinning (MAS) at -100 degrees C. The detailed characterization of mixed hydrogen hydrates required low temperature hydrogen MAS. The quantification problems encountered during these experiments were also discussed. The purpose of these recent experimental developments was to prompt wider application of Solid State NMR in hydrate research. NMR proved to be a viable method for analyzing the composition and structure of multi-component mixed gas hydrates; characterizing natural gas hydrates; and, evaluating the formation conditions and properties of mixed hydrogen hydrates. The limitations of the method were highlighted and sensible choices of experimental conditions and techniques that ensure accurate results were discussed. 34 refs., 10 figs.

The structure of phosphate and borosilicate glasses and their structural evolution at high temperatures as studied with solid state NMR spectroscopy: Phase separation, crystallisation and dynamic species exchange

International Nuclear Information System (INIS)

Wegner, S.; Van Wullen, L.; Tricot, G.; Tricot, G.

2010-01-01

In this contribution we present an in-depth study of the network structure of different phosphate based and borosilicate glasses and its evolution at high temperatures. Employing a range of advanced solid state NMR methodologies, complemented by the results of XPS, the structural motifs on short and intermediate length scales are identified. For the phosphate based glasses, at temperatures above the glass transition temperature Tg, structural relaxation processes and the devitrification of the glasses were monitored in situ employing MAS NMR spectroscopy and X-ray diffraction. Dynamic species exchange involving rapid P-O-P and P-O-Al bond breaking and reforming was observed employing in situ 27 Al and 31 P MAS NMR spectroscopy and could be linked to viscous flow. For the borosilicate glasses, an atomic scale investigation of the phase separation processes was possible in a combined effort of ex situ NMR studies on glass samples with different thermal histories and in situ NMR studies using high temperature MAS NMR spectroscopy including 11 B MAS, 29 Si MAS and in situ 29 Si{ 11 B} REAPDOR NMR spectroscopy. (authors)

NMR studies of bent DNA using {sup 13}C-enriched samples

Energy Technology Data Exchange (ETDEWEB)

Zimmer, D.P.; Crothers, D.M. [Yale Univ., New Haven, CT (United States)

1994-12-01

Bending of the DNA double helix can be brought about by introducing runs of adenines (A-tracts) in phase with the helical repeat of the DNA. The requirements for bending of DNA by A-tracts are that the length of the A-tract be greater than 3 base pairs and that the A-tracts must be in phase with the helical repeat (every 10 or 11 bp). Other factors, such as the number of adenines in the run, flanking sequences, and whether the A-tracts are phased with respect to the 5{prime}A or the 3{prime}A, have effects upon the degree of bending as assayed by electrophoretic mobility on native polyacrylamide gels. There are a number of models for bending A-tract DNA. The junction-bending model postulates that the structure of A-tracts is similar to the fiber diffraction structure of poly A, in which there is a significant degree of base pair tilt with respect to the helix axis. In this model, bending occurs at the junction between the A-tract and the B-form helix to allow favorable stacking interactions to occur. The bend of the helix could arise as a result of some other perturbation of B-form DNA by A-tracts, such as propeller twist; bending also could be due to a combination of factors. Our goal is to find the structural features of A-tracts responsible for bending of the helix by performing NMR on oligonucleotides containing A-tracts to obtain higher resolution structural data. One of the problems encountered in NMR structure determination of nucleic acids and other macromolecules is the assignment of resonances to nuclei. This procedure can be greatly facilitated through the use of {sup 13}C-enriched nucleic acid samples. We are developing a technique for the enzymatic synthesis of labeled DNA for NMR. The technique we are developing is similar to RNA labeling techniques already in use. The technique involves growth of methylotrophic bacteria on {sup 13}CH{sub 3}OH.

Advanced experimental and numerical techniques for cavitation erosion prediction

CERN Document Server

Chahine, Georges; Franc, Jean-Pierre; Karimi, Ayat

2014-01-01

This book provides a comprehensive treatment of the cavitation erosion phenomenon and state-of-the-art research in the field. It is divided into two parts. Part 1 consists of seven chapters, offering a wide range of computational and experimental approaches to cavitation erosion. It includes a general introduction to cavitation and cavitation erosion, a detailed description of facilities and measurement techniques commonly used in cavitation erosion studies, an extensive presentation of various stages of cavitation damage (including incubation and mass loss), and insights into the contribution of computational methods to the analysis of both fluid and material behavior. The proposed approach is based on a detailed description of impact loads generated by collapsing cavitation bubbles and a physical analysis of the material response to these loads. Part 2 is devoted to a selection of nine papers presented at the International Workshop on Advanced Experimental and Numerical Techniques for Cavitation Erosion (Gr...

New methods for the correction of 31P NMR spectra in in vivo NMR spectroscopy

International Nuclear Information System (INIS)

Starcuk, Z.; Bartusek, K.; Starcuk, Z. jr.

1994-01-01

The new methods for the correction of 31 P NMR spectra in vivo NMR spectroscopy have been performed. A method for the baseline correction of the spectra which represents a combination of time-domain and frequency-domain has been discussed.The method is very fast and efficient for minimization of base line artifacts of biological tissues impact

DNP-enhanced solid-state NMR spectroscopy of active pharmaceutical ingredients.

Science.gov (United States)

Zhao, Li; Pinon, Arthur C; Emsley, Lyndon; Rossini, Aaron J

2017-11-28

Solid-state NMR spectroscopy has become a valuable tool for the characterization of both pure and formulated active pharmaceutical ingredients (APIs). However, NMR generally suffers from poor sensitivity that often restricts NMR experiments to nuclei with favorable properties, concentrated samples, and acquisition of one-dimensional (1D) NMR spectra. Here, we review how dynamic nuclear polarization (DNP) can be applied to routinely enhance the sensitivity of solid-state NMR experiments by one to two orders of magnitude for both pure and formulated APIs. Sample preparation protocols for relayed DNP experiments and experiments on directly doped APIs are detailed. Numerical spin diffusion models illustrate the dependence of relayed DNP enhancements on the relaxation properties and particle size of the solids and can be used for particle size determination when the other factors are known. We then describe the advanced solid-state NMR experiments that have been enabled by DNP and how they provide unique insight into the molecular and macroscopic structure of APIs. For example, with large sensitivity gains provided by DNP, natural isotopic abundance, 13 C- 13 C double-quantum single-quantum homonuclear correlation NMR spectra of pure APIs can be routinely acquired. DNP also enables solid-state NMR experiments with unreceptive quadrupolar nuclei such as 2 H, 14 N, and 35 Cl that are commonly found in APIs. Applications of DNP-enhanced solid-state NMR spectroscopy for the molecular level characterization of low API load formulations such as commercial tablets and amorphous solid dispersions are described. Future perspectives for DNP-enhanced solid-state NMR experiments on APIs are briefly discussed. Copyright © 2017 John Wiley & Sons, Ltd.

Contributions of computational chemistry and biophysical techniques to fragment-based drug discovery.

Science.gov (United States)

Gozalbes, Rafael; Carbajo, Rodrigo J; Pineda-Lucena, Antonio

2010-01-01

In the last decade, fragment-based drug discovery (FBDD) has evolved from a novel approach in the search of new hits to a valuable alternative to the high-throughput screening (HTS) campaigns of many pharmaceutical companies. The increasing relevance of FBDD in the drug discovery universe has been concomitant with an implementation of the biophysical techniques used for the detection of weak inhibitors, e.g. NMR, X-ray crystallography or surface plasmon resonance (SPR). At the same time, computational approaches have also been progressively incorporated into the FBDD process and nowadays several computational tools are available. These stretch from the filtering of huge chemical databases in order to build fragment-focused libraries comprising compounds with adequate physicochemical properties, to more evolved models based on different in silico methods such as docking, pharmacophore modelling, QSAR and virtual screening. In this paper we will review the parallel evolution and complementarities of biophysical techniques and computational methods, providing some representative examples of drug discovery success stories by using FBDD.

Is Low-field NMR a Complementary Tool to GC-MS in Quality Control of Essential Oils? A Case Study

NARCIS (Netherlands)

Krause, Andre; Wu, Yu; Tian, Runtao; Beek, van Teris A.

2018-01-01

High-field NMR is an expensive and important quality control technique. In recent years, cheaper and simpler low-field NMR has become available as a new quality control technique. In this study, 60 MHz 1 H-NMR was compared with GC-MS and refractometry for the detection of adulteration of essential

Characterization of natural bentonite by NMR; Caracterizacao de bentonitas naturais por ressonancia magnetica nuclear

Energy Technology Data Exchange (ETDEWEB)

Leite, Sidnei Q.M.; Dieguez, Lidia C [Universidade Federal, Rio de Janeiro, RJ (Brazil). Coordenacao dos Programas de Pos-graduacao de Engenharia; Menezes, Sonia M.C. [PETROBRAS, Rio de Janeiro, RJ (Brazil). Centro de Pesquisas; San Gil, Rosane A.S. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Inst. de Quimica

1994-12-31

Solid state NMR as well as several other instrumental chemical analysis techniques were used in order to characterize two natural occurring bentonite. The methodology is described. The NMR spectra, together with the other used techniques suggest that the observed differences are due to iron inclusions in tetrahedral and octahedral sites 5 refs., 3 figs., 5 tabs.

The flexibility of SIMPSON and SIMMOL for numerical simulations in solid-and liquid-state NMR spectroscopy

International Nuclear Information System (INIS)

Vosegaard, T.; Malmendal, A.; Nielsen, N.C.

2002-01-01

Addressing the need for numerical simulations in the design and interpretation of advanced solid- and liquid-state NMR experiments, we present a number of novel features for numerical simulations based on the SIMPSON and SIMMOL open source software packages. Major attention is devoted to the flexibility of these Tcl-interfaced programs for numerical simulation of NMR experiments being complicated by demands for efficient powder averaging, large spin systems, and multiple-pulse rf irradiation. These features are exemplified by fast simulation of second-order quadrupolar powder patterns using crystallite interpolation, analysis of rotary resonance triple-quantum excitation for quadrupolar nuclei, iterative fitting of MQ-MAS spectra by combination of SIMIPSON and MINUIT, simulation of multiple-dimensional PISEMA-type correlation experiments for macroscopically oriented membrane proteins, simulation of Hartman-Hahn polarization transfers in liquid-state NMR, and visualization of the spin evolution under complex composite broad-band excitation pulses. (author)

Study by 31P NMR spectroscopy of the triacylglycerol degradation processes in olive oil with different heat-transfer mechanisms.

OpenAIRE

Lucas Torres, Covadonga; Pérez Martínez, Angel; Cabañas Galán, Beatriz; Moreno Moreno, Andrés

2014-01-01

The thermal degradation of olive oil using conventional and microwave heating under the same experimental conditions were compared. A powerful identification and quantification technique based on 31P NMR has been developed to characterise the differences between the minor components including diacylglycerol and free fatty acids in the heated samples. The 31P NMR spectra of the degraded olive oils, which contain single bondOH groups derivatised with a phosphorus reagent, showed that convention...

Evaluation of PHB nanocomposite by low field NMR

International Nuclear Information System (INIS)

Silva, Mariana Bruno Rocha e; Tavares, Maria Ines Bruno

2009-01-01

Poly(3-hydroxybutyrate) (PHB) based on nanocomposites containing different amounts of a commercial organically modified clay (viscogel B8) were prepared employing solution intercalation method. The relationship among the processing conditions; molecular structure and intermolecular interaction, between both nanocomposite components, were investigated using a nuclear magnetic resonance (NMR), as a part of characterization methodology, which has been used by Tavares et al. It involves the proton spin-lattice relaxation time, T1 H, by solid state nuclear magnetic resonance, employing low field NMR. X-ray diffraction was also employed because it is a conventional technique, generally used to obtain the first information on nanocomposite formation. Changes in PHB crystallinity were observed after the organophilic nanoclay had been incorporated in the polymer matrix. These changes, in the microstructure, were detected by the variation of proton nuclear relaxation time values and by X-ray, which showed an increase in the clay interlamellar space due to the intercalation of the polymer in the clay between lamellae. (author)

NMR relaxation rate in quasi one-dimensional antiferromagnets

Science.gov (United States)

Capponi, Sylvain; Dupont, Maxime; Laflorencie, Nicolas; Sengupta, Pinaki; Shao, Hui; Sandvik, Anders W.

We compare results of different numerical approaches to compute the NMR relaxation rate 1 /T1 in quasi one-dimensional (1d) antiferromagnets. In the purely 1d regime, recent numerical simulations using DMRG have provided the full crossover behavior from classical regime at high temperature to universal Tomonaga-Luttinger liquid at low-energy (in the gapless case) or activated behavior (in the gapped case). For quasi 1d models, we can use mean-field approaches to reduce the problem to a 1d one that can be studied using DMRG. But in some cases, we can also simulate the full microscopic model using quantum Monte-Carlo techniques. This allows to compute dynamical correlations in imaginary time and we will discuss recent advances to perform stochastic analytic continuation to get real frequency spectra. Finally, we connect our results to experiments on various quasi 1d materials.

Flow units from integrated WFT and NMR data

Energy Technology Data Exchange (ETDEWEB)

Kasap, E.; Altunbay, M.; Georgi, D.

1997-08-01

Reliable and continuous permeability profiles are vital as both hard and soft data required for delineating reservoir architecture. They can improve the vertical resolution of seismic data, well-to-well stratigraphic correlations, and kriging between the well locations. In conditional simulations, permeability profiles are imposed as the conditioning data. Variograms, covariance functions and other geostatistical indicators are more reliable when based on good quality permeability data. Nuclear Magnetic Resonance (NMR) logging and Wireline Formation Tests (WFT) separately generate a wealth of information, and their synthesis extends the value of this information further by providing continuous and accurate permeability profiles without increasing the cost. NMR and WFT data present a unique combination because WFTs provide discrete, in situ permeability based on fluid-flow, whilst NMR responds to the fluids in the pore space and yields effective porosity, pore-size distribution, bound and moveable fluid saturations, and permeability. The NMR permeability is derived from the T{sub 2}-distribution data. Several equations have been proposed to transform T{sub 2} data to permeability. Regardless of the transform model used, the NMR-derived permeabilities depend on interpretation parameters that may be rock specific. The objective of this study is to integrate WFT permeabilities with NMR-derived, T{sub 2} distribution-based permeabilities and thereby arrive at core quality, continuously measured permeability profiles. We outlined the procedures to integrate NMR and WFT data and applied the procedure to a field case. Finally, this study advocates the use of hydraulic unit concepts to extend the WFT-NMR derived, core quality permeabilities to uncored intervals or uncored wells.

Solid state NMR of spin-1/2 nuclei

International Nuclear Information System (INIS)

Wind, R.A.

1991-01-01

The detection of nuclear magnetic resonance by Bloch et al. and Purcell and co-workers in 1946 has led to the development of one of the most powerful spectroscopic techniques known today. The reason is that, besides the applied external magnetic field, a nuclear spin also experiences extra local magnetic fields, which are due to surrounding electron clouds (the chemical shift) and other spins. These local fields differ for nuclei located at chemically different positions in a molecule. The result is that an NMR spectrum often consists of several lines, which can be considered to be a fingerprint of the material under investigation an can assist the clarifying its molecular structure. NMR has been especially successful in liquids and liquid like materials, where fast molecular tumblings average out the anisotropies in the local fields, resulting in well-resolved NMR spectra. This paper reports that initially the development of solid-state NMR was less dramatic. Originally, for reasons of sensitivity, attention was focused mainly on 1 H NMR. The result is that the NMR spectrum usually consists of single, broad, featureless line, which, except for special cases such as more or less isolated spin pairs or methyl groups, does not provide much information

Synthesis, Multinuclear NMR Characterization and Dynamic Property of Organic–Inorganic Hybrid Electrolyte Membrane Based on Alkoxysilane and Poly(oxyalkylene Diamine

Directory of Open Access Journals (Sweden)

Hsien-Ming Kao

2012-06-01

Full Text Available Organic–inorganic hybrid electrolyte membranes based on poly(propylene glycol-block-poly(ethylene glycol-block-poly(propylene glycol bis(2-aminopropyl ether complexed with LiClO₄ via the co-condensation of tetraethoxysilane (TEOS and 3-(triethoxysilylpropyl isocyanate have been prepared and characterized. A variety of techniques such as differential scanning calorimetry (DSC, Fourier transform infrared (FTIR spectroscopy, alternating current (AC impedance and solid-state nuclear magnetic resonance (NMR spectroscopy are performed to elucidate the relationship between the structural and dynamic properties of the hybrid electrolyte and the ion mobility. A VTF (Vogel-Tamman-Fulcher-like temperature dependence of ionic conductivity is observed for all the compositions studied, implying that the diffusion of charge carriers is assisted by the segmental motions of the polymer chains. A maximum ionic conductivity value of 5.3 × 10⁻⁵ Scm⁻¹ is obtained at 30 °C. Solid-state NMR results provide a microscopic view of the effects of salt concentrations on the dynamic behavior of the polymer chains.

Method of T2 spectrum inversion with conjugate gradient algorithm from NMR data

International Nuclear Information System (INIS)

Li Pengju; Shi Shangming; Song Yanjie

2010-01-01

Based on the optimization techniques, the T 2 spectrum inversion method of conjugate gradient that is easy to realize non-negativity constraint of T2 spectrum is proposed. The method transforms the linear mixed-determined problem of T2 spectrum inversion into the typical optimization problem of searching the minimum of objective function by building up the objective function according to the basic idea of geophysics modeling. The optimization problem above is solved with the conjugate gradient algorithm that has quick convergence rate and quadratic termination. The method has been applied to the inversion of noise free echo train generated from artificial spectrum, artificial echo train with signal-to-noise ratio (SNR)=25 and NMR experimental data of drilling core. The comparison between the inversion results of this paper and artificial spectrum or the result of software imported in NMR laboratory shows that the method can correctly invert T 2 spectrum from artificial NMR relaxation data even though SNR=25 and that inversion T 2 spectrum with good continuity and smoothness from core NMR experimental data accords perfectly with that of laboratory software imported, and moreover,the absolute error between the NMR porosity computed from T 2 spectrum and helium (He) porosity in laboratory is 0.65%. (authors)

Solid state NMR method development and studies of biological and biomimetic nanocomposites

Energy Technology Data Exchange (ETDEWEB)

Hu, Yanyan [Iowa State Univ., Ames, IA (United States)

2011-01-01

This thesis describes application and development of advanced solid-state nuclear magnetic resonance techniques for complex materials, in particular organic-inorganic nanocomposites and thermoelectric tellurides. The apatite-collagen interface, essential for understanding the biomineralization process in bone and engineering the interface for controlled bio-mimetic synthesis and optimized mechanical properties, is buried within the nanocomposite of bone. We used multinuclear solid-state NMR to study the composition and structure of the interface. Citrate has been identified as the main organic molecule strongly bound to the apatite surface with a density of 1/(2 nm)², covering 1/6 of the total surface area in bovine bone. Citrate provides more carboxylate groups, one of the key functional groups found to affect apatite nucleation and growth, than all the non-collagenous proteins all together in bone; thus we propose that citrate stabilizes apatite crystals at a very small thickness of ~3 nm (4 unit cells) to increase bone fracture tolerance. The hypothesis has been confirmed in vitro by adding citrate in the bio-mimetic synthesis of polymerhydroxyapatite nanocomposites. The results have shown that the size of hydroxyapatite nanocrystals decreases as increasing citrate concentration. With citrate concentrations comparable to that in body fluids, similar-sized nanocrystals as in bone have been produced. Besides the dimensions of the apatite crystals, the composition of bone also affects its biofunctional and macroscopic mechanical properties; therefore, our team also extended its effort to enhance the inorganic portion in our bio-mimetic synthesis from originally 15 wt% to current 50 wt% compared to 65 wt% in bovine bone, by using Lysine-Leucine hydroxyapatite nucleating diblock co-polypeptide, which forms a gel at very low concentration. In this thesis, various advanced solid state NMR techniques have been employed to characterize nanocomposites

NMR studies of phase behaviour in polyacrylonitrile solutions

International Nuclear Information System (INIS)

Golightly, J.A.

1998-10-01

The aim of the thesis was to study the phase behaviour of aqueous polyacrylonitrile/NaSCN solutions using a variety of nuclear magnetic resonance techniques. Polyacrylonitrile (PAN) is the basis of the acrylic fibre industry, as such fibres contain at least 85% PAN. Despite this industrial importance, the available literature describing the phase behaviour of PAN in solution is far from comprehensive. Bulk 1 H NMR relaxation measurements were carried out over a wide range of concentrations and temperatures to probe the molecular dynamics of the PAN and water molecules. The relaxation data was found to be biexponential decay for all samples, the relative amplitudes of which were shown to be equal to the ratio of PAN protons to water protons. Both species were found to be in the regime of rapid molecular motion. Bulk 1 H NMR self diffusion measurements, using the PFGSTE technique, exhibited a bi-exponential decay of the echo amplitudes. By careful selection of the observation time, Δ, it was possible to independently probe the water and PAN translational diffusion. A background gradient, resulting from inhomogeneities of the magnetic field, complicated the analysis of the data and a novel polynomial least squares fitting procedure was devised to overcome this effect. The measured attenuation of the water diffusion coefficients (D∼10 -6 -10 -5 cm 2 s -1 ) with increasing PAN volume fraction was modelled according to various theories, including free volume and scaling laws. The study of the PAN diffusion coefficient (D∼10 -7 -10 -6 cm 2 s -1 ) was limited by the experimental constraints of the NMR spectrometer. A 1 H NMR one-dimensional imaging technique was used to study the non-solvent induced phase separation (coagulation) of a PAN solution. The time dependence of the measured profiles allowed observation of the coagulation process. A diffusion model was developed to fit the experimental data using a semi-infinite diffusion framework. The fitting parameters

Fourier transform NMR

International Nuclear Information System (INIS)

Hallenga, K.

1991-01-01

This paper discusses the concept of Fourier transformation one of the many precious legacies of the French mathematician Jean Baptiste Joseph Fourier, essential for understanding the link between continuous-wave (CW) and Fourier transform (FT) NMR. Although in modern FT NMR the methods used to obtain a frequency spectrum from the time-domain signal may vary greatly, from the efficient Cooley-Tukey algorithm to very elaborate iterative least-square methods based other maximum entropy method or on linear prediction, the principles for Fourier transformation are unchanged and give invaluable insight into the interconnection of many pairs of physical entities called Fourier pairs

Application of NMR Screening Methods with 19F Detection to Fluorinated Compounds Bound to Proteins

Directory of Open Access Journals (Sweden)

Kazuo Furihata

2017-12-01

Full Text Available The combinational use of one-dimensional (1D NMR-based screening techniques with 1H and 19F detections were applied to a human serum albumin–diflunisal complex. Since most NMR screening methods observe 1H spectra, the overlapped 1H signals were unavailable in the binding epitope mapping. However, the NMR experiments with 19F detection can be used as an effective complementary method. For the purpose of identifying the 1H and 19F binding epitopes of diflunisal, this paper carries out a combinatorial analysis using 1H{1H} and 19F{1H} saturation transfer difference experiments. The differences of the 1H-inversion recovery rates with and without target irradiation are also analyzed for a comprehensive interpretation of binding epitope mapping.

Advanced techniques using the plant as indicator of irrigation management

Directory of Open Access Journals (Sweden)

Barbara dos Santos Esteves

2015-05-01

Full Text Available The methodologies which are considered the most promising for irrigation management are those based on the analysis of the water status of the plants themselves. This justifies the study and improvement of indicators based on automatic and continuous measures to enable real-time monitoring data, as indices from sap flow, dendrometry and leaf turgor pressure techniques. The aim of this paper is to analyze such methodologies in order to demonstrate their principles, advantages and challenges. In conclusion, the methodologies analyzed still have many technological advances and challenges before being presented to the final user. The future research should work these tools for elaboration of technical indexes that allow their simplification, on the instrumental point of view, and the interpretation of their results.

A Preliminary Investigation of NSCL/P Plasma and Urine in Guizhou Province in China Using NMR-Based Metabonomics.

Science.gov (United States)

Lei, Huang Guang; Hong, Luo; Kun, Song Ju; Hai, Yin Xin; Dong, Wang Ya; Ke, Zhao; Ping, Xu; Hao, Chen

2013-09-01

Objective : To assess the feasibility of metabonomics in clinical studies. This is a pilot study introducing nuclear magnetic resonance (NMR)-based metabonomics to elucidate and compare the metabolism of patients with nonsyndromic cleft lip and/or palate (NSCL/P) and children without orofacial clefts. Methods : High-resolution (1)H NMR spectroscopy was performed on plasma and urine samples obtained from NSCL/P and healthy children. The (1)H NMR spectra were further analyzed with principal component analysis. Results : Compared to the control group, the level of low-molecular-weight metabolites in plasma such as asparagine was higher in NSCL/P patients, while arginine, lysine, acetate, lactate, proline, glutamine, pyruvate, creatinine, choline, and β-glucose were lower. The carnitine, citrate, and formate excretion in urine appeared to be higher in the healthy children, while the NSCL/P group excreted higher concentrations of aspartic acid and phenylalanine in urine. Conclusion : The present study clearly demonstrated the great potential of NMR-based metabonomics in elucidating NSCL/P plasma metabolism and the possible application of this technology in clinical diagnosis and screening.

ARDENT to develop advanced dosimetric techniques

CERN Document Server

Antonella Del Rosso

2012-01-01

Earlier this week, the EU-supported Marie Curie training network ARDENT kicked off at a meeting held at CERN. The overall aim of the project is the development of advanced instrumentation for radiation dosimetry. The applications range from radiation measurements around particle accelerators, onboard commercial flights and in space, to the characterization of radioactive waste and medicine, where accurate dosimetry is of vital importance.   The ARDENT (Advanced Radiation Dosimetry European Network Training) project is both a research and a training programme, which aims at developing new dosimetric techniques while providing 15 Early-Stage Researchers (ESR) with state-of-the-art training. The project, coordinated by CERN, is funded by the European Union with a contribution of about 3.9 million euros over four years. The ARDENT initiative will focus on three main technologies: gas detectors, in particular Gas Electron Multipliers (GEM) and Tissue Equivalent Proportional Counters (TEPC); solid stat...

Nuclear magnetic resonance (NMR): principles and applications

International Nuclear Information System (INIS)

Quibilan, E.I.

The basis for the phenomenon of nuclear magnetic resonance (NMR) is the ability of certain nuclei possessing both intrinsic angular momentum or ''spin'' I and magnetic moment to absorb electromagnetic energy in the radio frequency range. In principle, there are approximately 200 nuclei which may be investigated using the NMR technique. The NMR spectrum consists of intensity peaks along an axis calibrated in terms of the steady magnetic field or the frequency of the radiofrequency electromagnetic radiation. Analysis of the number, spacing, position and intensity of the lines in an NMR spectrum consists of intensity peaks along an axis calibrated in terms of the steady magnetic field or the frequency of the radiofrequency electromagnetic radiation. Analysis of the number, spacing, position and intensity of the lines in an NMR spectrum provides a variety of qualitative and quantitative analytical applications. The most obvious applications consist of the measurements of nuclear properties, such as spin number and nuclear magnetic moment. In liquids, the fine structure of resonance spectra provides a tool for chemical identification and molecular structure analysis. Other applications include the measurements of self-diffusion coefficients, magnetic fields and field homogeneity, inter-nuclear distances, and, in some cases, the water content of biological materials. (author)

A single-board NMR spectrometer based on a software defined radio architecture

International Nuclear Information System (INIS)

Tang, Weinan; Wang, Weimin

2011-01-01

A single-board software defined radio (SDR) spectrometer for nuclear magnetic resonance (NMR) is presented. The SDR-based architecture, realized by combining a single field programmable gate array (FPGA) and a digital signal processor (DSP) with peripheral radio frequency (RF) front-end circuits, makes the spectrometer compact and reconfigurable. The DSP, working as a pulse programmer, communicates with a personal computer via a USB interface and controls the FPGA through a parallel port. The FPGA accomplishes digital processing tasks such as a numerically controlled oscillator (NCO), digital down converter (DDC) and gradient waveform generator. The NCO, with agile control of phase, frequency and amplitude, is part of a direct digital synthesizer that is used to generate an RF pulse. The DDC performs quadrature demodulation, multistage low-pass filtering and gain adjustment to produce a bandpass signal (receiver bandwidth from 3.9 kHz to 10 MHz). The gradient waveform generator is capable of outputting shaped gradient pulse waveforms and supports eddy-current compensation. The spectrometer directly acquires an NMR signal up to 30 MHz in the case of baseband sampling and is suitable for low-field (<0.7 T) application. Due to the featured SDR architecture, this prototype has flexible add-on ability and is expected to be suitable for portable NMR systems

Influence of Freezing and Storage Procedure on Human Urine Samples in NMR-Based Metabolomics

Directory of Open Access Journals (Sweden)

Burkhard Luy

2013-04-01

Full Text Available It is consensus in the metabolomics community that standardized protocols should be followed for sample handling, storage and analysis, as it is of utmost importance to maintain constant measurement conditions to identify subtle biological differences. The aim of this work, therefore, was to systematically investigate the influence of freezing procedures and storage temperatures and their effect on NMR spectra as a potentially disturbing aspect for NMR-based metabolomics studies. Urine samples were collected from two healthy volunteers, centrifuged and divided into aliquots. Urine aliquots were frozen either at −20 °C, on dry ice, at −80 °C or in liquid nitrogen and then stored at −20 °C, −80 °C or in liquid nitrogen vapor phase for 1–5 weeks before NMR analysis. Results show spectral changes depending on the freezing procedure, with samples frozen on dry ice showing the largest deviations. The effect was found to be based on pH differences, which were caused by variations in CO2 concentrations introduced by the freezing procedure. Thus, we recommend that urine samples should be frozen at −20 °C and transferred to lower storage temperatures within one week and that freezing procedures should be part of the publication protocol.

Influence of Freezing and Storage Procedure on Human Urine Samples in NMR-Based Metabolomics.

Science.gov (United States)

Rist, Manuela J; Muhle-Goll, Claudia; Görling, Benjamin; Bub, Achim; Heissler, Stefan; Watzl, Bernhard; Luy, Burkhard

2013-04-09

It is consensus in the metabolomics community that standardized protocols should be followed for sample handling, storage and analysis, as it is of utmost importance to maintain constant measurement conditions to identify subtle biological differences. The aim of this work, therefore, was to systematically investigate the influence of freezing procedures and storage temperatures and their effect on NMR spectra as a potentially disturbing aspect for NMR-based metabolomics studies. Urine samples were collected from two healthy volunteers, centrifuged and divided into aliquots. Urine aliquots were frozen either at -20 °C, on dry ice, at -80 °C or in liquid nitrogen and then stored at -20 °C, -80 °C or in liquid nitrogen vapor phase for 1-5 weeks before NMR analysis. Results show spectral changes depending on the freezing procedure, with samples frozen on dry ice showing the largest deviations. The effect was found to be based on pH differences, which were caused by variations in CO2 concentrations introduced by the freezing procedure. Thus, we recommend that urine samples should be frozen at -20 °C and transferred to lower storage temperatures within one week and that freezing procedures should be part of the publication protocol.

Ehrlich and sarcoma 180 tumour characterisation and early detection by 1H NMR-based metabonomics of mice serum

International Nuclear Information System (INIS)

Grandizoli, Caroline W.P. da S.; Simonelli, Fabio; Nagata, Noemi; Barison, Andersson; Carrenho, Luise Z.B.; Francisco, Thais M.G. de; Campos, Francinete R.; Santana Filho, Arquimedes P. de; Sassaki, Guilherme L.; Kreuger, Maria R.O.

2014-01-01

The success of cancer treatment is directly related to early detection before symptoms emerge, although nowadays few cancers can be detected early. In this sense, 1 H nuclear magnetic resonance ( 1 H NMR)-based metabonomics was used to identify metabolic changes in biofluid as a consequence of tumours growing in mice. Through partial least squares discriminant analysis (PLS-DA) analysis of 1 H NMR spectra from serum samples it was possible to diagnose Ehrlich ascites and Sarcoma 180 tumours five and ten days after cell inoculation, respectively. Lipids, lipoproteins and lactate were the main biomarkers at onset as well as in the progress of carcinogenic process. Thus, NMR-based metabonomics can be a valuable tool to study the effects of tumour establishment on the chemical composition of biofluids. (author)

Metabolite profiling of Clinacanthus nutans leaves extracts obtained from different drying methods by 1H NMR-based metabolomics

Science.gov (United States)

Hashim, Noor Haslinda Noor; Latip, Jalifah; Khatib, Alfi

2016-11-01

The metabolites of Clinacanthus nutans leaves extracts and their dependence on drying process were systematically characterized using 1H nuclear magnetic resonance spectroscopy (NMR) multivariate data analysis. Principal component analysis (PCA) and partial least square-discriminant analysis (PLS-DA) were able to distinguish the leaves extracts obtained from different drying methods. The identified metabolites were carbohydrates, amino acid, flavonoids and sulfur glucoside compounds. The major metabolites responsible for the separation in PLS-DA loading plots were lupeol, cycloclinacosides, betulin, cerebrosides and choline. The results showed that the combination of 1H NMR spectroscopy and multivariate data analyses could act as an efficient technique to understand the C. nutans composition and its variation.

Biosynthetic origin of acetic acid using SNIF-NMR; Determinacao da origem biossintetica de acido acetico atraves da tecnica 'Site Specific Natural Isotopic Fractionation Studied by Nuclear Magnetic Resonance (SNIF-NMR)'

Energy Technology Data Exchange (ETDEWEB)

Boffo, Elisangela Fabiana; Ferreira, Antonio Gilberto [Sao Carlos Univ., SP (Brazil). Dept. de Quimica

2006-05-15

The main purpose of this work is to describe the use of the technique Site-Specific Natural Isotopic Fractionation of hydrogen (SNIF-NMR), using {sup 2}H and {sup 1}H NMR spectroscopy, to investigate the biosynthetic origin of acetic acid in commercial samples of Brazilian vinegar. This method is based on the deuterium to hydrogen ratio at a specific position (methyl group) of acetic acitained by fermentation, through different biosynthetic mechanisms, which result in different isotopic ratios. We measured the isotopic ratio of vinegars obtained through C{sub 3}, C{sub 4}, and CAM biosynthetic mechanisms, blends of C{sub 3} and C{sub 4} (agrins) and synthetic acetic acid. (author)

Applications of NMR to studies of tissue metabolism

International Nuclear Information System (INIS)

Avison, M.J.; Hetherington, H.P.; Shulman, R.G.

1986-01-01

From its beginnings as a tool for the elucidation of biochemical pathways and bioenergetic status in unicellular organisms, the field of NMR studie in vivo has grown to encompass not only the study of isolated perfused organs, but also the study of various aspects of the biochemistry, physiology, and pathophysiology of these same organs in the intact animal. In recent years several groups have begun to extend the techniques developed in animals to the study of clinically relevant conditions in humans. A comprehensive review of all areas of NMR studies in vivo would be either unacceptably long or very superficial. For this reason the authors have restricted this review to studies published since 1980, except where an earlier study is particularly relevant to the topic under discussion. Furthermore, they have concentrated on areas that have been extending the scope of NMR in vivo. One specific omission is review of NMR studies of tumors, since a comprehensive review has recently appeared

Automated sequence-specific protein NMR assignment using the memetic algorithm MATCH

International Nuclear Information System (INIS)

Volk, Jochen; Herrmann, Torsten; Wuethrich, Kurt

2008-01-01

MATCH (Memetic Algorithm and Combinatorial Optimization Heuristics) is a new memetic algorithm for automated sequence-specific polypeptide backbone NMR assignment of proteins. MATCH employs local optimization for tracing partial sequence-specific assignments within a global, population-based search environment, where the simultaneous application of local and global optimization heuristics guarantees high efficiency and robustness. MATCH thus makes combined use of the two predominant concepts in use for automated NMR assignment of proteins. Dynamic transition and inherent mutation are new techniques that enable automatic adaptation to variable quality of the experimental input data. The concept of dynamic transition is incorporated in all major building blocks of the algorithm, where it enables switching between local and global optimization heuristics at any time during the assignment process. Inherent mutation restricts the intrinsically required randomness of the evolutionary algorithm to those regions of the conformation space that are compatible with the experimental input data. Using intact and artificially deteriorated APSY-NMR input data of proteins, MATCH performed sequence-specific resonance assignment with high efficiency and robustness

Recent advances on Charpy specimen reconstitution techniques

Energy Technology Data Exchange (ETDEWEB)

Andrade, Arnaldo H.P.; Lobo, Raquel M.; Miranda, Carlos Alexandre J., E-mail: aandrade@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

2017-07-01

Charpy specimen reconstitution is widely used around the world as a tool to enhance or supplement surveillance programs of nuclear reactor pressure vessels. The reconstitution technique consists in the incorporation of a small piece from a previously tested specimen into a compound specimen, allowing to increase the number of tests. This is especially important if the available materials is restricted and fracture mechanics parameter have to be determined. The reconstitution technique must fulfill some demands, among them tests results like the original standard specimens and the loaded material of the insert must not be influenced by the welding and machining procedure. It is known that reconstitution of Charpy specimens may affect the impact energy in a consequence of the constraint of plastic deformation by the hardened weldment and HAZ. This paper reviews some recent advances of the reconstitution technique and its applications. (author)

Recent advances on Charpy specimen reconstitution techniques

International Nuclear Information System (INIS)

Andrade, Arnaldo H.P.; Lobo, Raquel M.; Miranda, Carlos Alexandre J.

2017-01-01

Charpy specimen reconstitution is widely used around the world as a tool to enhance or supplement surveillance programs of nuclear reactor pressure vessels. The reconstitution technique consists in the incorporation of a small piece from a previously tested specimen into a compound specimen, allowing to increase the number of tests. This is especially important if the available materials is restricted and fracture mechanics parameter have to be determined. The reconstitution technique must fulfill some demands, among them tests results like the original standard specimens and the loaded material of the insert must not be influenced by the welding and machining procedure. It is known that reconstitution of Charpy specimens may affect the impact energy in a consequence of the constraint of plastic deformation by the hardened weldment and HAZ. This paper reviews some recent advances of the reconstitution technique and its applications. (author)

NMR investigation and theoretical calculations of the solvent effect on the conformation of valsartan

Science.gov (United States)

Chashmniam, Saeed; Tafazzoli, Mohsen

2017-11-01

Structure and conformational properties of valsartan were studied by advanced NMR techniques and quantum calculation methods. Potential energy scanning using B3LYP/6-311++g** and B3LYP-D3/6-311++g** methods were performed and four conformers (V1-V4) at minimum points of PES diagram were observed. According to the NMR spectra in acetone-d6, there are two conformers (M and m) with m/M = 0.52 ratio simultaneously and energy barriers of the two conformers were predicted from chemical shifts and multiplicities. While, intramolecular hydrogen bond at tetrazole ring and carboxylic groups prevent the free rotation on N6sbnd C11 bond in M-conformer, this bond rotates freely in m-conformer. On the other hand, intramolecular hydrogen bond at carbonyl and carboxylic acid can be observed at m-conformer. So, different intramolecular hydrogen bond is the reason for the stability of both M and m structures. Quite interestingly, 1H NMR spectra in CDCl3 show two distinct conformers (N and n) with unequal ratio which are differ from M-m conformers. Also, intramolecular hydrogen bond seven-member ring involving five-membered tetrazole ring and carboxylic acid group observed in both N and n-conformers Solvent effect, by using a set of polar and non-polar solvents including DMSO-d6, methanol-d4, benzene-d6, THF-d8, nitromethane-d3, methylene chloride-d2 and acetonitrile-d3 were investigated. NMR parameters include chemical shifts and spin-spin coupling constants were obtained from a set of 2D NMR spectra (H-H COSY, HMQC and HMBC). For this purpose, several DFT functionals from LDA, GGA and hybrid categories were used which the hybrid method showed better agreement with experiment values.

Increasing rigor in NMR-based metabolomics through validated and open source tools.

Science.gov (United States)

Eghbalnia, Hamid R; Romero, Pedro R; Westler, William M; Baskaran, Kumaran; Ulrich, Eldon L; Markley, John L

2017-02-01

The metabolome, the collection of small molecules associated with an organism, is a growing subject of inquiry, with the data utilized for data-intensive systems biology, disease diagnostics, biomarker discovery, and the broader characterization of small molecules in mixtures. Owing to their close proximity to the functional endpoints that govern an organism's phenotype, metabolites are highly informative about functional states. The field of metabolomics identifies and quantifies endogenous and exogenous metabolites in biological samples. Information acquired from nuclear magnetic spectroscopy (NMR), mass spectrometry (MS), and the published literature, as processed by statistical approaches, are driving increasingly wider applications of metabolomics. This review focuses on the role of databases and software tools in advancing the rigor, robustness, reproducibility, and validation of metabolomics studies. Copyright © 2016. Published by Elsevier Ltd.

SpecPad: device-independent NMR data visualization and processing based on the novel DART programming language and Html5 Web technology.

Science.gov (United States)

Guigas, Bruno

2017-09-01

SpecPad is a new device-independent software program for the visualization and processing of one-dimensional and two-dimensional nuclear magnetic resonance (NMR) time domain (FID) and frequency domain (spectrum) data. It is the result of a project to investigate whether the novel programming language DART, in combination with Html5 Web technology, forms a suitable base to write an NMR data evaluation software which runs on modern computing devices such as Android, iOS, and Windows tablets as well as on Windows, Linux, and Mac OS X desktop PCs and notebooks. Another topic of interest is whether this technique also effectively supports the required sophisticated graphical and computational algorithms. SpecPad is device-independent because DART's compiled executable code is JavaScript and can, therefore, be run by the browsers of PCs and tablets. Because of Html5 browser cache technology, SpecPad may be operated off-line. Network access is only required during data import or export, e.g. via a Cloud service, or for software updates. A professional and easy to use graphical user interface consistent across all hardware platforms supports touch screen features on mobile devices for zooming and panning and for NMR-related interactive operations such as phasing, integration, peak picking, or atom assignment. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Visualising substrate-fingermark interactions: Solid-state NMR spectroscopy of amino acid reagent development on cellulose substrates.

Science.gov (United States)

Spindler, Xanthe; Shimmon, Ronald; Roux, Claude; Lennard, Chris

2015-05-01

Most spectroscopic studies of the reaction products formed by ninhydrin, 1,2-indanedione-zinc (Ind-Zn) and 1,8-diazafluoren-9-one (DFO) when reacted with amino acids or latent fingermarks on paper substrates are focused on visible absorption or luminescence spectroscopy. In addition, structural elucidation studies are typically limited to solution-based mass spectrometry or liquid nuclear magnetic resonance (NMR) spectroscopy, which does not provide an accurate representation of the fingermark development process on common paper substrates. The research presented in this article demonstrates that solid-state carbon-13 magic angle spinning NMR ((13)C-MAS-NMR) is a technique that can not only be utilised for structural studies of fingermark enhancement reagents, but is a promising technique for characterising the effect of paper chemistry on fingermark deposition and enhancement. The latter opens up a research area that has been under-explored to date but has the potential to improve our understanding of how fingermark secretions and enhancement reagents interact with paper substrates. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

NMR-based approach to the analysis of radiopharmaceuticals: radiochemical purity, specific activity, and radioactive concentration values by proton and tritium NMR spectroscopy.

Science.gov (United States)

Schenk, David J; Dormer, Peter G; Hesk, David; Pollack, Scott R; Lavey, Carolee Flader

2015-06-15

Compounds containing tritium are widely used across the drug discovery and development landscape. These materials are widely utilized because they can be efficiently synthesized and produced at high specific activity. Results from internally calibrated (3)H and (1)H nuclear magnetic resonance (NMR) spectroscopy suggests that at least in some cases, this calibrated approach could supplement or potentially replace radio-high-performance liquid chromatography for radiochemical purity, dilution and scintillation counting for the measurement of radioactivity per volume, and liquid chromatography/mass spectrometry analysis for the determination of specific activity. In summary, the NMR-derived values agreed with those from the standard approaches to within 1% to 9% for solution count and specific activity. Additionally, the NMR-derived values for radiochemical purity deviated by less than 5%. A benefit of this method is that these values may be calculated at the same time that (3)H NMR analysis provides the location and distribution of tritium atoms within the molecule. Presented and discussed here is the application of this method, advantages and disadvantages of the approach, and a rationale for utilizing internally calibrated (1)H and (3)H NMR spectroscopy for specific activity, radioactive concentration, and radiochemical purity whenever acquiring (3)H NMR for tritium location. Copyright © 2015 John Wiley & Sons, Ltd.

Recommendations and Standardization of Biomarker Quantification Using NMR-based Metabolomics with Particular Focus on Urinary Analysis

KAUST Repository

Emwas, Abdul-Hamid M.

2016-01-08

NMR-based metabolomics has shown considerable promise in disease diagnosis and biomarker discovery because it allows one to non-destructively identify and quantify large numbers of novel metabolite biomarkers in both biofluids and tissues. Indeed, precise metabolite quantification is a necessary prerequisite to move any chemical biomarker or biomarker panel from the lab into the clinic. Among the many biofluids (urine, serum, plasma, cerebrospinal fluid and saliva) commonly used for disease diagnosis and prognosis, urine has several advantages. It is abundant, sterile, easily obtained, needs little sample preparation and does not require any invasive medical procedures for collection. Furthermore, urine captures and concentrates many “unwanted” or “undesirable” compounds throughout the body, thereby providing a rich source of potentially useful disease biomarkers. However, the incredible variation in urine chemical concentrations due to effects such as gender, age, diet, life style, health conditions, and physical activity make the analysis of urine and the identification of useful urinary biomarkers by NMR quite challenging. In this review, we discuss a number of the most significant issues regarding NMR-based urinary metabolomics with a specific emphasis on metabolite quantification for disease biomarker applications. We also propose a number of data collection and instrumental recommendations regarding NMR pulse sequences, acceptable acquisition parameter ranges, relaxation effects on quantitation, proper handling of instrumental differences, as well as recommendations regarding sample preparation and biomarker assessment.

Recommendations and Standardization of Biomarker Quantification Using NMR-based Metabolomics with Particular Focus on Urinary Analysis

KAUST Repository

Emwas, Abdul-Hamid M.; Roy, Raja; McKay, Ryan T.; Ryan, Danielle; Brennan, Lorraine; Tenori, Leonardo; Luchinat, Claudio; Gao, Xin; Zeri, Ana Carolina; Gowda, G. A. Nagana; Raftery, Daniel; Steinbeck, Christoph; Salek, Reza M; Wishart, David S.

2016-01-01

NMR-based metabolomics has shown considerable promise in disease diagnosis and biomarker discovery because it allows one to non-destructively identify and quantify large numbers of novel metabolite biomarkers in both biofluids and tissues. Indeed, precise metabolite quantification is a necessary prerequisite to move any chemical biomarker or biomarker panel from the lab into the clinic. Among the many biofluids (urine, serum, plasma, cerebrospinal fluid and saliva) commonly used for disease diagnosis and prognosis, urine has several advantages. It is abundant, sterile, easily obtained, needs little sample preparation and does not require any invasive medical procedures for collection. Furthermore, urine captures and concentrates many “unwanted” or “undesirable” compounds throughout the body, thereby providing a rich source of potentially useful disease biomarkers. However, the incredible variation in urine chemical concentrations due to effects such as gender, age, diet, life style, health conditions, and physical activity make the analysis of urine and the identification of useful urinary biomarkers by NMR quite challenging. In this review, we discuss a number of the most significant issues regarding NMR-based urinary metabolomics with a specific emphasis on metabolite quantification for disease biomarker applications. We also propose a number of data collection and instrumental recommendations regarding NMR pulse sequences, acceptable acquisition parameter ranges, relaxation effects on quantitation, proper handling of instrumental differences, as well as recommendations regarding sample preparation and biomarker assessment.

A new Schiff base compound N,N'-(2,2-dimetylpropane)-bis(dihydroxylacetophenone): synthesis, experimental and theoretical studies on its crystal structure, FTIR, UV-visible, 1H NMR and 13C NMR spectra.

Science.gov (United States)

Saheb, Vahid; Sheikhshoaie, Iran

2011-10-15

The Schiff base compound, N,N'-(2,2-dimetylpropane)-bis(dihydroxylacetophenone) (NDHA) is synthesized through the condensation of 2-hydroxylacetophenone and 2,2-dimethyl 1,3-amino propane in methanol at ambient temperature. The yellow crystalline precipitate is used for X-ray single-crystal determination and measuring Fourier transform infrared (FTIR), UV-visible, (1)H NMR and (13)C NMR spectra. Electronic structure calculations at the B3LYP, PBEPBE and PW91PW91 levels of theory are performed to optimize the molecular geometry and to calculate the FTIR, (1)H NMR and (13)C NMR spectra of the compound. Time-dependent density functional theory (TDDFT) method is used to calculate the UV-visible spectrum of NDHA. Vibrational frequencies are determined experimentally and compared with those obtained theoretically. Vibrational assignments and analysis of the fundamental modes of the compound are also performed. All theoretical methods can well reproduce the structure of the compound. The (1)H NMR and (13)C NMR chemical shifts calculated by all DFT methods are consistent with the experimental data. However, the NMR shielding tensors computed at the B3LYP/6-31+G(d,p) level of theory are in better agreement with experimental (1)H NMR and (13)C NMR spectra. The electronic absorption spectrum calculated at the B3LYP/6-31+G(d,p) level by using TD-DFT method is in accordance with the observed UV-visible spectrum of NDHA. In addition, some quantum descriptors of the molecule are calculated and conformational analysis is performed and the results were compared with the crystallographic data. Copyright © 2011 Elsevier B.V. All rights reserved.

Magnetic force microscopy: advanced technique for the observation of magnetic domains

International Nuclear Information System (INIS)

Asenjo, A.; Garcia, J. M.; Vazquez, M.

2001-01-01

An overview on the Magnetic Force Microscopy, MFM, as an advanced technique to observe magnetic domains and walls is displayed. Basic concepts are first introduced on the domain structure formation as well as on other techniques to observe magnetic domains. Afterwards, the MFM instrumentation is described making also an emphasis in micro magnetic consideration to interpret the images. Finally, a set of selected advanced magnetic materials with different domain structures is chosen to show the wide possibilities of this techniques to characterise the surface magnetic behaviour. The domain structure of materials as commercial magnetic recording media, thin films and multilayers, amorphous micro tubes, nanocrystalline ribbons, perovskites or magnetic nano wires is shown. (Author) 16 refs

Fiber Optic Surface Plasmon Resonance-Based Biosensor Technique: Fabrication, Advancement, and Application.

Science.gov (United States)

Liang, Gaoling; Luo, Zewei; Liu, Kunping; Wang, Yimin; Dai, Jianxiong; Duan, Yixiang

2016-05-03

Fiber optic-based biosensors with surface plasmon resonance (SPR) technology are advanced label-free optical biosensing methods. They have brought tremendous progress in the sensing of various chemical and biological species. This review summarizes four sensing configurations (prism, grating, waveguide, and fiber optic) with two ways, attenuated total reflection (ATR) and diffraction, to excite the surface plasmons. Meanwhile, the designs of different probes (U-bent, tapered, and other probes) are also described. Finally, four major types of biosensors, immunosensor, DNA biosensor, enzyme biosensor, and living cell biosensor, are discussed in detail for their sensing principles and applications. Future prospects of fiber optic-based SPR sensor technology are discussed.

Piperamides from Piper ottonoides by NMR and GC-MS based mixture analysis

International Nuclear Information System (INIS)

Wolff, Thiago; Valente, Ligia M.M.; Magalhães, Alvicler; Guimarães, Elsie F.

2015-01-01

The species Piper ottonoides Yuncker (Piperaceae), known as 'joão-brandim', is a shrub that occurs in the Brazilian Amazon rainforest. Its roots and leaves are used in traditional medicine as local anesthetic to treat toothache and sore throat. In this study, the structural characterization in mixture of isobutyl amides present in semi-purified fractions from fruits, leaves, stems and roots of P. ottonoides was achieved by employing gas chromatography-mass spectrometry (GC-MS) and a combination of nuclear magnetic resonance (NMR) techniques ( 1 H, 1 H- 1 H COSY, 1 H- 13 CHSQC, 1 H- 13 CHMBC, TOCSY and 1 H- 1 H J-RES). The MS fragmentation patterns and the NMR chemical shifts, multiplicities, coupling constants and the signal correlations in the two-dimensional spectra were carefully analyzed also taking into account some key elements of differentiation among the compounds. The data set allowed identifying unequivocally the new amide N-isobutyl-7-(4'- methoxyphenyl)-2E,4E-heptadienamide, which we named ottonoidenamide as well as piperovatine and chingchengenamide A in all parts of the plant, the additional presence of pipercallosine and pipercallosidine in roots and of dihydropiperlonguminine in fruits and leaves. The presence of piperovatine and pipercallosine in P. ottonoides should be associated to its traditional use. (author)

Advanced Packaging Materials and Techniques for High Power TR Module: Standard Flight vs. Advanced Packaging

Science.gov (United States)

Hoffman, James Patrick; Del Castillo, Linda; Miller, Jennifer; Jenabi, Masud; Hunter, Donald; Birur, Gajanana

2011-01-01

The higher output power densities required of modern radar architectures, such as the proposed DESDynI [Deformation, Ecosystem Structure, and Dynamics of Ice] SAR [Synthetic Aperture Radar] Instrument (or DSI) require increasingly dense high power electronics. To enable these higher power densities, while maintaining or even improving hardware reliability, requires advances in integrating advanced thermal packaging technologies into radar transmit/receive (TR) modules. New materials and techniques have been studied and compared to standard technologies.

Laser-based direct-write techniques for cell printing

Energy Technology Data Exchange (ETDEWEB)

Schiele, Nathan R; Corr, David T [Biomedical Engineering Department, Rensselaer Polytechnic Institute, Troy, NY (United States); Huang Yong [Department of Mechanical Engineering, Clemson University, Clemson, SC (United States); Raof, Nurazhani Abdul; Xie Yubing [College of Nanoscale Science and Engineering, University at Albany, SUNY, Albany, NY (United States); Chrisey, Douglas B, E-mail: schien@rpi.ed, E-mail: chrisd@rpi.ed [Material Science and Engineering Department, Rensselaer Polytechnic Institute, Troy, NY (United States)

2010-09-15

Fabrication of cellular constructs with spatial control of cell location ({+-}5 {mu}m) is essential to the advancement of a wide range of applications including tissue engineering, stem cell and cancer research. Precise cell placement, especially of multiple cell types in co- or multi-cultures and in three dimensions, can enable research possibilities otherwise impossible, such as the cell-by-cell assembly of complex cellular constructs. Laser-based direct writing, a printing technique first utilized in electronics applications, has been adapted to transfer living cells and other biological materials (e.g., enzymes, proteins and bioceramics). Many different cell types have been printed using laser-based direct writing, and this technique offers significant improvements when compared to conventional cell patterning techniques. The predominance of work to date has not been in application of the technique, but rather focused on demonstrating the ability of direct writing to pattern living cells, in a spatially precise manner, while maintaining cellular viability. This paper reviews laser-based additive direct-write techniques for cell printing, and the various cell types successfully laser direct-written that have applications in tissue engineering, stem cell and cancer research are highlighted. A particular focus is paid to process dynamics modeling and process-induced cell injury during laser-based cell direct writing. (topical review)

Laser-based direct-write techniques for cell printing

International Nuclear Information System (INIS)

Schiele, Nathan R; Corr, David T; Huang Yong; Raof, Nurazhani Abdul; Xie Yubing; Chrisey, Douglas B

2010-01-01

Fabrication of cellular constructs with spatial control of cell location (±5 μm) is essential to the advancement of a wide range of applications including tissue engineering, stem cell and cancer research. Precise cell placement, especially of multiple cell types in co- or multi-cultures and in three dimensions, can enable research possibilities otherwise impossible, such as the cell-by-cell assembly of complex cellular constructs. Laser-based direct writing, a printing technique first utilized in electronics applications, has been adapted to transfer living cells and other biological materials (e.g., enzymes, proteins and bioceramics). Many different cell types have been printed using laser-based direct writing, and this technique offers significant improvements when compared to conventional cell patterning techniques. The predominance of work to date has not been in application of the technique, but rather focused on demonstrating the ability of direct writing to pattern living cells, in a spatially precise manner, while maintaining cellular viability. This paper reviews laser-based additive direct-write techniques for cell printing, and the various cell types successfully laser direct-written that have applications in tissue engineering, stem cell and cancer research are highlighted. A particular focus is paid to process dynamics modeling and process-induced cell injury during laser-based cell direct writing. (topical review)

The search for neuroimaging biomarkers of Alzheimer's disease with advanced MRI techniques

International Nuclear Information System (INIS)

Li, Tie-Qiang; Wahlund, Lars-Olof

2011-01-01

The aim of this review is to examine the recent literature on using advanced magnetic resonance imaging (MRI) techniques for finding neuroimaging biomarkers that are sensitive to the detection of risks for Alzheimer's disease (AD). Since structural MRI techniques, such as brain structural volumetry and voxel based morphometry (VBM), have been widely used for AD studies and extensively reviewed, we will only briefly touch on the topics of volumetry and morphometry. The focus of the current review is about the more recent developments in the search for AD neuroimaging biomarkers with functional MRI (fMRI), resting-state functional connectivity MRI (fcMRI), diffusion tensor imaging (DTI), arterial spin-labeling (ASL), and magnetic resonance spectroscopy (MRS)

Camtasia Studio 8 advanced editing and publishing techniques

CERN Document Server

Dixon, Claire Broadley

2013-01-01

A practical guide packed with examples that will show you how to implement the different features of Camtasia Studio 8 and create professional looking projects.If you are familiar with Camtasia Studio and you want to experiment with more advanced techniques, then this is the guide you have been looking for!

Solid-state (49/47)Ti NMR of titanium-based MCM-41 hybrid materials.

Science.gov (United States)

Ballesteros, Ruth; Fajardo, Mariano; Sierra, Isabel; Force, Carmen; del Hierro, Isabel

2009-11-03

Titanium solid-state NMR spectroscopy data for a series of organic-inorganic titanium MCM-41 based materials have been collected. These materials have been synthesized by first modifying the mesoporous silica MCM-41 in one step with a mixture of silanes: a triazine propyl triethoxysilane acting as functional linker and methyltrimethoxysilane or hexamethyldisilizane as capped agents to mask the remaining silanol groups. Second, the appropiate titanium precursor Ti(OPr(i))(4), [{Ti(OPr(i))(3)(OMent)}(2)] (OMent = 1R,2S,5R-(-)-menthoxo), Ti(OPr(i))(4), or [Ti(eta(5)-C(5)HMe(4))Cl(3)], has been immobilized by reaction with the modified MCM-41. Finally, after Ti(OPr(i))(4) immobilization onto the organomodified support the reaction with the chiral (+)-diethyl-l-tartrate was accomplished. The materials without functional linker have been also prepared by reaction in one step of the capped agent and the titanium precursor with the mesoporous silica. Relevant correlations of titanium NMR resonance chemical shifts and line widths can be inferred depending on different factors. The immobilization procedure used to prepare titanium-based MCM-41 hybrid materials and the choice of the silylating reagents employed to mask the silanol groups present on the silica surfaces produce significant differences in the Ti NMR spectra. Furthermore, depending on the electronic and sterical influence of the substituents directly attached to the titanium center, chemical shifts and line widths are modified providing novel information about titanium structure.

Solid state NMR study of cumbaru flour

International Nuclear Information System (INIS)

Nogueira, Jose S.; Bathista, Andre L.B.S.; Silva, Emerson O.; Priante Filho, Nicolau; Tavares, Maria I.B.

2001-01-01

The polysaccharide obtained by seed of Dipteryx alata Vog, has been characterised by 13 C solid state, using the basic routine techniques, like MAS and CPMAS and by the proton spin-lattice relaxation time in the rotating frame parameter (T 1 H ρ). Knowing that the chemical structure and molecular dynamic are extremely necessary route to obtain information on the polysaccharides, this work contributes to the classification of the seed containing in the cumbaru fruit to get response on its application. To obtain the initial responses for our purposes some solid state NMR techniques were chosen. The CPMAS 13 C NMR spectrum of the polysaccharide was investigated to know if it has some crystallinity. The MAS 13 C NMR spectrum showed the presence of domains with distinct molecular mobility, because these domains will differ basically in the distribution size and chain packing. The variable contact time experiment was used to analyse the distribution form of 13 C decays, which give us more information about sample heterogeneity. The T 1 H ρHr values were obtained from the variable contact time and by delayed contact time experiment, because these parameter indicate the order of polysaccharides. From the values of this parameter, we found that this polysaccharide is completely non-ordered. (author)

[Non-invasive analysis of proteins in living cells using NMR spectroscopy].

Science.gov (United States)

Tochio, Hidehito; Murayama, Shuhei; Inomata, Kohsuke; Morimoto, Daichi; Ohno, Ayako; Shirakawa, Masahiro

2015-01-01

NMR spectroscopy enables structural analyses of proteins and has been widely used in the structural biology field in recent decades. NMR spectroscopy can be applied to proteins inside living cells, allowing characterization of their structures and dynamics in intracellular environments. The simplest "in-cell NMR" approach employs bacterial cells; in this approach, live Escherichia coli cells overexpressing a specific protein are subjected to NMR. The cells are grown in an NMR active isotope-enriched medium to ensure that the overexpressed proteins are labeled with the stable isotopes. Thus the obtained NMR spectra, which are derived from labeled proteins, contain atomic-level information about the structure and dynamics of the proteins. Recent progress enables us to work with higher eukaryotic cells such as HeLa and HEK293 cells, for which a number of techniques have been developed to achieve isotope labeling of the specific target protein. In this review, we describe successful use of electroporation for in-cell NMR. In addition, (19)F-NMR to characterize protein-ligand interactions in cells is presented. Because (19)F nuclei rarely exist in natural cells, when (19)F-labeled proteins are delivered into cells and (19)F-NMR signals are observed, one can safely ascertain that these signals originate from the delivered proteins and not other molecules.

Les écoulements par RMN à gradient pulsé Pulsed Gradient Nmr Techniques for Studying Flows

Directory of Open Access Journals (Sweden)

Lebon L.

2006-12-01

Full Text Available Nous présentons ici les techniques de RMN à gradient pulsé qui permettent d'étudier les écoulements multiphasiques en canalisation ou en milieu poreux. Les principaux avantages sont de pouvoir travailler sur des milieux non transparents et d'accéder à des échelles de longueurs faibles. On montre qu'il est possible d'obtenir des informations locales sur l'écoulement, telles que le profil de vitesse et ses fluctuations dans les écoulements diphasiques, ou les cartes de distribution des probabilités de déplacement dans des échantillons poreux hétérogènes. Pulsed gradient NMR techniques are presented here. They allow the study of multiphase flow in pipes as well as porous media. The main advantages are the possibilities of studying non transparent media at small length scales. We show that it is possible to obtain local information on the fluid flow, such as velocity profiles in two phase systems, or maps of distribution of displacement probabilities in heterogeneous porous media.

Recommended strategies for spectral processing and post-processing of 1D 1H-NMR data of biofluids with a particular focus on urine

KAUST Repository

Emwas, Abdul-Hamid M.

2018-02-12

1H NMR spectra from urine can yield information-rich data sets that offer important insights into many biological and biochemical phenomena. However, the quality and utility of these insights can be profoundly affected by how the NMR spectra are processed and interpreted. For instance, if the NMR spectra are incorrectly referenced or inconsistently aligned, the identification of many compounds will be incorrect. If the NMR spectra are mis-phased or if the baseline correction is flawed, the estimated concentrations of many compounds will be systematically biased. Furthermore, because NMR permits the measurement of concentrations spanning up to five orders of magnitude, several problems can arise with data analysis. For instance, signals originating from the most abundant metabolites may prove to be the least biologically relevant while signals arising from the least abundant metabolites may prove to be the most important but hardest to accurately and precisely measure. As a result, a number of data processing techniques such as scaling, transformation and normalization are often required to address these issues. Therefore, proper processing of NMR data is a critical step to correctly extract useful information in any NMR-based metabolomic study. In this review we highlight the significance, advantages and disadvantages of different NMR spectral processing steps that are common to most NMR-based metabolomic studies of urine. These include: chemical shift referencing, phase and baseline correction, spectral alignment, spectral binning, scaling and normalization. We also provide a set of recommendations for best practices regarding spectral and data processing for NMR-based metabolomic studies of biofluids, with a particular focus on urine.

Recommended strategies for spectral processing and post-processing of 1D 1H-NMR data of biofluids with a particular focus on urine

KAUST Repository

Emwas, Abdul-Hamid M.; Saccenti, Edoardo; Gao, Xin; McKay, Ryan T.; dos Santos, Vitor A. P. Martins; Roy, Raja; Wishart, David S.

2018-01-01

1H NMR spectra from urine can yield information-rich data sets that offer important insights into many biological and biochemical phenomena. However, the quality and utility of these insights can be profoundly affected by how the NMR spectra are processed and interpreted. For instance, if the NMR spectra are incorrectly referenced or inconsistently aligned, the identification of many compounds will be incorrect. If the NMR spectra are mis-phased or if the baseline correction is flawed, the estimated concentrations of many compounds will be systematically biased. Furthermore, because NMR permits the measurement of concentrations spanning up to five orders of magnitude, several problems can arise with data analysis. For instance, signals originating from the most abundant metabolites may prove to be the least biologically relevant while signals arising from the least abundant metabolites may prove to be the most important but hardest to accurately and precisely measure. As a result, a number of data processing techniques such as scaling, transformation and normalization are often required to address these issues. Therefore, proper processing of NMR data is a critical step to correctly extract useful information in any NMR-based metabolomic study. In this review we highlight the significance, advantages and disadvantages of different NMR spectral processing steps that are common to most NMR-based metabolomic studies of urine. These include: chemical shift referencing, phase and baseline correction, spectral alignment, spectral binning, scaling and normalization. We also provide a set of recommendations for best practices regarding spectral and data processing for NMR-based metabolomic studies of biofluids, with a particular focus on urine.

Measuring diffusion-relaxation correlation maps using non-uniform field gradients of single-sided NMR devices.

Science.gov (United States)

Nogueira d'Eurydice, Marcel; Galvosas, Petrik

2014-11-01

Single-sided NMR systems are becoming a relevant tool in industry and laboratory environments due to their low cost, low maintenance and capacity to evaluate quantity and quality of hydrogen based materials. The performance of such devices has improved significantly over the last decade, providing increased field homogeneity, field strength and even controlled static field gradients. For a class of these devices, the configuration of the permanent magnets provides a linear variation of the magnetic field and can be used in diffusion measurements. However, magnet design depends directly on its application and, according to the purpose, the field homogeneity may significantly be compromised. This may prevent the determination of diffusion properties of fluids based on the natural inhomogeneity of the field using known techniques. This work introduces a new approach that extends the applicability of diffusion-editing CPMG experiments to NMR devices with highly inhomogeneous magnetic fields, which do not vary linearly in space. Herein, we propose a method to determine a custom diffusion kernel based on the gradient distribution, which can be seen as a signature of each NMR device. This new diffusion kernel is then utilised in the 2D inverse Laplace transform (2D ILT) in order to determine diffusion-relaxation correlation maps of homogeneous multi-phasic fluids. The experiments were performed using NMR MObile Lateral Explore (MOLE), which is a single-sided NMR device designed to maximise the volume at the sweet spot with enhanced depth penetration. Copyright © 2014 Elsevier Inc. All rights reserved.

New dereplication method applied to NMR-Based metabolomics on different fusarium species isolated from Rhizosphere of Senna spectabilis

International Nuclear Information System (INIS)

Selegato, Denise M.; Castro-Gamboa, Ian; Freire, Rafael T.; Tannús, Alberto

2016-01-01

The search for new sources of natural products steadily increased the use of bioinformatics tools that enabled efficient analysis of complex matrices. In this context, dereplication methods emerged as a fast way of identifying known compounds, accelerating the identification of bioactive chemotypes. Although 1 H NMR is widely used as an analytical technique, few studies have been reported using it as a dereplication tool, primarily because of the spectral complexity. This work aims to create a new computational method that analyses 1 H NMR data from Fusarium solani and F. oxysporum isolated from Senna spectabilis' srhizosphere through principal component analysis (PCA). The algorithm uses loading values to select important peaks that distinguish both species in PCA, allowing compound dereplication, even in highly similar profiles. As a result, the method, associated with other NMR experiments and information from an in-house Fusarium's metabolite library was able to distinguish different mycotoxins produced by both fungi, identifying fusaric acid and beauvericin for F. oxysporum and the depsipeptide HA23 from F. solani. (author)

New dereplication method applied to NMR-Based metabolomics on different fusarium species isolated from Rhizosphere of Senna spectabilis

Energy Technology Data Exchange (ETDEWEB)

Selegato, Denise M.; Castro-Gamboa, Ian, E-mail: ian.castro@gmail.com [Universidade Estadual Paulista Júlio de Mesquita Filho (NuBBE/UNESP), Araraquara, SP (Brazil). Núcleo de Bioensaios, Biossíntese e Ecofisiologia de Produtos Naturais; Freire, Rafael T.; Tannús, Alberto [Universidade de São Paulo (CIERMag/USP), São Carlos, SP (Brazil). Centro de Imagens e Espectroscopia in Vivo por Ressonância Magnética

2016-07-01

The search for new sources of natural products steadily increased the use of bioinformatics tools that enabled efficient analysis of complex matrices. In this context, dereplication methods emerged as a fast way of identifying known compounds, accelerating the identification of bioactive chemotypes. Although {sup 1}H NMR is widely used as an analytical technique, few studies have been reported using it as a dereplication tool, primarily because of the spectral complexity. This work aims to create a new computational method that analyses {sup 1}H NMR data from Fusarium solani and F. oxysporum isolated from Senna spectabilis' srhizosphere through principal component analysis (PCA). The algorithm uses loading values to select important peaks that distinguish both species in PCA, allowing compound dereplication, even in highly similar profiles. As a result, the method, associated with other NMR experiments and information from an in-house Fusarium's metabolite library was able to distinguish different mycotoxins produced by both fungi, identifying fusaric acid and beauvericin for F. oxysporum and the depsipeptide HA23 from F. solani. (author)

Overcoming the solubility limit with solubility-enhancement tags: successful applications in biomolecular NMR studies

International Nuclear Information System (INIS)

Zhou Pei; Wagner, Gerhard

2010-01-01

Although the rapid progress of NMR technology has significantly expanded the range of NMR-trackable systems, preparation of NMR-suitable samples that are highly soluble and stable remains a bottleneck for studies of many biological systems. The application of solubility-enhancement tags (SETs) has been highly effective in overcoming solubility and sample stability issues and has enabled structural studies of important biological systems previously deemed unapproachable by solution NMR techniques. In this review, we provide a brief survey of the development and successful applications of the SET strategy in biomolecular NMR. We also comment on the criteria for choosing optimal SETs, such as for differently charged target proteins, and recent new developments on NMR-invisible SETs.

NMR imaging and spectroscopy of the mammalian central nervous system after heavy ion radiation

International Nuclear Information System (INIS)

Richards, T.

1984-09-01

NMR imaging, NMR spectroscopic, and histopathologic techniques were used to study the proton relaxation time and related biochemical changes in the central nervous system after helium beam in vivo irradiation of the rodent brain. The spectroscopic observations reported in this dissertation were made possible by development of methods for measuring the NMR parameters of the rodent brain in vivo and in vitro. The methods include (1) depth selective spectroscopy using an optimization of rf pulse energy based on a priori knowledge of N-acetyl aspartate and lipid spectra of the normal brain, (2) phase-encoded proton spectroscopy of the living rodent using a surface coil, and (3) dual aqueous and organic tissue extraction technique for spectroscopy. Radiation induced increases were observed in lipid and p-choline peaks of the proton spectrum, in vivo. Proton NMR spectroscopy measurements on brain extracts (aqueous and organic solvents) were made to observe chemical changes that could not be seen in vivo. Radiation-induced changes were observed in lactate, GABA, glutamate, and p-choline peak areas of the aqueous fraction spectra. In the organic fraction, decreases were observed in peak area ratios of the terminal-methyl peaks, the N-methyl groups of choline, and at a peak at 2.84 ppM (phosphatidyl ethanolamine and phosphatidyl serine resonances) relative to TMS. With histology and Evans blue injections, blood-brain barrier alternations were seen as early as 4 days after irradiation. 83 references, 53 figures

NMR imaging and spectroscopy of the mammalian central nervous system after heavy ion radiation

Energy Technology Data Exchange (ETDEWEB)

Richards, T.

1984-09-01

NMR imaging, NMR spectroscopic, and histopathologic techniques were used to study the proton relaxation time and related biochemical changes in the central nervous system after helium beam in vivo irradiation of the rodent brain. The spectroscopic observations reported in this dissertation were made possible by development of methods for measuring the NMR parameters of the rodent brain in vivo and in vitro. The methods include (1) depth selective spectroscopy using an optimization of rf pulse energy based on a priori knowledge of N-acetyl aspartate and lipid spectra of the normal brain, (2) phase-encoded proton spectroscopy of the living rodent using a surface coil, and (3) dual aqueous and organic tissue extraction technique for spectroscopy. Radiation induced increases were observed in lipid and p-choline peaks of the proton spectrum, in vivo. Proton NMR spectroscopy measurements on brain extracts (aqueous and organic solvents) were made to observe chemical changes that could not be seen in vivo. Radiation-induced changes were observed in lactate, GABA, glutamate, and p-choline peak areas of the aqueous fraction spectra. In the organic fraction, decreases were observed in peak area ratios of the terminal-methyl peaks, the N-methyl groups of choline, and at a peak at 2.84 ppM (phosphatidyl ethanolamine and phosphatidyl serine resonances) relative to TMS. With histology and Evans blue injections, blood-brain barrier alternations were seen as early as 4 days after irradiation. 83 references, 53 figures.

NMR studies of electrophoretic mobility in surfactant systems

International Nuclear Information System (INIS)

Conveney, F.M.; Strange, J.H.; Smith, A.L.; Smith, E.G.

1989-01-01

An experimental technique is described in which the flow of electrically charged micelles is measured in the presence of an applied electric field using an NMR technique. The method is used to determine the electrophoretic mobility at ambient temperature of a 5% aqueous solution of sodium dodecyl sulphate and is shown to provide a new technique for the study of electrophoresis in surfactant solutions. (author). 8 refs.; 4 figs

Ameliorating effects of Mango (Mangifera indica L.) fruit on plasma ethanol level in a mouse model assessed with 1H-NMR based metabolic profiling

Science.gov (United States)

Kim, So-Hyun; K. Cho, Somi; Min, Tae-Sun; Kim, Yujin; Yang, Seung-Ok; Kim, Hee-Su; Hyun, Sun-Hee; Kim, Hana; Kim, Young-Suk; Choi, Hyung-Kyoon

2011-01-01

The ameliorating effects of Mango (Mangifera indica L.) flesh and peel samples on plasma ethanol level were investigated using a mouse model. Mango fruit samples remarkably decreased mouse plasma ethanol levels and increased the activities of alcohol dehydrogenase and acetaldehyde dehydrogenase. The 1H-NMR-based metabolomic technique was employed to investigate the differences in metabolic profiles of mango fruits, and mouse plasma samples fed with mango fruit samples. The partial least squares-discriminate analysis of 1H-NMR spectral data of mouse plasma demonstrated that there were clear separations among plasma samples from mice fed with buffer, mango flesh and peel. A loading plot demonstrated that metabolites from mango fruit, such as fructose and aspartate, might stimulate alcohol degradation enzymes. This study suggests that mango flesh and peel could be used as resources for functional foods intended to decrease plasma ethanol level after ethanol uptake. PMID:21562641

Advanced flow MRI: emerging techniques and applications

International Nuclear Information System (INIS)

Markl, M.; Schnell, S.; Wu, C.; Bollache, E.; Jarvis, K.; Barker, A.J.; Robinson, J.D.; Rigsby, C.K.

2016-01-01

Magnetic resonance imaging (MRI) techniques provide non-invasive and non-ionising methods for the highly accurate anatomical depiction of the heart and vessels throughout the cardiac cycle. In addition, the intrinsic sensitivity of MRI to motion offers the unique ability to acquire spatially registered blood flow simultaneously with the morphological data, within a single measurement. In clinical routine, flow MRI is typically accomplished using methods that resolve two spatial dimensions in individual planes and encode the time-resolved velocity in one principal direction, typically oriented perpendicular to the two-dimensional (2D) section. This review describes recently developed advanced MRI flow techniques, which allow for more comprehensive evaluation of blood flow characteristics, such as real-time flow imaging, 2D multiple-venc phase contrast MRI, four-dimensional (4D) flow MRI, quantification of complex haemodynamic properties, and highly accelerated flow imaging. Emerging techniques and novel applications are explored. In addition, applications of these new techniques for the improved evaluation of cardiovascular (aorta, pulmonary arteries, congenital heart disease, atrial fibrillation, coronary arteries) as well as cerebrovascular disease (intra-cranial arteries and veins) are presented.

Combining NMR and small angle X-ray and neutron scattering in the structural analysis of a ternary protein-RNA complex

International Nuclear Information System (INIS)

Hennig, Janosch; Wang, Iren; Sonntag, Miriam; Gabel, Frank; Sattler, Michael

2013-01-01

Many processes in the regulation of gene expression and signaling involve the formation of protein complexes involving multi-domain proteins. Individual domains that mediate protein-protein and protein-nucleic acid interactions are typically connected by flexible linkers, which contribute to conformational dynamics and enable the formation of complexes with distinct binding partners. Solution techniques are therefore required for structural analysis and to characterize potential conformational dynamics. Nuclear magnetic resonance spectroscopy (NMR) provides such information but often only sparse data are obtained with increasing molecular weight of the complexes. It is therefore beneficial to combine NMR data with additional structural restraints from complementary solution techniques. Small angle X-ray/neutron scattering (SAXS/SANS) data can be efficiently combined with NMR-derived information, either for validation or by providing additional restraints for structural analysis. Here, we show that the combination of SAXS and SANS data can help to refine structural models obtained from data-driven docking using HADDOCK based on sparse NMR data. The approach is demonstrated with the ternary protein-protein-RNA complex involving two RNA recognition motif (RRM) domains of Sex-lethal, the N-terminal cold shock domain of Upstream-to-N-Ras, and msl-2 mRNA. Based on chemical shift perturbations we have mapped protein-protein and protein-RNA interfaces and complemented this NMR-derived information with SAXS data, as well as SANS measurements on subunit-selectively deuterated samples of the ternary complex. Our results show that, while the use of SAXS data is beneficial, the additional combination with contrast variation in SANS data resolves remaining ambiguities and improves the docking based on chemical shift perturbations of the ternary protein-RNA complex.

Combining NMR and small angle X-ray and neutron scattering in the structural analysis of a ternary protein-RNA complex

Energy Technology Data Exchange (ETDEWEB)

Hennig, Janosch; Wang, Iren; Sonntag, Miriam [Institute of Structural Biology, Helmholtz Zentrum Muenchen (Germany); Gabel, Frank [Extremophiles and Large Molecular Assemblies Group (ELMA), Institut de Biologie Structurale (IBS) CEA-CNRS-UJF (France); Sattler, Michael, E-mail: sattler@helmholtz-muenchen.de [Institute of Structural Biology, Helmholtz Zentrum Muenchen (Germany)

2013-05-15

Many processes in the regulation of gene expression and signaling involve the formation of protein complexes involving multi-domain proteins. Individual domains that mediate protein-protein and protein-nucleic acid interactions are typically connected by flexible linkers, which contribute to conformational dynamics and enable the formation of complexes with distinct binding partners. Solution techniques are therefore required for structural analysis and to characterize potential conformational dynamics. Nuclear magnetic resonance spectroscopy (NMR) provides such information but often only sparse data are obtained with increasing molecular weight of the complexes. It is therefore beneficial to combine NMR data with additional structural restraints from complementary solution techniques. Small angle X-ray/neutron scattering (SAXS/SANS) data can be efficiently combined with NMR-derived information, either for validation or by providing additional restraints for structural analysis. Here, we show that the combination of SAXS and SANS data can help to refine structural models obtained from data-driven docking using HADDOCK based on sparse NMR data. The approach is demonstrated with the ternary protein-protein-RNA complex involving two RNA recognition motif (RRM) domains of Sex-lethal, the N-terminal cold shock domain of Upstream-to-N-Ras, and msl-2 mRNA. Based on chemical shift perturbations we have mapped protein-protein and protein-RNA interfaces and complemented this NMR-derived information with SAXS data, as well as SANS measurements on subunit-selectively deuterated samples of the ternary complex. Our results show that, while the use of SAXS data is beneficial, the additional combination with contrast variation in SANS data resolves remaining ambiguities and improves the docking based on chemical shift perturbations of the ternary protein-RNA complex.

'In vivo' and high resolution spectroscopy in solids by NMR: an instrument for transgenic plants study

International Nuclear Information System (INIS)

Colnago, L.A.; Herrmann, P.S.P.; Bernardes Filho, R.

1995-01-01

This work has developed a study on transgenic plants using two different techniques of nuclear magnetic resonance, in vivo NMR and high resolution NMR. In order to understand the gene mutations and characterize the plants constituents, NMR spectral data were analysed and discussed, then the results were presented

NMR-based pharmacometabonomics: A new paradigm for personalised or precision medicine

OpenAIRE

Everett, Jeremy R.

2017-01-01

Metabolic profiling by NMR spectroscopy or hyphenated mass spectrometry, known as metabonomics or metabolomics, is an important tool for systems-based approaches in biology and medicine. The experiments are typically done in a diagnostic fashion where changes in metabolite profiles are interpreted as a consequence of an intervention or event; be that a change in diet, the administration of a drug, physical exertion or the onset of a disease. By contrast, pharmacometabonomics takes a prognosti...

SPE-NMR metabolite sub-profiling of urine

NARCIS (Netherlands)

Jacobs, D.M.; Spiesser, L.; Garnier, M.; Roo, de N.; Dorsten, van F.; Hollebrands, B.; Velzen, van E.; Draijer, R.; Duynhoven, van J.P.M.

2012-01-01

NMR-based metabolite profiling of urine is a fast and reproducible method for detection of numerous metabolites with diverse chemical properties. However, signal overlap in the (1)H NMR profiles of human urine may hamper quantification and identification of metabolites. Therefore, a new method has

Advanced Techniques in Web Intelligence-2 Web User Browsing Behaviour and Preference Analysis

CERN Document Server

Palade, Vasile; Jain, Lakhmi

2013-01-01

This research volume focuses on analyzing the web user browsing behaviour and preferences in traditional web-based environments, social  networks and web 2.0 applications,  by using advanced  techniques in data acquisition, data processing, pattern extraction and  cognitive science for modeling the human actions.  The book is directed to  graduate students, researchers/scientists and engineers  interested in updating their knowledge with the recent trends in web user analysis, for developing the next generation of web-based systems and applications.

¹²⁹ Xe NMR Relaxation-Based Macromolecular Sensing

Energy Technology Data Exchange (ETDEWEB)

Gomes, Muller D. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Materials Sciences Division; Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Dao, Phuong [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Materials Sciences Division; Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Jeong, Keunhong [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Materials Sciences Division; Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Slack, Clancy C. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Materials Sciences Division; Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Vassiliou, Christophoros C. [Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Finbloom, Joel A. [Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Francis, Matthew B. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Materials Sciences Division; Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Wemmer, David E. [Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Physical Biosciences Division; Pines, Alexander [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Materials Sciences Division; Univ. of California, Berkeley, CA (United States). Dept. of Chemistry

2016-07-29

A ¹²⁹Xe NMR relaxation-based sensing approach is reported on that exploits changes in the bulk xenon relaxation rate induced by slowed tumbling of a cryptophane-based sensor upon target binding. The amplification afforded by detection of the bulk dissolved xenon allows sensitive detection of targets. The sensor comprises a xenon-binding cryptophane cage, a target interaction element, and a metal chelating agent. Xenon associated with the target-bound cryptophane cage is rapidly relaxed and then detected after exchange with the bulk. Here we show that large macromolecular targets increase the rotational correlation time of xenon, increasing its relaxation rate. Upon binding of a biotin-containing sensor to avidin at 1.5 μM concentration, the free xenon T₂ is reduced by a factor of 4.

NMR of insensitive nuclei enhanced by dynamic nuclear polarization.

Science.gov (United States)

Miéville, Pascal; Jannin, Sami; Helm, Lothar; Bodenhausen, Geoffrey

2011-01-01

Despite the powerful spectroscopic information it provides, Nuclear Magnetic Resonance (NMR) spectroscopy suffers from a lack of sensitivity, especially when dealing with nuclei other than protons. Even though NMR can be applied in a straightforward manner when dealing with abundant protons of organic molecules, it is very challenging to address biomolecules in low concentration and/or many other nuclei of the periodic table that do not provide as intense signals as protons. Dynamic Nuclear Polarization (DNP) is an important technique that provides a way to dramatically increase signal intensities in NMR. It consists in transferring the very high electron spin polarization of paramagnetic centers (usually at low temperature) to the surrounding nuclear spins with appropriate microwave irradiation. DNP can lead to an enhancement of the nuclear spin polarization by up to four orders of magnitude. We present in this article some basic concepts of DNP, describe the DNP apparatus at EPFL, and illustrate the interest of the technique for chemical applications by reporting recent measurements of the kinetics of complexation of 89Y by the DOTAM ligand.

[Advanced online search techniques and dedicated search engines for physicians].

Science.gov (United States)

Nahum, Yoav

2008-02-01

In recent years search engines have become an essential tool in the work of physicians. This article will review advanced search techniques from the world of information specialists, as well as some advanced search engine operators that may help physicians improve their online search capabilities, and maximize the yield of their searches. This article also reviews popular dedicated scientific and biomedical literature search engines.

POC-scale testing of an advanced fine coal dewatering equipment/technique

Energy Technology Data Exchange (ETDEWEB)

Groppo, J.G.; Parekh, B.K. [Univ. of Kentucky, Lexington, KY (United States); Rawls, P. [Department of Energy, Pittsburgh, PA (United States)

1995-11-01

Froth flotation technique is an effective and efficient process for recovering of ultra-fine (minus 74 {mu}m) clean coal. Economical dewatering of an ultra-fine clean coal product to a 20 percent level moisture will be an important step in successful implementation of the advanced cleaning processes. This project is a step in the Department of Energy`s program to show that ultra-clean coal could be effectively dewatered to 20 percent or lower moisture using either conventional or advanced dewatering techniques. As the contract title suggests, the main focus of the program is on proof-of-concept testing of a dewatering technique for a fine clean coal product. The coal industry is reluctant to use the advanced fine coal recovery technology due to the non-availability of an economical dewatering process. in fact, in a recent survey conducted by U.S. DOE and Battelle, dewatering of fine clean coal was identified as the number one priority for the coal industry. This project will attempt to demonstrate an efficient and economic fine clean coal slurry dewatering process.

Hyperpolarized Xenon Nuclear Magnetic Resonance (NMR of Building Stone Materials

Directory of Open Access Journals (Sweden)

Michele Mauri

2012-09-01

Full Text Available We have investigated several building stone materials, including minerals and rocks, using continuous flow hyperpolarized xenon (CF-HP NMR spectroscopy to probe the surface composition and porosity. Chemical shift and line width values are consistent with petrographic information. Rare upfield shifts were measured and attributed to the presence of transition metal cations on the surface. The evolution of freshly cleaved rocks exposed to the atmosphere was also characterized. The CF-HP 129Xe NMR technique is non-destructive and it could complement currently used techniques, like porosimetry and microscopy, providing additional information on the chemical nature of the rock surface and its evolution.

Advanced Laser-Based Techniques for Gas-Phase Diagnostics in Combustion and Aerospace Engineering.

Science.gov (United States)

Ehn, Andreas; Zhu, Jiajian; Li, Xuesong; Kiefer, Johannes

2017-03-01

Gaining information of species, temperature, and velocity distributions in turbulent combustion and high-speed reactive flows is challenging, particularly for conducting measurements without influencing the experimental object itself. The use of optical and spectroscopic techniques, and in particular laser-based diagnostics, has shown outstanding abilities for performing non-intrusive in situ diagnostics. The development of instrumentation, such as robust lasers with high pulse energy, ultra-short pulse duration, and high repetition rate along with digitized cameras exhibiting high sensitivity, large dynamic range, and frame rates on the order of MHz, has opened up for temporally and spatially resolved volumetric measurements of extreme dynamics and complexities. The aim of this article is to present selected important laser-based techniques for gas-phase diagnostics focusing on their applications in combustion and aerospace engineering. Applicable laser-based techniques for investigations of turbulent flows and combustion such as planar laser-induced fluorescence, Raman and Rayleigh scattering, coherent anti-Stokes Raman scattering, laser-induced grating scattering, particle image velocimetry, laser Doppler anemometry, and tomographic imaging are reviewed and described with some background physics. In addition, demands on instrumentation are further discussed to give insight in the possibilities that are offered by laser flow diagnostics.

Non-Uniform Sampling and J-UNIO Automation for Efficient Protein NMR Structure Determination.

Science.gov (United States)

Didenko, Tatiana; Proudfoot, Andrew; Dutta, Samit Kumar; Serrano, Pedro; Wüthrich, Kurt

2015-08-24

High-resolution structure determination of small proteins in solution is one of the big assets of NMR spectroscopy in structural biology. Improvements in the efficiency of NMR structure determination by advances in NMR experiments and automation of data handling therefore attracts continued interest. Here, non-uniform sampling (NUS) of 3D heteronuclear-resolved [(1)H,(1)H]-NOESY data yielded two- to three-fold savings of instrument time for structure determinations of soluble proteins. With the 152-residue protein NP_372339.1 from Staphylococcus aureus and the 71-residue protein NP_346341.1 from Streptococcus pneumonia we show that high-quality structures can be obtained with NUS NMR data, which are equally well amenable to robust automated analysis as the corresponding uniformly sampled data. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The NMR probe of high-Tc materials and correlated electron systems

CERN Document Server

Walstedt, Russell E

2018-01-01

This new edition updates readers in three areas of NMR studies, namely, recent developments in high-Tc materials, heavy fermion systems and actinide oxides are presented.  The NMR probe has yielded a vast array of data for solid state materials, corresponding to different compounds, ionic sites, and nuclear species, as well as to a wide variety of experimental conditions. The last two parts of the book are completely new in this edition, while the first part has seen major updates. This edition features the latest developments for high-Tc materials, especially the advances in the area of pseudogap studies are reviewed.  An in depth overview of heavy fermion systems is presented in the second part,  notably Kondo lattices, quantum critical points and unconventional superconductivity are areas of intense research recently and are covered extensively. Finally, valuable information from NMR studies with actinide oxides will be provided. Ongoing analysis and discussion of NMR data have resulted in a wealth o...

Proton NMR imaging in experimental ischemic infarction

International Nuclear Information System (INIS)

Buonanno, F.S.; Pykett, I.L.; Brady, T.J.; Vielma, J.; Burt, C.T.; Goldman, M.R.; Hinshaw, W.S.; Pohost, G.M.; Kistler, J.P.

1983-01-01

Proton nuclear magnetic resonance (NMR) images depict the distribution and concentration of mobile protons modified by the relaxation times T1 and T2. Using the steady-state-free-precession (SSFP) technique, serial coronal images were obtained sequentially over time in laboratory animals with experimental ischemic infarction. Image changes were evident as early as 2 hours after carotid artery ligation, and corresponded to areas of ischemic infarction noted pathologically. Resulting SSFP images in experimental stroke are contrasted to inversion-recovery NMR images in an illustrative patient with established cerebral infarction. Bulk T1 and T2 measurements were made in vitro in three groups of gerbils: normal, those with clinical evidence of infarction, and those clinically normal after carotid ligature. Infarcted hemispheres had significantly prolonged T1 and T2 (1.47 +/- .12 sec, 76.0 +/- 9.0 msec, respectively) when compared to the contralateral hemisphere (T1 . 1.28 +/- .05 sec, T2 . 58.7 +/- 3.9 msec) or to the other two groups. These data suggest that changes in NMR parameters occur and can be detected by NMR imaging as early as two hours after carotid artery ligation

Ehrlich and sarcoma 180 tumour characterisation and early detection by {sup 1}H NMR-based metabonomics of mice serum

Energy Technology Data Exchange (ETDEWEB)

Grandizoli, Caroline W.P. da S.; Simonelli, Fabio; Nagata, Noemi; Barison, Andersson [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Quimica; Carrenho, Luise Z.B.; Francisco, Thais M.G. de; Campos, Francinete R. [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Farmacia; Santana Filho, Arquimedes P. de; Sassaki, Guilherme L. [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Bioquimica; Kreuger, Maria R.O. [Universidade do Vale do Itajai (UNIVALI), (Brazil). Centro de Ciencias da Saude

2014-05-15

The success of cancer treatment is directly related to early detection before symptoms emerge, although nowadays few cancers can be detected early. In this sense, {sup 1}H nuclear magnetic resonance ({sup 1}H NMR)-based metabonomics was used to identify metabolic changes in biofluid as a consequence of tumours growing in mice. Through partial least squares discriminant analysis (PLS-DA) analysis of {sup 1}H NMR spectra from serum samples it was possible to diagnose Ehrlich ascites and Sarcoma 180 tumours five and ten days after cell inoculation, respectively. Lipids, lipoproteins and lactate were the main biomarkers at onset as well as in the progress of carcinogenic process. Thus, NMR-based metabonomics can be a valuable tool to study the effects of tumour establishment on the chemical composition of biofluids. (author)

NMR imaging of bladder tumors in males. Preliminary clinical experience

International Nuclear Information System (INIS)

Sigal, R.; Rein, A.J.J.T.; Atlan, H.; Lanir, A.; Kedar, S.; Segal, S.

1985-01-01

Nuclear magnetic resonance (NMR) of the normal and pathologic bladder was performed in 10 male subjects: 5 normal volunteers, 4 with bladder primary carcinoma, 1 with bladder metastasis. All scanning was done using a superconductive magnet operating at 0.5 T. Spin echo was used as pulse sequence. The diagnosis was confirmed in all cases by NMR imaging. The ability of the technique to provide images in axial, sagital and coronal planes allowed a precise assessment of the morphology and the size of the tumors. The lack of hazards and the quality of images may promote NMR imaging to a prominent role in the diagnosis of human bladder cancer [fr

Advanced CFD and radiotracer techniques - A complementary technology - for industrial multiphase applications

International Nuclear Information System (INIS)

Tu, J.Y.

2004-01-01

A CFD and RTD Education Package was developed, in which lecture notes, tutorials and computer softwares for both CFD and RTD are included. A user-friendly web-based interface has been prepared to allow lecturers more effectively conducting their training courses or workshops, and to provide students or users more easily learning the CFD and RTD knowledge and practising computer softwares. This report gives an overview of the advances in development and use of CFD models and codes for industrial, particularly multiphase processing applications. Experimental needs for validation and improvement of CFD models and softwares are highlighted. Integration of advanced CFD modelling with radiotracer techniques as a complementary technology for future research and industrial applications is discussed. The features and examples of the developed CFD and RTD Education package are presented. (author)

Recent research in flaxseed (oil seed) on molecular structure and metabolic characteristics of protein, heat processing-induced effect and nutrition with advanced synchrotron-based molecular techniques.

Science.gov (United States)

Doiron, Kevin J; Yu, Peiqiang

2017-01-02

Advanced synchrotron radiation-based infrared microspectroscopy is able to reveal feed and food structure feature at cellular and molecular levels and simultaneously provides composition, structure, environment, and chemistry within intact tissue. However, to date, this advanced synchrotron-based technique is still seldom known to food and feed scientists. This article aims to provide detailed background for flaxseed (oil seed) protein research and then review recent progress and development in flaxseed research in ruminant nutrition in the areas of (1) dietary inclusion of flaxseed in rations; (2) heat processing effect; (3) assessing dietary protein; (4) synchrotron-based Fourier transform infrared microspectroscopy as a tool of nutritive evaluation within cellular and subcellular dimensions; (5) recent synchrotron applications in flaxseed research on a molecular basis. The information described in this paper gives better insight in flaxseed research progress and update.

1H NMR-Based Metabolomic Analysis of Sub-Lethal Perfluorooctane Sulfonate Exposure to the Earthworm, Eisenia fetida, in Soil

Directory of Open Access Journals (Sweden)

Myrna J. Simpson

2013-08-01

Full Text Available 1H NMR-based metabolomics was used to measure the response of Eisenia fetida earthworms after exposure to sub-lethal concentrations of perfluorooctane sulfonate (PFOS in soil. Earthworms were exposed to a range of PFOS concentrations (five, 10, 25, 50, 100 or 150 mg/kg for two, seven and fourteen days. Earthworm tissues were extracted and analyzed by 1H NMR. Multivariate statistical analysis of the metabolic response of E. fetida to PFOS exposure identified time-dependent responses that were comprised of two separate modes of action: a non-polar narcosis type mechanism after two days of exposure and increased fatty acid oxidation after seven and fourteen days of exposure. Univariate statistical analysis revealed that 2-hexyl-5-ethyl-3-furansulfonate (HEFS, betaine, leucine, arginine, glutamate, maltose and ATP are potential indicators of PFOS exposure, as the concentrations of these metabolites fluctuated significantly. Overall, NMR-based metabolomic analysis suggests elevated fatty acid oxidation, disruption in energy metabolism and biological membrane structure and a possible interruption of ATP synthesis. These conclusions obtained from analysis of the metabolic profile in response to sub-lethal PFOS exposure indicates that NMR-based metabolomics is an excellent discovery tool when the mode of action (MOA of contaminants is not clearly defined.

Characterization and quantification of N-(3-aminopropyl)-N-dodecyl-1,3-propanediamine biocide by NMR, HPLC/MS and titration techniques.

Science.gov (United States)

Mondin, Andrea; Bogialli, Sara; Venzo, Alfonso; Favaro, Gabriella; Badocco, Denis; Pastore, Paolo

2014-01-01

The present paper reports the determination of the tri-amine N-(3-aminopropyl)-N-dodecyl-1,3-propanediamine (TA) present in a raw material called LONZABAC used to formulate various, widely used commercial biocides. The active principle, TA, is present in LONZABAC together with other molecules at lower concentration levels. Three independent analytical approaches, namely solution NMR spectroscopy, liquid chromatography coupled to high resolution mass spectrometry (LC/HRMS) and acid-base titration in mixed solvent, were used to overcome the problem of the non-availability of the active principle as high purity standard. NMR analysis of raw material, using a suitable internal standard, evidenced in all analyzed lots the presence of the active principle, the N-dodecyl-1,3-propanediamine (DA) and the n-dodecylamine (MA) and the absence of non-organic, NMR-inactive species. NMR peak integration led to a rough composition of the MA:DA:TA as 1:9:90. The LC/HRMS analysis allowed the accurate determination of DA and MA and confirmed in all samples the presence of the TA, which was estimated by difference: MA=1.4±0.3%, DA=11.1±0.7%, TA=87.5±1.3%. The obtained results were used to setup an easy, rapid and cheap acid-base titration method able to furnish a sufficiently accurate evaluation of the active principle both in the raw material and in diluted commercial products. For the raw material the results were: TA+MA=91.1±0.8% and DA-MA=8.9±0.8%, statistically coherent with LC/MS ones. The LC/MS approach demonstrated also its great potentialities to recognize trace of the biocide components both in environmental samples and in the formulated commercial products. Copyright © 2013 Elsevier Ltd. All rights reserved.

NMR studies of stock process water and reaction pathways in hydrothermal carbonization of furfural residue

Directory of Open Access Journals (Sweden)

Fen Yue

2018-04-01

Full Text Available Hydrothermal carbonization (HTC is a valuable approach to convert furfural residue (FR into carbon material. The prepared biochars are usually characterized comprehensively, while the stock process water still remains to be studied in detail. Herein, a NMR study of the main components in stock process water generated at different HTC reaction conditions was reported. Various qualitative and quantitative NMR techniques (1H and 13C NMR, 1H–1H COSY and 1H13C HSQC etc. especially 1D selective gradient total correlation spectroscopy (TOCSY NMR were strategically applied in the analysis of HTC stock process water. Without separation and purification, it was demonstrated that the main detectable compounds are 5-hydroxymethylfurfural, formic acid, methanol, acetic acid, levulinic acid, glycerol, hydroxyacetone and acetaldehyde in this complicate mixture. Furthermore, the relationship between the concentration of major products and the reaction conditions (180–240 °C at 8 h, and 1–24 h at 240 °C was established. Finally, reasonable reaction pathways for hydrothermal conversion of FR were proposed based on this result and our previously obtained characteristics of biochars. The routine and challenging NMR methods utilized here would be an alternative other than HPLC or GC for biomass conversion research and can be extended to more studies. Keywords: NMR, Hydrothermal carbonization, Furfural residue, Stock process water

Applications of artificial intelligence techniques to organic chemistry. Study on 13C NMR of steroids using computer

International Nuclear Information System (INIS)

Lins, A.P.; Furlan, M.; Gastmans, G.P.; Emerenciano, V.P.

1991-01-01

This work describes the utilization of two groups of programs in searching for characteristic signals of NMR 13 C steroidal compounds. The first group of programs used data bases with the spectral data and a methodology that enables the choice and the search of substructures. The chemical shifts and multiplicities for each specific substructure are used as rules to identify different types and subtypes of steroidal compounds. The second one was built to apply the rules formulated by the first group of programs and to foresee any skeletal based on a spectral analysis. (author)

Fine hierarchy of the V-O bonds by advanced solid state NMR: novel Pb4(VO2)(PO4)3 structure as a textbook case.

Science.gov (United States)

Tricot, Grégory; Mentré, Olivier; Cristol, Sylvain; Delevoye, Laurent

2012-12-17

We report here a complete structural characterization of a new lead Pb(4)(VO(2))(PO(4))(3) vanadophosphate compound by single crystal X-ray diffraction and (51)V and (31)P solid-state NMR spectroscopy. Although structural data are commonly used for the estimation of bond lengths and further delimitation of the true coordination number (e.g., octahedral: 6 versus 5 + 1 versus 4 + 2), we show here for the first time by solid-state NMR a more accurate appreciation of the V-O bonding scheme in this complex oxide which appears well adapted to the full series of vanado-phosphate materials. The direct characterization of V-O-P bridges through the J-mediated correlation (51)V{(31)P} heteronuclear multiple quantum coherence (J-HMQC) technique allows a contrasted hierarchy of the V-O electronic delocalization and indirectly supports the presence or not of the V-O bond. In the reported lead vanado-phosphate structure, the two vanadium polyhedra that have been assigned to octahedra from a bond length point of view have been finally reclassified as tetra- and penta-coordinated units on the basis of the solid-state NMR results. More generally, we believe that the improved characterization of interatomic bonds in various vanado-phosphate structures by solid-state NMR will contribute to a better understanding of the structure/property relationships in this important class of materials.

In-cell NMR spectroscopy of proteins inside Xenopus laevis oocytes

International Nuclear Information System (INIS)

Sakai, Tomomi; Tochio, Hidehito; Tenno, Takeshi; Ito, Yutaka; Kokubo, Tetsuro; Hiroaki, Hidekazu; Shirakawa, Masahiro

2006-01-01

In-cell NMR is an application of solution NMR that enables the investigation of protein conformations inside living cells. We have measured in-cell NMR spectra in oocytes from the African clawed frog Xenopus laevis. 15 N-labeled ubiquitin, its derivatives and calmodulin were injected into Xenopus oocytes and two-dimensional 1 H- 15 N correlation spectra of the proteins were obtained. While the spectrum of wild-type ubiquitin in oocytes had rather fewer cross-peaks compared to its in vitro spectrum, ubiquitin derivatives that are presumably unable to bind to ubiquitin-interacting proteins gave a markedly larger number of cross-peaks. This observation suggests that protein-protein interactions between ubiquitin and ubiquitin-interacting proteins may cause NMR signal broadening, and hence spoil the quality of the in-cell HSQC spectra. In addition, we observed the maturation of ubiquitin precursor derivative in living oocytes using the in-cell NMR technique. This process was partly inhibited by pre-addition of ubiquitin aldehyde, a specific inhibitor for ubiquitin C-terminal hydrolase (UCH). Our work demonstrates the potential usefulness of in-cell NMR with Xenopus oocytes for the investigation of protein conformations and functions under intracellular environmental conditions

Analytical research using synchrotron radiation based techniques

International Nuclear Information System (INIS)

Jha, Shambhu Nath

2015-01-01

There are many Synchrotron Radiation (SR) based techniques such as X-ray Absorption Spectroscopy (XAS), X-ray Fluorescence Analysis (XRF), SR-Fourier-transform Infrared (SRFTIR), Hard X-ray Photoelectron Spectroscopy (HAXPS) etc. which are increasingly being employed worldwide in analytical research. With advent of modern synchrotron sources these analytical techniques have been further revitalized and paved ways for new techniques such as microprobe XRF and XAS, FTIR microscopy, Hard X-ray Photoelectron Spectroscopy (HAXPS) etc. The talk will cover mainly two techniques illustrating its capability in analytical research namely XRF and XAS. XRF spectroscopy: XRF spectroscopy is an analytical technique which involves the detection of emitted characteristic X-rays following excitation of the elements within the sample. While electron, particle (protons or alpha particles), or X-ray beams can be employed as the exciting source for this analysis, the use of X-ray beams from a synchrotron source has been instrumental in the advancement of the technique in the area of microprobe XRF imaging and trace level compositional characterisation of any sample. Synchrotron radiation induced X-ray emission spectroscopy, has become competitive with the earlier microprobe and nanoprobe techniques following the advancements in manipulating and detecting these X-rays. There are two important features that contribute to the superb elemental sensitivities of microprobe SR induced XRF: (i) the absence of the continuum (Bremsstrahlung) background radiation that is a feature of spectra obtained from charged particle beams, and (ii) the increased X-ray flux on the sample associated with the use of tunable third generation synchrotron facilities. Detection sensitivities have been reported in the ppb range, with values of 10 -17 g - 10 -14 g (depending on the particular element and matrix). Keeping in mind its demand, a microprobe XRF beamline has been setup by RRCAT at Indus-2 synchrotron

An improved ultrafast 2D NMR experiment: Towards atom-resolved real-time studies of protein kinetics at multi-Hz rates

International Nuclear Information System (INIS)

Gal, Maayan; Kern, Thomas; Schanda, Paul; Frydman, Lucio; Brutscher, Bernhard

2009-01-01

Multidimensional NMR spectroscopy is a well-established technique for the characterization of structure and fast-time-scale dynamics of highly populated ground states of biological macromolecules. The investigation of short-lived excited states that are important for molecular folding, misfolding and function, however, remains a challenge for modern biomolecular NMR techniques. Off-equilibrium real-time kinetic NMR methods allow direct observation of conformational or chemical changes by following peak positions and intensities in a series of spectra recorded during a kinetic event. Because standard multidimensional NMR methods required to yield sufficient atom-resolution are intrinsically time-consuming, many interesting phenomena are excluded from real-time NMR analysis. Recently, spatially encoded ultrafast 2D NMR techniques have been proposed that allow one to acquire a 2D NMR experiment within a single transient. In addition, when combined with the SOFAST technique, such ultrafast experiments can be repeated at high rates. One of the problems detected for such ultrafast protein NMR experiments is related to the heteronuclear decoupling during detection with interferences between the pulses and the oscillatory magnetic field gradients arising in this scheme. Here we present a method for improved ultrafast data acquisition yielding higher signal to noise and sharper lines in single-scan 2D NMR spectra. In combination with a fast-mixing device, the recording of 1 H- 15 N correlation spectra with repetition rates of up to a few Hertz becomes feasible, enabling real-time studies of protein kinetics occurring on time scales down to a few seconds

Structural investigation of molten fluorides of nuclear interest by NMR and XAFS spectroscopies

International Nuclear Information System (INIS)

Pauvert, Olivier

2009-01-01

In the frame of the renewal of the different nuclear plans, the molten salt reactor is one of the six concepts of reactors of 4. generation. This reactor has the particularity to use a liquid fuel based on LiF-ThF 4 mixtures. In order to develop and to optimize this concept, it is important to characterize the structure of the melt and to describe its physical and chemical properties. Our work has been based on the study of the system MF-ZrF 4 (M = Li, Na, K) selected as a model of ThF 4 based systems. We have combined two spectroscopic techniques, the Nuclear Magnetic Resonance and the X-ray Absorption at high temperature, with molecular dynamics calculations. We particularly focused on the local environments of the fluorine and the zirconium. In order to interpret the NMR data obtain in the molten state, we performed a preliminary study on zirconium halides and rare earth and alkali fluoro zirconates using the 91 Zr solid-state NMR at very high magnetic fields. New correlations between structural parameters and NMR data have been established. At high temperature, in MF-ZrF 4 melts we have shown the coexistence of three different kind of Zr-based complexes with different proportions depending on the amount of ZrF 4 and on the nature of the alkali. Depending on the ZrF 4 content, three kinds of fluorine have been characterized: form free fluorines at low amount of zirconium fluorides, fluorines involved in Zr-based complexes and bridging fluorines at higher ZrF 4 content. This original and innovative approach of molten fluorides mixtures, combining NMR and EXAFS at high temperature with molecular dynamics calculations, is very efficient to describe their speciation and thus their fluoro-acidity. (author)

Advanced of X-ray fluorescence logging technique in China

International Nuclear Information System (INIS)

Zhou Sichun; Ge Liangquan; Lai Wanchang; Yang Qiang

2010-01-01

The paper discuses principle of X-ray fluorescence logging, and introduces advanced of X-ray fluorescence logging technique in China. By 2009, third generation XRF logging instrument has been developed in China, and good logging result has been obtained in Lala copper mine. (authors)

Structural level characterization of base oils using advanced analytical techniques