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Sample records for superscript 1h noesy

  1. The interaction of small molecules with phospholipid membranes studied by 1H NOESY NMR under magic-angle spinning1

    Institute of Scientific and Technical Information of China (English)

    Holger A SCHEIDT; Daniel HUSTER

    2008-01-01

    The interaction of small molecules with lipid membranes and the exact knowledge of their binding site and bilayer distribution is of great pharmacological impor-tance and represents an active field of current biophysical research. Over the last decade, a highly resolved 1H solid-state NMR method has been developed that allows measuring localization and distribution of small molecules in membranes. The classical solution 1H NMR NOESY technique is applied to lipid membrane samples under magic-angle spinning (MAS) and NOESY cross-relaxation rates are determined quantitatively. These rates are proportional to the contact probability between molecular segments and therefore an ideal tool to study intermolecular interactions in membranes. Here, we review recent 1H MAS NOESY applications that were carried out to study lateral lipid organization in mixed membranes and the interaction of membranes with water, ethanol, small aromatic compounds, peptides, fluorescence labels, and lipophilic nucleosides.

  2. Discovering [superscript 13]C NMR, [superscript 1]H NMR, and IR Spectroscopy in the General Chemistry Laboratory through a Sequence of Guided-Inquiry Exercises

    Science.gov (United States)

    Iler, H. Darrell; Justice, David; Brauer, Shari; Landis, Amanda

    2012-01-01

    This sequence of three guided-inquiry labs is designed for a second-semester general chemistry course and challenges students to discover basic theoretical principles associated with [superscript 13]C NMR, [superscript 1]H NMR, and IR spectroscopy. Students learn to identify and explain basic concepts of magnetic resonance and vibrational…

  3. Discovering [superscript 13]C NMR, [superscript 1]H NMR, and IR Spectroscopy in the General Chemistry Laboratory through a Sequence of Guided-Inquiry Exercises

    Science.gov (United States)

    Iler, H. Darrell; Justice, David; Brauer, Shari; Landis, Amanda

    2012-01-01

    This sequence of three guided-inquiry labs is designed for a second-semester general chemistry course and challenges students to discover basic theoretical principles associated with [superscript 13]C NMR, [superscript 1]H NMR, and IR spectroscopy. Students learn to identify and explain basic concepts of magnetic resonance and vibrational…

  4. Extraction and [superscript 1]H NMR Analysis of Fats from Convenience Foods: A Laboratory Experiment for Organic Chemistry

    Science.gov (United States)

    Hartel, Aaron M.; Moore, Amy C.

    2014-01-01

    The extraction and analysis of fats from convenience foods (crackers, cookies, chips, candies) has been developed as an experiment for a second-year undergraduate organic chemistry laboratory course. Students gravimetrically determine the fat content per serving and then perform a [superscript 1]H NMR analysis of the recovered fat to determine the…

  5. Extraction and [superscript 1]H NMR Analysis of Fats from Convenience Foods: A Laboratory Experiment for Organic Chemistry

    Science.gov (United States)

    Hartel, Aaron M.; Moore, Amy C.

    2014-01-01

    The extraction and analysis of fats from convenience foods (crackers, cookies, chips, candies) has been developed as an experiment for a second-year undergraduate organic chemistry laboratory course. Students gravimetrically determine the fat content per serving and then perform a [superscript 1]H NMR analysis of the recovered fat to determine the…

  6. Using a Problem Solving-Cooperative Learning Approach to Improve Students' Skills for Interpreting [Superscript 1]H NMR Spectra of Unknown Compounds in an Organic Spectroscopy Course

    Science.gov (United States)

    Angawi, Rihab F.

    2014-01-01

    To address third- and fourth-year chemistry students' difficulties with the challenge of interpreting [superscript 1]H NMR spectra, a problem solving-cooperative learning technique was incorporated in a Spectra of Organic Compounds course. Using this approach helped students deepen their understanding of the basics of [superscript 1]H NMR…

  7. [superscript 1]H NMR Spectroscopy-Based Configurational Analysis of Mono- and Disaccharides and Detection of ß-Glucosidase Activity: An Undergraduate Biochemistry Laboratory

    Science.gov (United States)

    Periyannan, Gopal R.; Lawrence, Barbara A.; Egan, Annie E.

    2015-01-01

    A [superscript 1]H NMR spectroscopy-based laboratory experiment explores mono- and disaccharide structural chemistry, and the enzyme-substrate specificity of glycosidic bond cleavage by ß-glucosidase towards cellobiose (ß-linked gluco-disaccharide) and maltose (a-linked gluco-disaccharide). Structural differences between cellobiose, maltose, and…

  8. [superscript 1]H NMR Spectroscopy-Based Configurational Analysis of Mono- and Disaccharides and Detection of ß-Glucosidase Activity: An Undergraduate Biochemistry Laboratory

    Science.gov (United States)

    Periyannan, Gopal R.; Lawrence, Barbara A.; Egan, Annie E.

    2015-01-01

    A [superscript 1]H NMR spectroscopy-based laboratory experiment explores mono- and disaccharide structural chemistry, and the enzyme-substrate specificity of glycosidic bond cleavage by ß-glucosidase towards cellobiose (ß-linked gluco-disaccharide) and maltose (a-linked gluco-disaccharide). Structural differences between cellobiose, maltose, and…

  9. Lower "N"-Acetyl-Aspartate Levels in Prefrontal Cortices in Pediatric Bipolar Disorder: A (Superscript 1]H Magnetic Resonance Spectroscopy Study

    Science.gov (United States)

    Caetano, Sheila C.; Olvera, Rene L.; Hatch, John P.; Sanches, Marsal; Chen, Hua Hsuan; Nicoletti, Mark; Stanley, Jeffrey A.; Fonseca, Manoela; Hunter, Kristina; Lafer, Beny; Pliszka, Steven R.; Soares, Jair C.

    2011-01-01

    Objective: The few studies applying single-voxel [superscript 1]H spectroscopy in children and adolescents with bipolar disorder (BD) have reported low "N"-acetyl-aspartate (NAA) levels in the dorsolateral prefrontal cortex (DLPFC), and high myo-inositol/phosphocreatine plus creatine (PCr+Cr) ratios in the anterior cingulate. The aim of this study…

  10. Lower "N"-Acetyl-Aspartate Levels in Prefrontal Cortices in Pediatric Bipolar Disorder: A (Superscript 1]H Magnetic Resonance Spectroscopy Study

    Science.gov (United States)

    Caetano, Sheila C.; Olvera, Rene L.; Hatch, John P.; Sanches, Marsal; Chen, Hua Hsuan; Nicoletti, Mark; Stanley, Jeffrey A.; Fonseca, Manoela; Hunter, Kristina; Lafer, Beny; Pliszka, Steven R.; Soares, Jair C.

    2011-01-01

    Objective: The few studies applying single-voxel [superscript 1]H spectroscopy in children and adolescents with bipolar disorder (BD) have reported low "N"-acetyl-aspartate (NAA) levels in the dorsolateral prefrontal cortex (DLPFC), and high myo-inositol/phosphocreatine plus creatine (PCr+Cr) ratios in the anterior cingulate. The aim of this study…

  11. Polymer Molecular Weight Analysis by [Superscript 1]H NMR Spectroscopy

    Science.gov (United States)

    Izunobi, Josephat U.; Higginbotham, Clement L.

    2011-01-01

    The measurement and analysis of molecular weight and molecular weight distribution remain matters of fundamental importance for the characterization and physical properties of polymers. Gel permeation chromatography (GPC) is the most routinely used method for the molecular weight determination of polymers whereas matrix-assisted laser…

  12. Polymer Molecular Weight Analysis by [Superscript 1]H NMR Spectroscopy

    Science.gov (United States)

    Izunobi, Josephat U.; Higginbotham, Clement L.

    2011-01-01

    The measurement and analysis of molecular weight and molecular weight distribution remain matters of fundamental importance for the characterization and physical properties of polymers. Gel permeation chromatography (GPC) is the most routinely used method for the molecular weight determination of polymers whereas matrix-assisted laser…

  13. Do Humans Really Learn A[superscript n] B[superscript n] Artificial Grammars from Exemplars?

    Science.gov (United States)

    Hochmann, Jean-Remy; Azadpour, Mahan; Mehler, Jacques

    2008-01-01

    An important topic in the evolution of language is the kinds of grammars that can be computed by humans and other animals. Fitch and Hauser (F&H; 2004) approached this question by assessing the ability of different species to learn 2 grammars, (AB)[superscript n] and A[superscript n] B[superscript n]. A[superscript n] B[superscript n] was taken to…

  14. NMR Kinetics of the S[subscript N]2 Reaction between BuBr and I[superscript -]: An Introductory Organic Chemistry Laboratory Exercise

    Science.gov (United States)

    Mobley, T. Andrew

    2015-01-01

    A simple organic chemistry experiment is described that investigates the kinetics of the reaction between 1-bromobutane (BuBr) and iodide (I[superscript -]) as followed by observing the disappearance of BuBr and the appearance of 1-iodobutane (BuI) using [superscript 1]H NMR spectroscopy. In small groups of three to four, students acquire data to…

  15. NMR Kinetics of the S[subscript N]2 Reaction between BuBr and I[superscript -]: An Introductory Organic Chemistry Laboratory Exercise

    Science.gov (United States)

    Mobley, T. Andrew

    2015-01-01

    A simple organic chemistry experiment is described that investigates the kinetics of the reaction between 1-bromobutane (BuBr) and iodide (I[superscript -]) as followed by observing the disappearance of BuBr and the appearance of 1-iodobutane (BuI) using [superscript 1]H NMR spectroscopy. In small groups of three to four, students acquire data to…

  16. Phantasia, a Mediation between Perception (Aesthesis and Thought (Noesis

    Directory of Open Access Journals (Sweden)

    Gabriela VASILESCU

    2013-01-01

    Full Text Available The present paper aims at analyzing the creative force of phantasia, as it reveals itself in various works of art. The concept of phantasia defines the affectivity stirred in the mind of the spectator immediately after ceasing the physical contact with the image, sound, form or colour. This psychological state is opposed in meaning to the apatheia, as pathe (the affectivity is associated with the affects, which are, in their turn, bound to the bodily perception and senses. Pathe gives dynamism to the phantasia triggered at the end of the sensorial contact and it stimulates the illusions. Only the human being, in its ephemeral passage through existence, can experience the state of phantasia. This specific state is the mingle of perception and judgement which leads to a certain “impression” that we can relate to the illusion, appearance or the fiction we delude ourselves with but which, at the same time, constructs our identity in the realm of culture. The two ontological levels – dream and reality – will never be conciliated; on the contrary, they will eternally keep on alternating in the illusion of fiction. Through this illusion we give life to imaginary things and events and this strive draws together both perception (aisthesis and thought (noesis. When perception fades away, representation sheds its light on forms, contents, colours, sounds, words, all these being the fittest tools for the artistic expression. Yet each chimeric frame we bear inside is nothing but our cultural identity, “the measure” (as Protagoras said of our phantasia or, consequently, of the illusion we lived in and we imagined in and by culture

  17. Detection of Fe[superscript 3+] and Al[superscript 3+] by Test Paper

    Science.gov (United States)

    Li, Lili; Xiang, Haifeng; Zhou, Xiangge; Li, Menglong; Wu, Di

    2012-01-01

    A porphyrin-based test paper has been designed and prepared. It can be used to analyze for Al[superscript 3+] and Fe[superscript 3+] in aqueous solution. An experiment employing the test paper can help students understand basic principles of spectrophotometry and how spectrophotometry is used in analyzing for metal ions. (Contains 1 scheme and 1…

  18. Molecular Orbitals of NO, NO[superscript+], and NO[superscript-]: A Computational Quantum Chemistry Experiment

    Science.gov (United States)

    Orenha, Renato P.; Galembeck, Sérgio E.

    2014-01-01

    This computational experiment presents qualitative molecular orbital (QMO) and computational quantum chemistry exercises of NO, NO[superscript+], and NO[superscript-]. Initially students explore several properties of the target molecules by Lewis diagrams and the QMO theory. Then, they compare qualitative conclusions with EHT and DFT calculations…

  19. Assignments of 1H and 13C NMR Signals of Mogroside IVa

    Institute of Scientific and Technical Information of China (English)

    ZHANGJian-ye; YANGXiu-wei

    2003-01-01

    Aim To investigate the structure of mogroside IVa isolated from traditional Chinese medicine fructus momordicae [fruits of Siraitia grosvenori (Swingle) C. Jeffery] and summarize the NMR characteristics of the structure. Methods Cormnon extraction, separafion and purification methods were used. Various NMR techniques including 1H NMR,13C NMR, DEPT, 1H-1H COSY, HSQC, HMBC, NOESY and molecular model simulated by comtmter were used to elucidate the structure. Results 1H and 13C NMR signals of mogroside IVa were assigned, and spectroscopic basis was obtained for identification of such type of compounds. Conclusion 1D and 2D NMR techniques including 1H-1H COSY, HSQC, HMBC, NOESY spectra are powerful tools for structure analysis. The structure determined by NMR methods is identical with energy minimized conformation simulated by computer.

  20. Complete {sup 1}H and {sup 13}C NMR assignments of isojuripidine from Solanum asterophorum Mart

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Tania M.S.; Costa, Rodrigo A.; Oliveira, Eduardo J.; Barbosa-Filho, Jose M.; Agra, Maria F.; Camara, Celso A. [Universidade Federal da Paraiba, Joao Pessoa, PB (Brazil). Lab. de Tecnologia Farmaceutica]. E-mail: sarmento@ltf.ufpb.br

    2005-11-15

    Isojuripidine was isolated from the aerial parts of Solanum astherophorum Mart. Its structure was determined using a combination of homo- (1D {sup 1}H NMR, {sup 13}C NMR-HBBD and {sup 13}C NMRDEPT) and heteronuclear 2D NMR techniques ({sup 1}H-{sup 1}H-COSY, {sup 1}H-{sup 1}H-NOESY, HSQC, HMBC), and HREIMS. The unambiguous assignments of {sup 1}H and {sup 13}C NMR data of derivatives 3-N,6-Odiacetyl- isojuripidine and 3-N-cinnamoyl-isojuripidine are described. (author)

  1. Use of [superscript 1]H, [superscript 13]C, and [superscript 19]F-NMR Spectroscopy and Computational Modeling to Explore Chemoselectivity in the Formation of a Grignard Reagent

    Science.gov (United States)

    Hein, Sara M.; Kopitzke, Robert W.; Nalli, Thomas W.; Esselman, Brian J.; Hill, Nicholas J.

    2015-01-01

    A discovery-based Grignard experiment for a second-year undergraduate organic chemistry course is described. The exclusive Grignard reagent formed by the reaction of 1-bromo-4-fluorobenzene (1) with Mg is 4-fluorophenylmagnesium bromide (2), which is treated with either benzophenone or CO[subscript 2] to produce the corresponding fluorinated…

  2. Use of [superscript 1]H, [superscript 13]C, and [superscript 19]F-NMR Spectroscopy and Computational Modeling to Explore Chemoselectivity in the Formation of a Grignard Reagent

    Science.gov (United States)

    Hein, Sara M.; Kopitzke, Robert W.; Nalli, Thomas W.; Esselman, Brian J.; Hill, Nicholas J.

    2015-01-01

    A discovery-based Grignard experiment for a second-year undergraduate organic chemistry course is described. The exclusive Grignard reagent formed by the reaction of 1-bromo-4-fluorobenzene (1) with Mg is 4-fluorophenylmagnesium bromide (2), which is treated with either benzophenone or CO[subscript 2] to produce the corresponding fluorinated…

  3. Confirming the 3D Solution Structure of a Short Double-Stranded DNA Sequence Using NMR Spectroscopy

    Science.gov (United States)

    Ruhayel, Rasha A.; Berners-Price, Susan J.

    2010-01-01

    2D [superscript 1]H NOESY NMR spectroscopy is routinely used to give information on the closeness of hydrogen atoms through space. This work is based on a 2D [superscript 1]H NOESY NMR spectrum of a 12 base-pair DNA duplex. This 6-h laboratory workshop aims to provide advanced-level chemistry students with a basic, yet solid, understanding of how…

  4. Confirming the 3D Solution Structure of a Short Double-Stranded DNA Sequence Using NMR Spectroscopy

    Science.gov (United States)

    Ruhayel, Rasha A.; Berners-Price, Susan J.

    2010-01-01

    2D [superscript 1]H NOESY NMR spectroscopy is routinely used to give information on the closeness of hydrogen atoms through space. This work is based on a 2D [superscript 1]H NOESY NMR spectrum of a 12 base-pair DNA duplex. This 6-h laboratory workshop aims to provide advanced-level chemistry students with a basic, yet solid, understanding of how…

  5. Activity-Dependent Excitability Changes Suggest Na[superscript +]/K[superscript +] Pump Dysfunction in Diabetic Neuropathy

    Science.gov (United States)

    Krishnan, Arun V.; Lin, Cindy S.-Y.; Kiernan, Matthew C.

    2008-01-01

    The present study was undertaken to evaluate the role of Na[superscript +]/K[superscript +] pump dysfunction in the development of diabetic neuropathy (DN). Nerve excitability techniques, which provide information about membrane potential and axonal ion channel function, were undertaken in 15 patients with established DN and in 10 patients with…

  6. Diagonal-free 3D/4D HN,HN-TROSY-NOESY-TROSY.

    Science.gov (United States)

    Diercks, Tammo; Truffault, Vincent; Coles, Murray; Millet, Oscar

    2010-02-24

    Structural biology by NMR spectroscopy relies on measuring interproton distances via NOE cross-signals in nuclear Overhauser effect spectroscopy (NOESY) spectra. In proteins, the subset of H(N)-H'(N) NOE contacts is most important for deriving initial structural models and for spectral assignment by "NOE walking". Here we present a fully optimized NMR experiment for measuring these pivotal contacts: diagonal-free 3D/4D HN,HN-TROSY-NOESY-TROSY. It combines all of the critical requirements for extracting the optimal H(N)-H'(N) distance information: the highest resolution by consistent transverse relaxation-optimized spectroscopy (TROSY) evolution, the largest spectral dispersion in two (15)N dimensions, and maximal coverage and purity through specific suppression of the intense diagonal signals that are the main source of overlap, artifacts, and bias in any NOESY spectrum. Most notably, diagonal suppression here comes without compromising the NOE cross-signal intensities. This optimized experiment appears to be ideal for a broad range of structural studies, particularly on large deuterated, partially unfolded, helical, and membrane proteins.

  7. Proof without Words: (1 + 1/n)[superscript n] less than e less than (1 + 1/n)[superscript n+1

    Science.gov (United States)

    Khattri, Sanjay Kumar

    2008-01-01

    We present a pictorial proof of the inequation (1 + 1/n)[superscript n] less than e less than (1 + 1/n)[superscript n+1]. The inequation is also confirmed through the Taylor expansion and alternating series theorem.

  8. Proof without Words: (1 + 1/n)[superscript n] less than e less than (1 + 1/n)[superscript n+1

    Science.gov (United States)

    Khattri, Sanjay Kumar

    2008-01-01

    We present a pictorial proof of the inequation (1 + 1/n)[superscript n] less than e less than (1 + 1/n)[superscript n+1]. The inequation is also confirmed through the Taylor expansion and alternating series theorem.

  9. Rapid Protein Global Fold Determination Using Ultrasparse Sampling, High-Dynamic Range Artifact Suppression, and Time-Shared NOESY

    OpenAIRE

    Coggins, Brian E.; Werner-Allen, Jonathan W.; Yan, Anthony; Zhou, Pei

    2012-01-01

    In structural studies of large proteins by NMR, global fold determination plays an increasingly important role in providing a first look at a target’s topology and reducing assignment ambiguity in NOESY spectra of fully-protonated samples. In this work, we demonstrate the use of ultrasparse sampling, a new data processing algorithm, and a 4-D time-shared NOESY experiment (1) to collect all NOEs in 2H/13C/15N-labeled protein samples with selectively-protonated amide and ILV methyl groups at hi...

  10. {sup 13}C-{sup 13}C NOESY spectra of a 480 kDa protein: solution NMR of ferritin

    Energy Technology Data Exchange (ETDEWEB)

    Matzapetakis, Manolis; Turano, Paola [University of Florence, Department of Chemistry, CERM (Italy); Theil, Elizabeth C. [Children' s Hospital Oakland Research Institute, CeBIC (Council for BioIron at CHORI) (United States); Bertini, Ivano [University of Florence, Department of Chemistry, CERM (Italy)], E-mail: ivanobertini@cerm.unifi.it

    2007-07-15

    Molecular size has limited solution NMR analyses of proteins. We report {sup 13}C-{sup 13}C NOESY experiments on a 480 kDa protein, the multi-subunit ferritin nanocage with gated pores. By exploiting {sup 13}C-resonance-specific chemical shifts and spin diffusion effects, we identified 75% of the amino acids, with intraresidue C-C connectivities between nuclei separated by 1-4 bonds. These results show the potential of {sup 13}C-{sup 13}C NOESY for solution studies of molecular assemblies >100 kDa.

  11. M[superscript 2+]•EDTA Binding Affinities: A Modern Experiment in Thermodynamics for the Physical Chemistry Laboratory

    Science.gov (United States)

    O'Brien, Leah C.; Root, Hannah B.; Wei, Chin-Chuan; Jensen, Drake; Shabestary, Nahid; De Meo, Cristina; Eder, Douglas J.

    2015-01-01

    Isothermal titration calorimetry was used to experimentally determine thermodynamic values for the ethylenediaminetetraacetic acid (EDTA)(aq) + M[superscript 2+](aq) reactions (M[superscript 2+] = Ca[superscript 2+] and Mg[superscript 2+]). Students showed that for reactions in a N-(2-hydroxyethyl)piperazine-N"-ethanesulfonic acid (HEPES)…

  12. Synthesis and NMR Spectral Analysis of Amine Heterocycles: The Effect of Asymmetry on the [superscript 1]H and [superscript 13]C NMR Spectra of N,O-Acetals

    Science.gov (United States)

    Saba, Shahrokh; Ciaccio, James A.; Espinal, Jennifer; Aman, Courtney E.

    2007-01-01

    The stereochemical investigation is conducted to give students the combined experience of chemical synthesis of amines and N-heterocycles and structural stereochemical analysis using NMR spectroscopy. Students are introduced to the concept of topicity-stereochemical relationships between ligands within a molecule by synthesizing N,O-acetals.

  13. Concerning the Integral dx/x[superscript m] (1+x)

    Science.gov (United States)

    Walters, William; Huber, Michael

    2010-01-01

    Consider the integral dx/x[superscript m] (1+x). In the "CRC Standard Mathematical Tables," this integral can require repeated integral evaluations. Enter this integral into your favourite computer algebra system, and the results may be unrecognizable. In this article, we seek to provide a simpler evaluation for integrals of this form. We state up…

  14. Concerning the Integral dx/x[superscript m] (1+x)

    Science.gov (United States)

    Walters, William; Huber, Michael

    2010-01-01

    Consider the integral dx/x[superscript m] (1+x). In the "CRC Standard Mathematical Tables," this integral can require repeated integral evaluations. Enter this integral into your favourite computer algebra system, and the results may be unrecognizable. In this article, we seek to provide a simpler evaluation for integrals of this form. We state up…

  15. Determination of the structure of [Nle7]-endothelin by 1H NMR.

    Science.gov (United States)

    Aumelas, A; Chiche, L; Mahe, E; Le-Nguyen, D; Sizun, P; Berthault, P; Perly, B

    1991-04-01

    [Nle7]-endothelin was synthesized and studied by 1H NMR and distance geometry calculations. The NMR study was performed first in DMSO-d6 and then in 50% acetonitrile/water since this peptide aggregates in pure water. In both cases, all spin systems were identified and assigned with the aid of two-dimensional spectroscopy (2D): COSY (for scalar couplings) and NOESY (for dipolar couplings). On the basis of the acetonitrile/water NMR parameters, and using the DISGEO program, a three-dimensional structure of [Nle7]-endothelin is proposed and discussed.

  16. Rapid protein global fold determination using ultrasparse sampling, high-dynamic range artifact suppression, and time-shared NOESY.

    Science.gov (United States)

    Coggins, Brian E; Werner-Allen, Jonathan W; Yan, Anthony; Zhou, Pei

    2012-11-14

    In structural studies of large proteins by NMR, global fold determination plays an increasingly important role in providing a first look at a target's topology and reducing assignment ambiguity in NOESY spectra of fully protonated samples. In this work, we demonstrate the use of ultrasparse sampling, a new data processing algorithm, and a 4-D time-shared NOESY experiment (1) to collect all NOEs in (2)H/(13)C/(15)N-labeled protein samples with selectively protonated amide and ILV methyl groups at high resolution in only four days, and (2) to calculate global folds from this data using fully automated resonance assignment. The new algorithm, SCRUB, incorporates the CLEAN method for iterative artifact removal but applies an additional level of iteration, permitting real signals to be distinguished from noise and allowing nearly all artifacts generated by real signals to be eliminated. In simulations with 1.2% of the data required by Nyquist sampling, SCRUB achieves a dynamic range over 10000:1 (250× better artifact suppression than CLEAN) and completely quantitative reproduction of signal intensities, volumes, and line shapes. Applied to 4-D time-shared NOESY data, SCRUB processing dramatically reduces aliasing noise from strong diagonal signals, enabling the identification of weak NOE crosspeaks with intensities 100× less than those of diagonal signals. Nearly all of the expected peaks for interproton distances under 5 Å were observed. The practical benefit of this method is demonstrated with structure calculations for 23 kDa and 29 kDa test proteins using the automated assignment protocol of CYANA, in which unassigned 4-D time-shared NOESY peak lists produce accurate and well-converged global fold ensembles, whereas 3-D peak lists either fail to converge or produce significantly less accurate folds. The approach presented here succeeds with an order of magnitude less sampling than required by alternative methods for processing sparse 4-D data.

  17. Fast acquisition of high resolution 4-D amide-amide NOESY with diagonal suppression, sparse sampling and FFT-CLEAN.

    Science.gov (United States)

    Werner-Allen, Jon W; Coggins, Brian E; Zhou, Pei

    2010-05-01

    Amide-amide NOESY provides important distance constraints for calculating global folds of large proteins, especially integral membrane proteins with beta-barrel folds. Here, we describe a diagonal-suppressed 4-D NH-NH TROSY-NOESY-TROSY (ds-TNT) experiment for NMR studies of large proteins. The ds-TNT experiment employs a spin state selective transfer scheme that suppresses diagonal signals while providing TROSY optimization in all four dimensions. Active suppression of the strong diagonal peaks greatly reduces the dynamic range of observable signals, making this experiment particularly suitable for use with sparse sampling techniques. To demonstrate the utility of this method, we collected a high resolution 4-D ds-TNT spectrum of a 23kDa protein using randomized concentric shell sampling (RCSS), and we used FFT-CLEAN processing for further reduction of aliasing artifacts - the first application of these techniques to a NOESY experiment. A comparison of peak parameters in the high resolution 4-D dataset with those from a conventionally-sampled 3-D control spectrum shows an accurate reproduction of NOE crosspeaks in addition to a significant reduction in resonance overlap, which largely eliminates assignment ambiguity. Likewise, a comparison of 4-D peak intensities and volumes before and after application of the CLEAN procedure demonstrates that the reduction of aliasing artifacts by CLEAN does not systematically distort NMR signals.

  18. Integral Representation of the Pictorial Proof of Sum of [superscript n][subscript k=1]k[superscript 2] = 1/6n(n+1)(2n+1)

    Science.gov (United States)

    Kobayashi, Yukio

    2011-01-01

    The pictorial proof of the sum of [superscript n][subscript k=1] k[superscript 2] = 1/6n(n+1)(2n+1) is represented in the form of an integral. The integral representations are also applicable to the sum of [superscript n][subscript k-1] k[superscript m] (m greater than or equal to 3). These representations reveal that the sum of [superscript…

  19. Integral Representation of the Pictorial Proof of Sum of [superscript n][subscript k=1]k[superscript 2] = 1/6n(n+1)(2n+1)

    Science.gov (United States)

    Kobayashi, Yukio

    2011-01-01

    The pictorial proof of the sum of [superscript n][subscript k=1] k[superscript 2] = 1/6n(n+1)(2n+1) is represented in the form of an integral. The integral representations are also applicable to the sum of [superscript n][subscript k-1] k[superscript m] (m greater than or equal to 3). These representations reveal that the sum of [superscript…

  20. Determination of (3)J((1)H3'-(31)P) couplings in a DNA oligomer with enhanced sensitivity employing a constant-time TOCSY difference experiment.

    Science.gov (United States)

    Reith, Lorenz M; Schlagnitweit, Judith; Smrecki, Vilko; Knör, Günther; Müller, Norbert; Schoefberger, Wolfgang

    2011-03-01

    A constant-time TOCSY difference experiment for the determination of (3)J((1)H3'-(31)P) coupling constants in non-isotope-labelled DNA oligonucleotides is presented. The method is tested on a DNA octamer and compared with the established constant-time NOESY difference method. Each (3)J((1)H3'-(31)P) coupling constant is determined from amplitude changes caused by phosphorous decoupling, which are observable on multiple cross-peaks, thus leading to a high accuracy of the value of the (3)J((1)H3'-(31)P) coupling constant. The new experiment delivers up to three times the sensitivity compared with previously reported methods.

  1. Assessing Cardiff University's Curricula Contribution to Sustainable Development Using the STAUNCH[superscript (RTM)] System

    Science.gov (United States)

    Lozano, Rodrigo; Peattie, Ken

    2011-01-01

    This article presents the results of the sustainable development curricula assessment undertaken at 19 of the 28 schools of Cardiff University using the Sustainability Tool for Assessing UNiversity's Curricula Holistically (STAUNCH[superscript (RTM)]. STAUNCH[superscript (RTM)] was developed with two objectives: (1) to systematically assess how…

  2. Construct Validity of the WISC-IV[superscript UK] with a Large Referred Irish Sample

    Science.gov (United States)

    Watkins, Marley W.; Canivez, Gary L.; James, Trevor; James, Kate; Good, Rebecca

    2013-01-01

    Irish educational psychologists frequently use the Wechsler Intelligence Scale for Children-Fourth U.K. Edition (WISC-IV[superscript UK]) in clinical assessments of children with learning difficulties. Unfortunately, reliability and validity studies of the WISC-IV[superscript UK] have not yet been reported. This study examined the construct…

  3. Phosphorylation of K[superscript +] Channels at Single Residues Regulates Memory Formation

    Science.gov (United States)

    Vernon, Jeffrey; Irvine, Elaine E.; Peters, Marco; Jeyabalan, Jeshmi; Giese, K. Peter

    2016-01-01

    Phosphorylation is a ubiquitous post-translational modification of proteins, and a known physiological regulator of K[superscript +] channel function. Phosphorylation of K[superscript +] channels by kinases has long been presumed to regulate neuronal processing and behavior. Although circumstantial evidence has accumulated from behavioral studies…

  4. Health Literacy Study Circles[superscript +]. Introduction: Overview, Planning, and Facilitation Tips

    Science.gov (United States)

    Rudd, Rima; Soricone, Lisa; Santos, Maricel; Zobel, Emily; Smith, Janet

    2005-01-01

    A Health Literacy Study Circle[superscript +] is a multi-session professional development activity for adult education practitioners, conducted by a facilitator. All the information and materials required to conduct each Health Literacy Study Circle[superscript +] is presented in two parts: this Introduction and the "Facilitator's Guide" for each…

  5. Using Email to Enable E[superscript 3] (Effective, Efficient, and Engaging) Learning

    Science.gov (United States)

    Kim, ChanMin

    2008-01-01

    This article argues that technology that supports both noncognitive and cognitive aspects can make learning more effective, efficient, and engaging (e[superscript 3]-learning). The technology of interest in this article is email. The investigation focuses on characteristics of email that are likely to enable e[superscript 3]-learning. In addition,…

  6. Teaching the Modes of Ca[superscript 2+] Transport between the Plasma Membrane and Endoplasmic Reticulum Using a Classic Paper by Kwan et al.

    Science.gov (United States)

    Liang, Willmann

    2009-01-01

    This teaching article uses the report by Kwan et al., "Effects of methacholine, thapsigargin, and La[superscript 3+] on plasmalemmal and intracellular Ca[superscript 2+] transport in lacrimal acinar cells," where the effects of Ca[superscript 2+]-mobilizing agents in regulating Ca[superscript 2+] fluxes were examined under various conditions.…

  7. Synthesis and [superscript 1]H NMR Spectroscopic Elucidation of Five- and Six-Membered D-Ribonolactone Derivatives

    Science.gov (United States)

    Sales, Eric S.; Silveira, Gustavo P.

    2015-01-01

    Lactone-size identification of [subscript D]-ribonolactone derivatives has been debated for four decades due to complex lactone-ring rearrangements and acetal migration. This laboratory experiment for an upper-division undergraduate organic chemistry laboratory course describes a fast and reliable assignment of lactone-size derivatives from…

  8. Why Is It so? The [superscript 1]H-NMR CH[subscript 2] Splitting in Substituted Propanes

    Science.gov (United States)

    Lim, Kieran F.; Dereani, Marino

    2010-01-01

    Nuclear magnetic resonance (NMR) spectroscopy is an important tool in the structural analysis of both organic and inorganic molecules. Proton NMR spectra can yield information about the chemical or bonding environment surrounding various protons, the number of protons in those environments, and the number of neighbouring protons around each…

  9. Synthesis and [superscript 1]H NMR Spectroscopic Elucidation of Five- and Six-Membered D-Ribonolactone Derivatives

    Science.gov (United States)

    Sales, Eric S.; Silveira, Gustavo P.

    2015-01-01

    Lactone-size identification of [subscript D]-ribonolactone derivatives has been debated for four decades due to complex lactone-ring rearrangements and acetal migration. This laboratory experiment for an upper-division undergraduate organic chemistry laboratory course describes a fast and reliable assignment of lactone-size derivatives from…

  10. Artifacts in time-resolved NUS: A case study of NOE build-up curves from 2D NOESY

    Science.gov (United States)

    Dass, Rupashree; Kasprzak, Paweł; Koźmiński, Wiktor; Kazimierczuk, Krzysztof

    2016-04-01

    Multidimensional NMR spectroscopy requires time-consuming sampling of indirect dimensions and so is usually used to study stable samples. However, dynamically changing compounds or their mixtures commonly occur in problems of natural science. Monitoring them requires the use multidimensional NMR in a time-resolved manner - in other words, a series of quick spectra must be acquired at different points in time. Among the many solutions that have been proposed to achieve this goal, time-resolved non-uniform sampling (TR-NUS) is one of the simplest. In a TR-NUS experiment, the signal is sampled using a shuffled random schedule and then divided into overlapping subsets. These subsets are then processed using one of the NUS reconstruction methods, for example compressed sensing (CS). The resulting stack of spectra forms a temporal "pseudo-dimension" that shows the changes caused by the process occurring in the sample. CS enables the use of small subsets of data, which minimizes the averaging of the effects studied. Yet, even within these limited timeframes, the sample undergoes certain changes. In this paper we discuss the effect of varying signal amplitude in a TR-NUS experiment. Our theoretical calculations show that the variations within the subsets lead to t1 -noise, which is dependent on the rate of change of the signal amplitude. We verify these predictions experimentally. As a model case we choose a novel 2D TR-NOESY experiment in which mixing time is varied in parallel with shuffled NUS in the indirect dimension. The experiment, performed on a sample of strychnine, provides a near-continuous NOE build-up curve, whose shape closely reflects the t1 -noise level. 2D TR-NOESY reduces the measurement time compared to the conventional approach and makes it possible to verify the theoretical predictions about signal variations during TR-NUS.

  11. Sequence-specific Assignment of 1H-NMR Resonance and Determination of the Secondary Structure of Jingzhaotoxin-Ⅰ

    Institute of Scientific and Technical Information of China (English)

    Xiong-Zhi ZENG; Qi ZHU; Song-Ping LIANG

    2005-01-01

    Jingzhaotoxin-Ⅰ (JZTX-Ⅰ) purified from the venom of the spider Chilobrachys jingzhao is a novel neurotoxin preferentially inhibiting cardiac sodium channel inactivation by binding to receptor site 3.The structure of this toxin in aqueous solution was investigated using 2-D 1H-NMR techniques. The complete sequence-specific assignments of proton resonance in the 1H-NMR spectra of JZTX-Ⅰ were obtained by analyzing a series of 2-D spectra, including DQF-COSY, TOCSY and NOESY spectra, in H2O and D2O. All the backbone protons except for Gln4 and more than 95% of the side-chain protons were identified by dαN,dαδ, dβN and dNN connectivities in the NOESY spectrum. These studies provide a basis for the further determination of the solution conformation of JZTX-Ⅰ. Furthermore, the secondary structure of JZTX-Ⅰ was identified from NMR data. It consists mainly of a short triple-stranded antiparallel β-sheet with Trp7-Cys9, Phe20-Lys23 and Leu28-Trp31. The characteristics of the secondary structure of JZTX-Ⅰ are similar to those of huwentoxin-Ⅰ (HWTX-Ⅰ) and hainantoxin-Ⅳ (HNTX-Ⅳ), whose structures in solution have previously been reported.

  12. Evaluation of the reliability of the maximum entropy method for reconstructing 3D and 4D NOESY-type NMR spectra of proteins.

    Science.gov (United States)

    Shigemitsu, Yoshiki; Ikeya, Teppei; Yamamoto, Akihiro; Tsuchie, Yuusuke; Mishima, Masaki; Smith, Brian O; Güntert, Peter; Ito, Yutaka

    2015-02-06

    Despite their advantages in analysis, 4D NMR experiments are still infrequently used as a routine tool in protein NMR projects due to the long duration of the measurement and limited digital resolution. Recently, new acquisition techniques for speeding up multidimensional NMR experiments, such as nonlinear sampling, in combination with non-Fourier transform data processing methods have been proposed to be beneficial for 4D NMR experiments. Maximum entropy (MaxEnt) methods have been utilised for reconstructing nonlinearly sampled multi-dimensional NMR data. However, the artefacts arising from MaxEnt processing, particularly, in NOESY spectra have not yet been clearly assessed in comparison with other methods, such as quantitative maximum entropy, multidimensional decomposition, and compressed sensing. We compared MaxEnt with other methods in reconstructing 3D NOESY data acquired with variously reduced sparse sampling schedules and found that MaxEnt is robust, quick and competitive with other methods. Next, nonlinear sampling and MaxEnt processing were applied to 4D NOESY experiments, and the effect of the artefacts of MaxEnt was evaluated by calculating 3D structures from the NOE-derived distance restraints. Our results demonstrated that sufficiently converged and accurate structures (RMSD of 0.91Å to the mean and 1.36Å to the reference structures) were obtained even with NOESY spectra reconstructed from 1.6% randomly selected sampling points for indirect dimensions. This suggests that 3D MaxEnt processing in combination with nonlinear sampling schedules is still a useful and advantageous option for rapid acquisition of high-resolution 4D NOESY spectra of proteins.

  13. Fluorescence Spectroscopy of tRNA[superscript Phe] Y Base in the Presence of Mg[superscript 2+] and Small Molecule Ligands

    Science.gov (United States)

    Kirk, Sarah R.; Silverstein, Todd P.; McFarlane Holman, Karen L.

    2008-01-01

    This laboratory project is one component of a semester-long advanced biochemistry laboratory course that uses several complementary techniques to study tRNA[superscript Phe] conformational changes induced by ligand binding. In this article we describe a set of experiments in which students use fluorescence spectroscopy to study tRNA[superscript…

  14. Incremental Validity of WISC-IV[superscript UK] Factor Index Scores with a Referred Irish Sample: Predicting Performance on the WIAT-II[superscript UK

    Science.gov (United States)

    Canivez, Gary L.; Watkins, Marley W.; James, Trevor; Good, Rebecca; James, Kate

    2014-01-01

    Background: Subtest and factor scores have typically provided little incremental predictive validity beyond the omnibus IQ score. Aims: This study examined the incremental validity of Wechsler Intelligence Scale for Children-Fourth UK Edition (WISC-IV[superscript UK]; Wechsler, 2004a, "Wechsler Intelligence Scale for Children-Fourth UK…

  15. Incremental Validity of WISC-IV[superscript UK] Factor Index Scores with a Referred Irish Sample: Predicting Performance on the WIAT-II[superscript UK

    Science.gov (United States)

    Canivez, Gary L.; Watkins, Marley W.; James, Trevor; Good, Rebecca; James, Kate

    2014-01-01

    Background: Subtest and factor scores have typically provided little incremental predictive validity beyond the omnibus IQ score. Aims: This study examined the incremental validity of Wechsler Intelligence Scale for Children-Fourth UK Edition (WISC-IV[superscript UK]; Wechsler, 2004a, "Wechsler Intelligence Scale for Children-Fourth UK…

  16. Main: 1H49 [RPSD[Archive

    Lifescience Database Archive (English)

    Full Text Available 1H49 トウモロコシ Corn Zea mays L. Beta-Glucosidase, Chloroplast Precursor Name=Glu1; Zea...NPWIYMYPEGLKDLLMIMKNKYGNPPIYITENGIGDVDTKETPLPMEAALNDYKRLDYIQRHIATLKESIDLGSNVQGYFAWSLLDNFEWFAGFTERYGIVYVDRNNNCTRYMKESAKWLKEFNTAKKPSKKILTPA corn_1H49.jpg ...

  17. Main: 1H81 [RPSD[Archive

    Lifescience Database Archive (English)

    Full Text Available 1H81 トウモロコシ Corn Zea mays L. Polyamine Oxidase Precursor Name=Pao; Zea Mays Molecul...PEGKGREFFLYASSRRGYYGVWQEFEKQYPDANVLLVTVTDEESRRIEQQSDEQTKAEIMQVLRKMFPGKDVPDATDILVPRWWSDRFYKGTFSNWPVGVNRYEYDQLRAPVGRVYFTGEHTSEHYNGYVHGAYLSGIDSAEILINCAQKKMCKYHVQGKYD corn_1H81.jpg ...

  18. Main: 1H86 [RPSD[Archive

    Lifescience Database Archive (English)

    Full Text Available 1H86 トウモロコシ Corn Zea mays L. Polyamine Oxidase Precursor Name=Pao; Zea Mays Molecul...PEGKGREFFLYASSRRGYYGVWQEFEKQYPDANVLLVTVTDEESRRIEQQSDEQTKAEIMQVLRKMFPGKDVPDATDILVPRWWSDRFYKGTFSNWPVGVNRYEYDQLRAPVGRVYFTGEHTSEHYNGYVHGAYLSGIDSAEILINCAQKKMCKYHVQGKYD corn_1H86.jpg ...

  19. Main: 1H84 [RPSD[Archive

    Lifescience Database Archive (English)

    Full Text Available 1H84 トウモロコシ Corn Zea mays L. Polyamine Oxidase Precursor Name=Pao; Zea Mays Molecul...GYYGVWQEFEKQYPDANVLLVTVTDEESRRIEQQSDEQTKAEIMQVLRKMFPGKDVPDATDILVPRWWSDRFYKGTFSNWPVGVNRYEYDQLRAPVGRVYFTGEHTSEHYNGYVHGAYLSGIDSAEILINCAQKKMCKYHVQGKYD corn_1H84.jpg ...

  20. Main: 1H83 [RPSD[Archive

    Lifescience Database Archive (English)

    Full Text Available 1H83 トウモロコシ Corn Zea mays L. Polyamine Oxidase Precursor Name=Pao; Zea Mays Molecul...GYYGVWQEFEKQYPDANVLLVTVTDEESRRIEQQSDEQTKAEIMQVLRKMFPGKDVPDATDILVPRWWSDRFYKGTFSNWPVGVNRYEYDQLRAPVGRVYFTGEHTSEHYNGYVHGAYLSGIDSAEILINCAQKKMCKYHVQGKYD corn_1H83.jpg ...

  1. Main: 1H82 [RPSD[Archive

    Lifescience Database Archive (English)

    Full Text Available 1H82 トウモロコシ Corn Zea mays L. Polyamine Oxidase Precursor Name=Pao; Zea Mays Molecul...PEGKGREFFLYASSRRGYYGVWQEFEKQYPDANVLLVTVTDEESRRIEQQSDEQTKAEIMQVLRKMFPGKDVPDATDILVPRWWSDRFYKGTFSNWPVGVNRYEYDQLRAPVGRVYFTGEHTSEHYNGYVHGAYLSGIDSAEILINCAQKKMCKYHVQGKYD corn_1H82.jpg ...

  2. Opposing Actions of Chronic[Deta][superscript 9] Tetrahydrocannabinol and Cannabinoid Antagonists on Hippocampal Long-Term Potentiation

    Science.gov (United States)

    Hoffman, Alexander F.; Oz, Murat; Yang, Ruiqin; Lichtman, Aron H.; Lupica, Carl R.

    2007-01-01

    Memory deficits produced by marijuana arise partly via interaction of the psychoactive component, [Deta][superscript 9]-tetrahydrocannabinol ([Deta][superscript 9]-THC), with cannabinoid receptors in the hippocampus. Although cannabinoids acutely reduce glutamate release and block hippocampal long-term potentiation (LTP), a potential substrate for…

  3. Integrating the SOP[superscript 2] Model into the Flipped Classroom to Foster Cognitive Presence and Learning Achievements

    Science.gov (United States)

    Chen, Hsiu-Ling; Chang, Chiung-Yun

    2017-01-01

    This study explored student teachers' cognitive presence and learning achievements by integrating the SOP[superscript 2] Model in which self-study (S), online group discussion (O) and double-stage presentations (P[superscript 2]) were implemented in the flipped classroom. The research was conducted at a university in Taiwan with 31 student…

  4. Combining ambiguous chemical shift mapping with structure-based backbone and NOE assignment from 15N-NOESY

    KAUST Repository

    Jang, Richard

    2011-01-01

    Chemical shift mapping is an important technique in NMRbased drug screening for identifying the atoms of a target protein that potentially bind to a drug molecule upon the molecule\\'s introduction in increasing concentrations. The goal is to obtain a mapping of peaks with known residue assignment from the reference spectrum of the unbound protein to peaks with unknown assignment in the target spectrum of the bound protein. Although a series of perturbed spectra help to trace a path from reference peaks to target peaks, a one-to-one mapping generally is not possible, especially for large proteins, due to errors, such as noise peaks, missing peaks, missing but then reappearing, overlapped, and new peaks not associated with any peaks in the reference. Due to these difficulties, the mapping is typically done manually or semi-automatically. However, automated methods are necessary for high-throughput drug screening. We present PeakWalker, a novel peak walking algorithm for fast-exchange systems that models the errors explicitly and performs many-to-one mapping. On the proteins: hBclXL, UbcH5B, and histone H1, it achieves an average accuracy of over 95% with less than 1.5 residues predicted per target peak. Given these mappings as input, we present PeakAssigner, a novel combined structure-based backbone resonance and NOE assignment algorithm that uses just 15N-NOESY, while avoiding TOCSY experiments and 13C- labeling, to resolve the ambiguities for a one-toone mapping. On the three proteins, it achieves an average accuracy of 94% or better. Copyright © 2011 ACM.

  5. Combining automated peak tracking in SAR by NMR with structure-based backbone assignment from 15N-NOESY

    KAUST Repository

    Jang, Richard

    2012-03-21

    Background: Chemical shift mapping is an important technique in NMR-based drug screening for identifying the atoms of a target protein that potentially bind to a drug molecule upon the molecule\\'s introduction in increasing concentrations. The goal is to obtain a mapping of peaks with known residue assignment from the reference spectrum of the unbound protein to peaks with unknown assignment in the target spectrum of the bound protein. Although a series of perturbed spectra help to trace a path from reference peaks to target peaks, a one-to-one mapping generally is not possible, especially for large proteins, due to errors, such as noise peaks, missing peaks, missing but then reappearing, overlapped, and new peaks not associated with any peaks in the reference. Due to these difficulties, the mapping is typically done manually or semi-automatically, which is not efficient for high-throughput drug screening.Results: We present PeakWalker, a novel peak walking algorithm for fast-exchange systems that models the errors explicitly and performs many-to-one mapping. On the proteins: hBclXL, UbcH5B, and histone H1, it achieves an average accuracy of over 95% with less than 1.5 residues predicted per target peak. Given these mappings as input, we present PeakAssigner, a novel combined structure-based backbone resonance and NOE assignment algorithm that uses just 15N-NOESY, while avoiding TOCSY experiments and 13C-labeling, to resolve the ambiguities for a one-to-one mapping. On the three proteins, it achieves an average accuracy of 94% or better.Conclusions: Our mathematical programming approach for modeling chemical shift mapping as a graph problem, while modeling the errors directly, is potentially a time- and cost-effective first step for high-throughput drug screening based on limited NMR data and homologous 3D structures. 2012 Jang et al.; licensee BioMed Central Ltd.

  6. Complete {sup 1}H and {sup 13}C NMR assignments and anti fungal activity of two 8-hydroxy flavonoids in mixture

    Energy Technology Data Exchange (ETDEWEB)

    Johann, Susana; Smania Junior, Artur [Universidade Federal de Santa Catarina (UFSC), Florianopolis, SC (Brazil). Dept. de Microbiologia e Parasitologia. Lab. de Antibioticos; Pizzolatti, Moacir G. [Universidade Federal de Santa Catarina (UFSC), Florianopolis, SC (Brazil). Dept. de Quimica; Schripsema, Jan; Braz-Filho, Raimundo [Universidade Estadual do Norte Fluminense (UENF), Campos dos Goytacazes, RJ (Brazil). Setor de Quimica de Produtos Naturais. Lab. de Quimica e Funcao de Proteinas e Peptideos (LQFPP); Branco, Alexsandro [Universidade Estadual de Feira de Santana, BA (Brazil). Dept. de Saude. Lab. de Fitoquimica]. E-mail: branco@uefs.br

    2007-06-15

    A mixture of the two new flavonols 8-hydroxy-3, 4', 5, 6, 7-pentamethoxyflavone (1) and 8-hydroxy-3, 3', 4', 5, 6, 7-hexamethoxyflavone (2) was isolated from a commercial sample of Citrus aurantifolia. An array of one- ({sup 1}H NMR, {l_brace}{sup 1}H{r_brace} {sup -13}C NMR, and APT{sup -13}C NMR) and two-dimensional NMR techniques (COSY, NOESY, HMQC and HMBC) was used to achieve the structural elucidation and the complete {sup 1}H and {sup 13}C chemical shift assignments of these natural compounds. In addition, the antifungal activity of these compounds against phytopathogenic and human pathogenic fungi was investigated. (author)

  7. Training Scientific Thinking Skills: Evidence from an MCAT[superscript 2015]-Aligned Classroom Module

    Science.gov (United States)

    Stevens, Courtney; Witkow, Melissa R.

    2014-01-01

    The present study reports on the development and evaluation of a classroom module to train scientific thinking skills. The module was implemented in two of four parallel sections of introductory psychology. To assess learning, a passage-based question set from the medical college admissions test (MCAT[superscript 2015]) preview guide was included…

  8. An Analysis of Different Representations for Vectors and Planes in R[superscript 3]: Learning Challenges

    Science.gov (United States)

    Sandoval, Ivonne; Possani, Edgar

    2016-01-01

    The purpose of this paper is to present an analysis of the difficulties faced by students when working with different representations of vectors, planes and their intersections in R[superscript 3]. Duval's theoretical framework on semiotic representations is used to design a set of evaluating activities, and later to analyze student work. The…

  9. Aligning Cost Assessment with Community-Based Participatory Research: The Kin Keeper (superscript SM) Intervention

    Science.gov (United States)

    Meghea, Cristian Ioan; Williams, Karen Patricia

    2015-01-01

    The few existing economic evaluations of community-based health promotion interventions were reported retrospectively at the end of the trial. We report an evaluation of the costs of the Kin Keeper(superscript SM) Cancer Prevention Intervention, a female family-focused educational intervention for underserved women applied to increase breast and…

  10. Relativistic Momentum and Kinetic Energy, and E = mc[superscript 2

    Science.gov (United States)

    Hu, Ben Yu-Kuang

    2009-01-01

    Based on relativistic velocity addition and the conservation of momentum and energy, I present simple derivations of the expressions for the relativistic momentum and kinetic energy of a particle, and for the formula E = mc[superscript 2]. (Contains 5 footnotes and 2 figures.)

  11. LE[superscript 3]AD Academy Builds Professionalism in Vocational Students

    Science.gov (United States)

    Hall, Candace

    2012-01-01

    Principal David Wheeler of Southeastern Regional Vocational-Technical High School founded LE[superscript 3]AD Academy--an innovative program that gives students the opportunity to build and run their own town in teams and with guidance from teachers. The program started in the spring of 2011, and it is innovative in many ways. The students' main…

  12. Characterization of heroin samples by 1H NMR and 2D DOSY 1H NMR.

    Science.gov (United States)

    Balayssac, Stéphane; Retailleau, Emmanuel; Bertrand, Geneviève; Escot, Marie-Pierre; Martino, Robert; Malet-Martino, Myriam; Gilard, Véronique

    2014-01-01

    Twenty-four samples of heroin from different illicit drug seizures were analyzed using proton Nuclear Magnetic Resonance ((1)H NMR) and two-dimensional diffusion-ordered spectroscopy (2D DOSY) (1)H NMR. A careful assignment and quantification of (1)H signals enabled a comprehensive characterization of the substances present in the samples investigated: heroin, its main related impurities (6-acetylmorphine, acetylcodeine, morphine, noscapine and papaverine) and cutting agents (caffeine and acetaminophen in nearly all samples as well as lactose, lidocaine, mannitol, piracetam in one sample only), and hence to establish their spectral signatures. The good agreement between the amounts of heroin, noscapine, caffeine and acetaminophen determined by (1)H NMR and gas chromatography, the reference method in forensic laboratories, demonstrates the validity of the (1)H NMR technique. In this paper, 2D DOSY (1)H NMR offers a new approach for a whole characterization of the various components of these complex mixtures.

  13. Applications of the Theorem of Pythagoras in R[superscript 3

    Science.gov (United States)

    Srinivasan, V. K.

    2010-01-01

    Three distinct points A = (a, 0, 0) B = (0, b, 0) and (c, 0, 0) with abc not equal to 0 are taken, respectively on the "x", "y" and the "z"-axes of a rectangular coordinate system in R[superscript 3]. Using the converse of the theorem of Pythagoras, it is shown that the triangle [delta]ABC can never be a right-angled triangle. The result seems to…

  14. Formation of an Oxidant-Sensible Pd(II) Coordination Compound and Its [superscript 1]H NMR Specific Characterization: A Preparative and Analytical Challenge in Current Coordination Chemistry

    Science.gov (United States)

    Abraham, Maria L.; Oppel, Iris M.

    2014-01-01

    A three-part experiment that leads to the synthesis of palladium(II) complex starting from a C[subscript 3]-symmetric triaminoguanidinium-based ligand is presented. In the first part, the preparation of tris-benzylidenetriaminoguanidinium chloride ([H[subscript 6]Br[subscript 3]L]Cl) by an acidic catalyzed 3-fold imine formation reaction of…

  15. Why Are [superscript 1]H NMR Integrations Not Perfect? An Inquiry-Based Exercise for Exploring the Relationship between Spin Dynamics and NMR Integration in the Organic Laboratory

    Science.gov (United States)

    Weizman, Haim

    2008-01-01

    When FT-NMR is used to collect data without a sufficient delay time between subsequent pulses, the integrated area under certain peaks may result in a lower value than should be observed under appropriate conditions. This discrepancy in integration may deceive the inexperienced eye and consequently can lead to a wrong assignment of the NMR…

  16. Enzymatic Resolution of 1-Phenylethanol and Formation of a Diastereomer: An Undergraduate [superscript 1]H NMR Experiment to Introduce Chiral Chemistry

    Science.gov (United States)

    Faraldos, Juan A.; Giner, Jos-Luis; Smith, David H.; Wilson, Mark; Ronhovde, Kyla; Wilson, Erin; Clevette, David; Holmes, Andrea E.; Rouhier, Kerry

    2011-01-01

    This organic laboratory experiment introduces students to stereoselective enzyme reactions, resolution of enantiomers, and NMR analysis of diastereomers. The reaction between racemic 1-phenylethanol and vinyl acetate in hexane to form an ester is catalyzed by acylase I. The unreacted alcohol is then treated with a chiral acid and the resulting…

  17. Test Review: Wechsler, D. (2014),"Wechsler Intelligence Scale for Children, Fifth Edition: Canadian 322 (WISC-V[superscript CDN])." Toronto, Ontario: Pearson Canada Assessment.

    Science.gov (United States)

    Cormier, Damien C.; Kennedy, Kathleen E.; Aquilina, Alexandra M.

    2016-01-01

    The Wechsler Intelligence Scale for Children, Fifth Edition: Canadian (WISC-V[superscript CDN]; Wechsler, 2014) is published by Pearson Canada Assessment. The WISC-V[superscript CDN] is a norm-referenced, individually administered intelligence battery that provides a comprehensive diagnostic profile of the cognitive strengths and weaknesses of…

  18. Sequential sup 1 H NMR assignments and secondary structure of an IgG-binding domain from protein G

    Energy Technology Data Exchange (ETDEWEB)

    Lian, L.Y.; Yang, J.C.; Derrick, J.P.; Sutcliffe, M.J.; Roberts, G.C.K. (Univ. of Leicester (England)); Murphy, J.P.; Goward, C.R.; Atkinson, T. (PHLS Center for Applied Microbiology and Research, Porton Down, Salisbury (England))

    1991-06-04

    Protein G is a member of a class of cell surface bacterial proteins from Streptococcus that bind IgG with high affinity. A fragment of molecular mass 6,988, which retains IgG-binding activity, has been generated by proteolytic digestion and analyzed by {sup 1}H NMR. Two-dimenstional DQF-COSY, TOCSY, and NOESY spectra have been employed to assign the {sup 1}H NMR spectrum of the peptide. Elements of regular secondary structure have been identified by using nuclear Overhauser enhancement, coupling constant, and amide proton exchange data. The secondary structure consists of a central {alpha}-helix (Ala28-Val44), flanked by two portions of {beta}-sheet (Val5-Val26 and Asp45-Lys62). This is a fundamentally different arrangement of secondary structure from that of protein A, which is made up of three consecutive {alpha}-helics in free solution. The authors conclude that the molecular mechanisms underlying the association of protein A and protein G with IgG are different.

  19. Solution 1H, 15N NMR spectroscopic characterization of substrate-bound, cyanide-inhibited human heme oxygenase: water occupation of the distal cavity.

    Science.gov (United States)

    Li, Yiming; Syvitski, Ray T; Auclair, Karine; Ortiz de Montellano, Paul; La Mar, Gerd N

    2003-11-05

    A solution NMR spectroscopic study of the cyanide-inhibited, substrate-bound complex of uniformly (15)N-labeled human heme oxygenase, hHO, has led to characterization of the active site with respect to the nature and identity of strong hydrogen bonds and the occupation of ordered water molecules within both the hydrogen bonding network and an aromatic cluster on the distal side. [(1)H-(15)N]-HSQC spectra confirm the functionalities of several key donors in particularly robust H-bonds, and [(1)H-(15)N]HSQC-NOESY spectra lead to the identification of three additional robust H-bonds, as well as the detection of two more relatively strong H-bonds whose identities could not be established. The 3D NMR experiments provided only a modest, but important, extension of assignments because of the loss of key TOCSY cross-peaks due to the line broadening from a dynamic heterogeneity in the active site. Steady-state NOEs upon saturating the water signal locate nine ordered water molecules in the immediate vicinity of the H-bond donors, six of which are readily identified in the crystal structure. The additional three are positioned in available spaces to account for the observed NOEs. (15)N-filtered steady-state NOEs upon saturating the water resonances and (15)N-filtered NOESY spectra demonstrate significant negative NOEs between water molecules and the protons of five aromatic rings. Many of the NOEs can be rationalized by water molecules located in the crystal structure, but strong water NOEs, particularly to the rings of Phe47 and Trp96, demand the presence of at least an additional two immobilized water molecules near these rings. The H-bond network appears to function to order water molecules to provide stabilization for the hydroperoxy intermediate and to serve as a conduit to the active site for the nine protons required per HO turnover.

  20. A sup 1 H NMR study of human calcitonin in solution

    Energy Technology Data Exchange (ETDEWEB)

    Motta, A. (Consiglio Nazionale delle Richerche, Napoli (Italy)); Temussi, P.A. (Univ. di Napoli (Italy)); Wuensch, E.; Bovermann, G. (Max-Planck-Inst. fuer Biochemie, Martinsried bei Muenchen (West Germany))

    1991-03-05

    Human calcitonin (hCT) has been investigated by NMR at 400 MHz in DMSO{sub d6} and in an 85% DMSO{sub d6}-15% {sup 1}H{sub 2}O (v/v) cryoprotective mixture. All backbone and side-chain resonances have been assigned and the secondary structure has been determined in both solvents. In DMSO{sub d6}, the simultaneous presence of d{sub {alpha}N}, d{sub NN}, and some specific weak medium-range nuclear Overhauser effects, together with the amide temperature coefficients and the analysis of the NH-{alpha}CH spin-spin coupling constants, indicates that hCT is highly flexible but with three domains (comprising segments Asn{sup 3}-Gly{sup 10}, Gln{sup 14}-Thr{sup 21}, and Thr{sup 25}-Ala{sup 31}) in extended conformations which dynamically transform into isolated {beta} turns in the N- and C-terminal regions and into adjacent tight turns, resembling a 3{sub 10} helix structure, in the central part. The DMSO-water mixture rigidifies the polypeptide chain, favoring and ordered, extended conformation. NOESY data indicate the presence of a short double-stranded antiparallel {beta} sheet in the central region made by residues 16-21 and connected by a two-residue hairpin loop formed by residues 18 and 19. Two tight turns, formed by residues 3-6 and 28-31, were also identified. The central {beta} sheet does not favor an amphipathic distribution of the residues as found for salmon calcitonin. This is in agreement with the smaller tendency of hCT to form the amphipathic {alpha} helix, postulated to be responsible for the interaction of hCT with lipids. The possible role of the cis-trans isomerism of Pro is discussed.

  1. NMR of 133Cs+ in stretched hydrogels: One-dimensional, z- and NOESY spectra, and probing the ion's environment in erythrocytes

    Science.gov (United States)

    Kuchel, Philip W.; Shishmarev, Dmitry; Puckeridge, Max; Levitt, Malcolm H.; Naumann, Christoph; Chapman, Bogdan E.

    2015-12-01

    133Cs nuclear magnetic resonance (NMR) spectroscopy was conducted on 133Cs+ in gelatin hydrogels that were either relaxed or stretched. Stretching generated a septet from this spin-7/2 nucleus, and its nuclear magnetic relaxation was studied via z-spectra, and two-dimensional nuclear Overhauser (NOESY) spectroscopy. Various spectral features were well simulated by using Mathematica and the software package SpinDynamica. Spectra of CsCl in suspensions of human erythrocytes embedded in gelatin gel showed separation of the resonances from the cation inside and outside the cells. Upon stretching the sample, the extracellular 133Cs+ signal split into a septet, while the intracellular peak was unchanged, revealing different alignment/ordering properties of the environment inside and around the cells. Differential interference contrast light microscopy confirmed that the cells were stretched when the overall sample was elongated. Analysis of the various spectral features of 133Cs+ reported here opens up applications of this K+ congener for studies of cation-handling by metabolically-active cells and tissues in aligned states.

  2. Hydrolysis Studies and Quantitative Determination of Aluminum Ions Using [superscript 27]Al NMR: An Undergraduate Analytical Chemistry Experiment

    Science.gov (United States)

    Curtin, Maria A.; Ingalls, Laura R.; Campbell, Andrew; James-Pederson, Magdalena

    2008-01-01

    This article describes a novel experiment focused on metal ion hydrolysis and the equilibria related to metal ions in aqueous systems. Using [superscript 27]Al NMR, the students become familiar with NMR spectroscopy as a quantitative analytical tool for the determination of aluminum by preparing a standard calibration curve using standard aluminum…

  3. Photochemical Synthesis and Ligand Exchange Reactions of Ru(CO)[subscript 4] (Eta[superscript 2]-Alkene) Compounds

    Science.gov (United States)

    Cooke, Jason; Berry, David E.; Fawkes, Kelli L.

    2007-01-01

    The photochemical synthesis and subsequent ligand exchange reactions of Ru(CO)[subscript 4] (eta[superscript2]-alkene) compounds has provided a novel experiment for upper-level inorganic chemistry laboratory courses. The experiment is designed to provide a system in which the changing electronic properties of the alkene ligands could be easily…

  4. [[superscript 3]H]-Flunitrazepam-Labeled Benzodiazepine Binding Sites in the Hippocampal Formation in Autism: A Multiple Concentration Autoradiographic Study

    Science.gov (United States)

    Guptill, Jeffrey T.; Booker, Anne B.; Gibbs, Terrell T.; Kemper, Thomas L.; Bauman, Margaret L.; Blatt, Gene J.

    2007-01-01

    Increasing evidence indicates that the GABAergic system in cerebellar and limbic structures is affected in autism. We extended our previous study that found reduced [[superscript 3]H] flunitrazepam-labeled benzodiazepine sites in the autistic hippocampus to determine whether this reduction was due to a decrease in binding site number (B [subscript…

  5. Role of L-Type Ca[superscript 2+] Channel Isoforms in the Extinction of Conditioned Fear

    Science.gov (United States)

    Busquet, Perrine; Hetzenauer, Alfred; Sinnegger-Brauns, Martina J.; Striessnig, Jorg; Singewald, Nicolas

    2008-01-01

    Dihydropyridine (DHP) L-type Ca[superscript 2+] channel (LTCC) antagonists, such as nifedipine, have been reported to impair the extinction of conditioned fear without interfering with its acquisition. Identification of the LTCC isoforms mediating this DHP effect is an essential basis to reveal their role as potential drug targets for the…

  6. Observation of 1H-13C and 1H-1H proximities in a paramagnetic solid by NMR at high magnetic field under ultra-fast MAS

    Science.gov (United States)

    Li, Shenhui; Trébosc, Julien; Lafon, Olivier; Zhou, Lei; Shen, Ming; Pourpoint, Frédérique; Amoureux, Jean-Paul; Deng, Feng

    2015-02-01

    The assignment of NMR signals in paramagnetic solids is often challenging since: (i) the large paramagnetic shifts often mask the diamagnetic shifts specific to the local chemical environment, and (ii) the hyperfine interactions with unpaired electrons broaden the NMR spectra and decrease the coherence lifetime, thus reducing the efficiency of usual homo- and hetero-nuclear NMR correlation experiments. Here we show that the assignment of 1H and 13C signals in isotopically unmodified paramagnetic compounds with moderate hyperfine interactions can be facilitated by the use of two two-dimensional (2D) experiments: (i) 1H-13C correlations with 1H detection and (ii) 1H-1H double-quantum ↔ single-quantum correlations. These methods are experimentally demonstrated on isotopically unmodified copper (II) complex of L-alanine at high magnetic field (18.8 T) and ultra-fast Magic Angle Spinning (MAS) frequency of 62.5 kHz. Compared to 13C detection, we show that 1H detection leads to a 3-fold enhancement in sensitivity for 1H-13C 2D correlation experiments. By combining 1H-13C and 1H-1H 2D correlation experiments with the analysis of 13C longitudinal relaxation times, we have been able to assign the 1H and 13C signals of each L-alanine ligand.

  7. Crystalline 1H-1,2,3-triazol-5-ylidenes

    Energy Technology Data Exchange (ETDEWEB)

    Bertrand, Guy; Gulsado-Barrios, Gregorio; Bouffard, Jean; Donnadieu, Bruno

    2016-08-02

    The present invention provides novel and stable crystalline 1H-1,2,3 triazolium carbenes and metal complexes of 1H-1,2,3 triazolium carbenes. The present invention also provides methods of making 1H-1,2,3 triazolium carbenes and metal complexes of 1H-1,2,3 triazolium carbenes. The present invention also provides methods of using 1H-1,2,3 triazolium carbenes and metal complexes of 1H-1,2,3 triazolium carbenes in catalytic reactions.

  8. Analysis list: Nr1h3 [Chip-atlas[Archive

    Lifescience Database Archive (English)

    Full Text Available Nr1h3 Liver + mm9 http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/target/Nr1h3.1.tsv... http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/target/Nr1h3.5.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/target/Nr1h...3.10.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/colo/Nr1h3.Liver.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/colo/Liver.gml ...

  9. Analysis list: Nr1h2 [Chip-atlas[Archive

    Lifescience Database Archive (English)

    Full Text Available Nr1h2 Blood + mm9 http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/target/Nr1h2.1.tsv... http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/target/Nr1h2.5.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/target/Nr1h...2.10.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/colo/Nr1h2.Blood.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/colo/Blood.gml ...

  10. Analysis list: NR1H3 [Chip-atlas[Archive

    Lifescience Database Archive (English)

    Full Text Available NR1H3 Adipocyte,Blood + hg19 http://dbarchive.biosciencedbc.jp/kyushu-u/hg19/target.../NR1H3.1.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/hg19/target/NR1H3.5.tsv http://dbarchive.bioscienced...bc.jp/kyushu-u/hg19/target/NR1H3.10.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/hg19/colo/NR1H3.Adipocyte....tsv,http://dbarchive.biosciencedbc.jp/kyushu-u/hg19/colo/NR1H3.Blood.tsv http://dbarchive.bioscience...dbc.jp/kyushu-u/hg19/colo/Adipocyte.gml,http://dbarchive.biosciencedbc.jp/kyushu-u/hg19/colo/Blood.gml ...

  11. Main: 1H1Y [RPSD[Archive

    Lifescience Database Archive (English)

    Full Text Available 1H1Y イネ Rice Oryza sativa L. D-Ribulose-5-Phosphate 3-Epimerase Oryza Sativa Molecu...V. 326 127 2003 3-Epimerase, Oxidative Pentose Phosphate Pathway, Isomerase SWS:Q9SE42,Q9SE42|EMBL; AF189365; AAF01048.1; -.|PDB; 1H...1Y; X-ray; A/B=1-228.|PDB; 1H1Z; X-ray; A/B=1-228.|Gramene; Q9SE42; -.|GO; GO:001685...ELIQSIKAKGMRPGVSLRPGTPVEEVFPLVEAENPVELVLVMTVEPGFGGQKFMPEMMEKVRALRKKYPSLDIEVDGGLGPSTIDVAASAGANCIVAGSSIFGAAEPGEVISALRKSVEGSQNKS rice_1H1Y.jpg ...

  12. The Flexible Mind Is Associated with the Catechol-O-Methyltransferase (COMT) Val[superscript 158]Met Polymorphism: Evidence for a Role of Dopamine in the Control of Task-Switching

    Science.gov (United States)

    Colzato, Lorenza S.; Waszak, Florian; Nieuwenhuis, Sander; Posthuma, Danielle; Hommel, Bernhard

    2010-01-01

    Genetic variability related to the catechol-O-methyltransferase (COMT) gene Val[superscript 128]Met polymorphism) has received increasing attention as a possible modulator of cognitive control functions. Recent evidence suggests that the Val[superscript 128]Met genotype may differentially affect cognitive stability and flexibility, in such a way…

  13. 4-Bromo-3-methoxy-1-phenyl-1H-pyrazole

    Directory of Open Access Journals (Sweden)

    Algirdas Šačkus

    2009-11-01

    Full Text Available The title compound was prepared by treatment of 4-bromo-1-phenyl-1H-pyrazol-3-ol with sodium hydride/methyl iodide in good yield. Detailed spectroscopic data (1H NMR, 13C NMR, 15N NMR, IR, MS are presented.

  14. Influence of local molecular motions on the determination of 1H-1H internuclear distances measured by 2D 1H spin-exchange experiments.

    Science.gov (United States)

    Brus, J; Petrícková, H; Dybal, J

    2003-06-01

    Analysis of spin-exchange build-up curves obtained by measurement of 2D 1H CRAMPS spectra of alpha-glycine was performed to evaluate the rate of 1H-1H spin-exchange process with respect to the influence of variation in internal molecular motion. Differences in local motions significantly affect spin-exchange constants even in highly rigid organic solids with virtually uniform motion behavior. The polarization transfer between nonequivalent alpha-protons is described by the spin-exchange constant D=0.77 nm(2)ms(-1), while the polarization transfer involving spin exchange between alphaH and NH(3)(+) protons is characterized by D=0.24-0.21 nm(2)ms(-1). This significant decrease corresponds to rotation of hydrogen-bonded amino groups. Neglecting this variation in local spin-exchange constants the resulting calculated 1H-1H distance can be overestimated by up to 100%. Complications following from relayed and back polarization transfer involving the nearest spins within one functional group (e.g., CH(2) and/or NH(3)(+)) and intermolecular spin exchange are discussed. It was shown that 2H quadrupolar splitting determined for selected sites directly correlates with the experimentally observed differences in spin-exchange coefficients. It is also demonstrated that a medium level quantum chemical calculation of molecular dynamics provides relevant data that can be used to estimate differences in molecular motions.

  15. {sup 1}H MR spectroscopic patterns of normal adult brain

    Energy Technology Data Exchange (ETDEWEB)

    Song, In Chan; Chang, Kee Hyun; Min, Kwan Hong; Kim, Dong Sung; Han, Moon Hee; Kang, Sa Ouk; Min, Byoung Goo; Han, Man Chung [Seoul National Univ. College of Medicine, Seoul (Korea, Republic of)

    1996-10-01

    To evaluate regional differences of {sup 1}H magnetic resonance(MR) spectral patterns in normal adult human brains. A total of 44 {sup 1}H MR spectra in 25 volunteers aged 27-45 were obtained in five regions including the frontal lobe(10), parietal lobe(10), temporal lobe(5), basal ganglia(10) and thalamus(9). {sup 1}H MR spectroscopy(MRS) was performed using a PRESS sequence with a TR of 2000 ms and a TE of 270ms from a volume of cm on a 1.5T clinical MR unit. Relative metabolite ratios of NAA/Cho, NAA/Cr and Cr/Cho in each region were measured and compared. A total of 44 reliable spectra were successfully obtained in all regions. NAA/Cho, NAA/Cr and Cr/Cho ratios varied considerably, ranging from 1.09{+-}0.2 to 2.46{+-}0.25, from 1.72{+-}0.35 to 2.45{+-}0.25 and from 0.64{+-}0.1 to 1.01{+-}0.12, respectively. Significant regional differences in metabolite ratios were observed; higher NAA/Cho and NAA/Cr ratios in the parietal lobe, lower NAA/Cho ratios in the temporal lobe, and lower Cr/Cho ratios in the temporal lobe compared to those of other regions(p<0.05). Differences in metabolite ratios between the right and left frontal lobes, and between the right and left basal ganglias were not significant. {sup 1}H MR spectra of the normal adult human brains using in vivo single voxel {sup 1}H MRS represented significant regional differences in metabolite ratios of NAA/Cho, NAA/Cr and Cr/Cho. Our {sup 1}H MR spectroscopic results are a useful reference for assessing the {sup 1}H MRS pattern of various intracranial diseases.

  16. Following Metabolism in Living Microorganisms by Hyperpolarized (1)H NMR.

    Science.gov (United States)

    Dzien, Piotr; Fages, Anne; Jona, Ghil; Brindle, Kevin M; Schwaiger, Markus; Frydman, Lucio

    2016-09-21

    Dissolution dynamic nuclear polarization (dDNP) is used to enhance the sensitivity of nuclear magnetic resonance (NMR), enabling monitoring of metabolism and specific enzymatic reactions in vivo. dDNP involves rapid sample dissolution and transfer to a spectrometer/scanner for subsequent signal detection. So far, most biologically oriented dDNP studies have relied on hyperpolarizing long-lived nuclear spin species such as (13)C in small molecules. While advantages could also arise from observing hyperpolarized (1)H, short relaxation times limit the utility of prepolarizing this sensitive but fast relaxing nucleus. Recently, it has been reported that (1)H NMR peaks in solution-phase experiments could be hyperpolarized by spontaneous magnetization transfers from bound (13)C nuclei following dDNP. This work demonstrates the potential of this sensitivity-enhancing approach to probe the enzymatic process that could not be suitably resolved by (13)C dDNP MR. Here we measured, in microorganisms, the action of pyruvate decarboxylase (PDC) and pyruvate formate lyase (PFL)-enzymes that catalyze the decarboxylation of pyruvate to form acetaldehyde and formate, respectively. While (13)C NMR did not possess the resolution to distinguish the starting pyruvate precursor from the carbonyl resonances in the resulting products, these processes could be monitored by (1)H NMR at 500 MHz. These observations were possible in both yeast and bacteria in minute-long kinetic measurements where the hyperpolarized (13)C enhanced, via (13)C → (1)H cross-relaxation, the signals of protons binding to the (13)C over the course of enzymatic reactions. In addition to these spontaneous heteronuclear enhancement experiments, single-shot acquisitions based on J-driven (13)C → (1)H polarization transfers were also carried out. These resulted in higher signal enhancements of the (1)H resonances but were not suitable for multishot kinetic studies. The potential of these (1)H-based approaches for

  17. 2D 1H -13C Heteronuclear Shift Correlation Of 2a - Hydroxy Aiantolactone From Pulicaria Undulata C.A. Mey

    Directory of Open Access Journals (Sweden)

    A. Rustaiyan

    1992-07-01

    Full Text Available We have reported recently the isolation and characterization of several sesquiterpene lactones from Pulicaria undulata (1."nThe lactones were isolated from an Et20 - Petrol (1:3 fraction by different chromatographic techniques including HPLC (RP 8, MeOH - H2O, 13:7."nIn this way three eudesmanolides 1 - 3, a guaianolide 4, a nor -guaianolide 5, as well as the pseudoguaianolide 6 and the xanthanolide 7 were isolated. One of the eudesmanolides (2a - hydroxy aiantolactone, 1, was present as the main component."nSuch lactones being known as biologically active substances, we have decided to describe for the first time a detailed interpretation of proton, 1H -NMR, 13C - NMR and 2D lH -13C - heteronuclear shift correlation spectra of 2a - hydroxy aiantolactone. The stereochemistry of C - 2 , C - 7 and C - 8 was determined by the NOESY experiments, H - 7 and H - 8 are in the a configuration and H - 2 is in the b configuration.

  18. 1H n.m.r. conformational studies on the C-terminal octapeptide of oxyntomodulin, a beta-turn locked by a salt bridge.

    Science.gov (United States)

    Aumelas, A; Audousset-Puech, M P; Heitz, A; Bataille, D; Martinez, J

    1989-10-01

    The octapeptide Lys-Arg-Asn-Lys-Asn-Asn-Ile-Ala (Arg4 in the human sequence) is the C-terminal part of porcine oxyntomodulin, an endogeneous peptide which is a potent inhibitor of stimulated acid secretion. This octapeptide exhibits the whole range of biological activities of the parent hormone. In the present work we report an 1H n.m.r. investigation of the conformational properties of the octapeptides of pig and human sequences in dimethylsulfoxide-d6 (DMSO) solution. The various resonances were assigned on the basis of two-dimensional COSY and NOESY experiments. Other experiments such as (i) temperature and concentration dependence of the amide proton chemical shifts, (ii) effects of ionic strength, (iii) comparison of the spectra with different analogues, were performed. We showed that in DMSO, the conformation of the octapeptide is directly related to the ionisation state of the C-terminus carboxyl group of alanine. In carboxylic state, the peptide adopts an extended conformation, while in the carboxylate state the four last residues (Asn-Asn-Ile-Ala) are involved in a type II beta-turn structure probably locked by a salt bridge between the carboxyl group of Ala8 and the epsilon ammonium group of Lys4 (or the guanidinium group of Arg4). These observations provide an insight into the possible conformational tendencies of this peptide in biological media.

  19. Screening protein-ligand interactions using {sup 1}H NMR techniques for detecting the ligand; Mapeamento das interacoes proteina-ligante atraves de tecnicas de RMN de {sup 1}H utilizando deteccao do ligante

    Energy Technology Data Exchange (ETDEWEB)

    Figueiredo, Isis Martins; Marsaioli, Anita Jocelyne [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Inst. de Quimica. Dept. de Quimica Organica]. E-mail: anita@iqm.unicamp.br

    2007-07-01

    NMR is a valuable screening tool for the binding of ligands to proteins providing structural information on both protein and ligands and is thus largely applied to drug-discovery. Among the recent NMR techniques to probe weak binding protein-ligand complexes we have critically evaluated the advantages and disadvantages of STD (Saturation Transfer Difference), WaterLOGSY (Water Ligand Observation with Gradient Spectroscopy), NOE pumping and DOSY-NOESY (Diffusion-Ordered NOESY) using a mixture of BSA (bovine serum albumin) plus salicylic acid, caffeine, citric acid, adipic acid and D-glucose. (author)

  20. A Discovery-Based Hydrochlorination of Carvone Utilizing a Guided-Inquiry Approach to Determine the Product Structure from [superscript 13]C NMR Spectra

    Science.gov (United States)

    Pelter, Michael W.; Walker, Natalie M.

    2012-01-01

    This experiment describes a discovery-based method for the regio- and stereoselective hydrochlorination of carvone, appropriate for a 3-h second-semester organic chemistry laboratory. The product is identified through interpretation of the [superscript 13]C NMR and DEPT spectra are obtained on an Anasazi EFT-60 at 15 MHz as neat samples. A…

  1. Binary Logistic Regression Analysis for Detecting Differential Item Functioning: Effectiveness of R[superscript 2] and Delta Log Odds Ratio Effect Size Measures

    Science.gov (United States)

    Hidalgo, Mª Dolores; Gómez-Benito, Juana; Zumbo, Bruno D.

    2014-01-01

    The authors analyze the effectiveness of the R[superscript 2] and delta log odds ratio effect size measures when using logistic regression analysis to detect differential item functioning (DIF) in dichotomous items. A simulation study was carried out, and the Type I error rate and power estimates under conditions in which only statistical testing…

  2. Binary Logistic Regression Analysis for Detecting Differential Item Functioning: Effectiveness of R[superscript 2] and Delta Log Odds Ratio Effect Size Measures

    Science.gov (United States)

    Hidalgo, Mª Dolores; Gómez-Benito, Juana; Zumbo, Bruno D.

    2014-01-01

    The authors analyze the effectiveness of the R[superscript 2] and delta log odds ratio effect size measures when using logistic regression analysis to detect differential item functioning (DIF) in dichotomous items. A simulation study was carried out, and the Type I error rate and power estimates under conditions in which only statistical testing…

  3. The Relationship between Post Reach Exit Exam (E[superscript 2]) Failure Remediation and NCLEX-RN Success of Graduates of Baccalaureate Nursing Programs

    Science.gov (United States)

    Allen, Patricia Gale

    2009-01-01

    An ex post facto study was conducted to determine whether any relationship exists between remediation post Reach Exit Exam (E[superscript 2]) failure and NCLEX-RN success of graduates of baccalaureate nursing programs. Data was gathered from responses to the seventh annual validity study (V7S) offered to deans and directors of nursing programs by…

  4. A Discovery-Based Hydrochlorination of Carvone Utilizing a Guided-Inquiry Approach to Determine the Product Structure from [superscript 13]C NMR Spectra

    Science.gov (United States)

    Pelter, Michael W.; Walker, Natalie M.

    2012-01-01

    This experiment describes a discovery-based method for the regio- and stereoselective hydrochlorination of carvone, appropriate for a 3-h second-semester organic chemistry laboratory. The product is identified through interpretation of the [superscript 13]C NMR and DEPT spectra are obtained on an Anasazi EFT-60 at 15 MHz as neat samples. A…

  5. Students' Understanding of Limiting Behavior at a Point for Functions from [Set of Real Numbers][superscript 2] to [Set of Real Numbers

    Science.gov (United States)

    Mamona-Downs, Joanna K.; Megalou, Foteini J.

    2013-01-01

    The aim of this paper is to examine students' understanding of the limiting behavior of a function from [set of real numbers][superscript 2] to [set of real numbers] at a point "P." This understanding depends on which definition is used for a limit. Several definitions are considered; two of these concern the notion of a neighborhood of "P", while…

  6. Alterations in CNS Activity Induced by Botulinum Toxin Treatment in Spasmodic Dysphonia: An H[subscript 2][superscript 15]O PET Study

    Science.gov (United States)

    Ali, S. Omar; Thomassen, Michael; Schulz, Geralyn M.; Hosey, Lara A.; Varga, Mary; Ludlow, Christy L.; Braun, Allen R.

    2006-01-01

    Speech-related changes in regional cerebral blood flow (rCBF) were measured using H[subscript 2][superscript 15]O positron-emission tomography in 9 adults with adductor spasmodic dysphonia (ADSD) before and after botulinum toxin (BTX) injection and 10 age- and gender-matched volunteers without neurological disorders. Scans were acquired at rest…

  7. The Influence of Tier One of RtI[superscript 2] and Instructional Coaching on Teacher Instruction and Student/ELL Learning: A Multiple Case Study

    Science.gov (United States)

    Valadez, Frances E.

    2012-01-01

    The purpose of this case study was to demonstrate the influence of Tier 1 of Response to Intervention and Instruction (RtI[superscript 2]) and instructional coaching on teachers' instruction and on students' and English Language Learners' (ELL) learning. Research was conducted in one large urban elementary school. The unit of study…

  8. What Does f[subscript xx]f[subscript yy] - f[superscript 2][subscript xy] Greater than 0 "Really" Mean?

    Science.gov (United States)

    McCartin, Brian J.

    2008-01-01

    This note presents geometric and physical interpretations of the sufficient condition for a critical point to be a strict relative extremum: f[subscript xx]f[subscript yy] - f[superscript 2][subscript xy] greater than 0. The role of the double derivative f[subscript xy] in this inequality will be highlighted in these interpretations. (Contains 14…

  9. Catechol-O-Methyltransferase "Val[superscript 158]Met" Genotype, Parenting Practices and Adolescent Alcohol Use: Testing the Differential Susceptibility Hypothesis

    Science.gov (United States)

    Laucht, Manfred; Blomeyer, Dorothea; Buchmann, Arlette F.; Treutlein, Jens; Schmidt, Martin H.; Esser, Gunter; Jennen-Steinmetz, Christine; Rietschel, Marcella; Zimmermann, Ulrich S.; Banaschewski, Tobias

    2012-01-01

    Background: Recently, first evidence has been reported for a gene-parenting interaction (G x E) with regard to adolescent alcohol use. The present investigation set out to extend this research using the catechol-O-methyltransferase ("COMT") "Val[superscript 158]Met" polymorphism as a genetic susceptibility factor. Moreover, the current study…

  10. What Does f[subscript xx]f[subscript yy] - f[superscript 2][subscript xy] Greater than 0 "Really" Mean?

    Science.gov (United States)

    McCartin, Brian J.

    2008-01-01

    This note presents geometric and physical interpretations of the sufficient condition for a critical point to be a strict relative extremum: f[subscript xx]f[subscript yy] - f[superscript 2][subscript xy] greater than 0. The role of the double derivative f[subscript xy] in this inequality will be highlighted in these interpretations. (Contains 14…

  11. Determining the Transference Number of H[superscript +](aq) by a Modified Moving Boundary Method: A Directed Study for the Undergraduate Physical Chemistry Laboratory

    Science.gov (United States)

    Dabke, Rajeev B.; Gebeyehu, Zewdu; Padelford, Jonathan

    2012-01-01

    A directed study for the undergraduate physical chemistry laboratory for determining the transference number of H[superscript +](aq) using a modified moving boundary method is presented. The laboratory study combines Faraday's laws of electrolysis with mole ratios and the perfect gas equation. The volume of hydrogen gas produced at the cathode is…

  12. PR[superscript 2]EPS: Preparation, Recruitment, Retention and Excellence in the Physical Sciences, Including Engineering. A Report on the 2004, 2005 and 2006 Science Summer Camps

    Science.gov (United States)

    Bachman, Nancy J.; Bischoff, Paul J.; Gallagher, Hugh; Labroo, Sunil; Schaumloffel, John C.

    2008-01-01

    Now in its fourth year, PR[superscript 2]EPS is a National Science Foundation funded initiative designed to recruit high school students to attend college majoring in the physical sciences, including engineering and secondary science education, and to help ensure their retention within the program until graduation. A central feature of the…

  13. Gray Matter Volume in Adolescent Anxiety: An Impact of the Brain-Derived Neurotrophic Factor Val[superscript 66]Met Polymorphism?

    Science.gov (United States)

    Mueller, Sven C.; Aouidad, Aveline; Gorodetsky, Elena; Goldman, David; Pine, Daniel S.; Ernst, Monique

    2013-01-01

    Objective: Minimal research links anxiety disorders in adolescents to regional gray matter volume (GMV) abnormalities and their modulation by genetic factors. Prior research suggests that a brain-derived neurotrophic factor (BNDF) Val[superscript 66]Met polymorphism may modulate such brain morphometry profiles. Method: Using voxel-based…

  14. Gray Matter Volume in Adolescent Anxiety: An Impact of the Brain-Derived Neurotrophic Factor Val[superscript 66]Met Polymorphism?

    Science.gov (United States)

    Mueller, Sven C.; Aouidad, Aveline; Gorodetsky, Elena; Goldman, David; Pine, Daniel S.; Ernst, Monique

    2013-01-01

    Objective: Minimal research links anxiety disorders in adolescents to regional gray matter volume (GMV) abnormalities and their modulation by genetic factors. Prior research suggests that a brain-derived neurotrophic factor (BNDF) Val[superscript 66]Met polymorphism may modulate such brain morphometry profiles. Method: Using voxel-based…

  15. Utilizing Organizational Culture to Predict Responses to Planned Change in a Public School: A Test of the OC[superscript 3] Model

    Science.gov (United States)

    Sandberg, Eric Christian

    2012-01-01

    The primary purpose of this research was to test the capability of the Organizational Change in Cultural Context (OC[superscript 3]) Model (Latta, 2009, 2011) to predict responses to change. According to Latta, predictions of resistance to or facilitation of change can be predicted by utilizing organizational culture and its alignment with the…

  16. Quantitative analysis of norfloxacin by 1H NMR and HPLC.

    Science.gov (United States)

    Frackowiak, Anita; Kokot, Zenon J

    2012-01-01

    1H NMR and developed previously HPLC methods were applied to quantitative determination of norfloxacin in veterinary solution form for pigeon. Changes in concentration can lead to significant changes in the 1H chemical shifts of non-exchangeable aromatic protons as a result of extensive self-association phenomena. This chemical shift variation of protons was analyzed and applied in the quantitative determination of norfloxacin. The method is simple, rapid, precise and accurate, and can be used for quality control of this drug.

  17. Metabolite Characterization in Peritoneal Dialysis Effluent Using High-resolution 1H and 1H-13C NMR Spectroscopy

    CERN Document Server

    Guleria, Anupam; Rawat, Atul; Khetrapal, C L; Prasad, Narayan; Kumar, Dinesh

    2014-01-01

    Metabolite analysis of peritoneal dialysis (PD) effluent may provide information regarding onset and progression of complications associated with prolonged PD therapy. In this context, the NMR detectable small metabolites of PD effluent samples were characterized using high resolution 1H and 1H-13C NMR spectroscopy. The various spectra were recorded (at 800 MHz proton frequency) on PD effluent samples obtained after 4 hour (intraperitoneal) dwell time from patients with end stage renal failure (ESRF) and continuing normally on PD therapy. Inspite of devastating spectral feature of PD effluent due to the presence of intense resonances from glucose and lactate, we were able to identify about 53 small endogenous metabolites (including many complex coupled spin systems) and more than 90 % of the total CH cross peaks of 1H-13C HSQC spectrum were identified specific to various metabolites of PD effluent. We foresee that the characteristic fingerprints of various metabolites of control PD effluent samples will be us...

  18. Nuclear receptor NR1H3 in familial multiple sclerosis

    Science.gov (United States)

    Wang, Zhe; Sadovnick, A. Dessa; Traboulsee, Anthony L.; Ross, Jay P.; Bernales, Cecily Q.; Encarnacion, Mary; Yee, Irene M.; de Lemos, Madonna; Greenwood, Talitha; Lee, Joshua D.; Wright, Galen; Ross, Colin J.; Zhang, Si; Song, Weihong; Vilariño-Güell, Carles

    2016-01-01

    SUMMARY Multiple sclerosis (MS) is an inflammatory disease characterized by myelin loss and neuronal dysfunction. Despite the aggregation observed in some families, pathogenic mutations have remained elusive. In this study we describe the identification of NR1H3 p.Arg415Gln in seven MS patients from two multi-incident families presenting severe and progressive disease, with an average age at onset of 34 years. Additionally, association analysis of common variants in NR1H3 identified rs2279238 conferring a 1.35-fold increased risk of developing progressive MS. The p.Arg415Gln position is highly conserved in orthologs and paralogs, and disrupts NR1H3 heterodimerization and transcriptional activation of target genes. Protein expression analysis revealed that mutant NR1H3 (LXRA) alters gene expression profiles, suggesting a disruption in transcriptional regulation as one of the mechanisms underlying MS pathogenesis. Our study indicates that pharmacological activation of LXRA or its targets may lead to effective treatments for the highly debilitating and currently untreatable progressive phase of MS. PMID:27253448

  19. 1H and 13C NMR study of perdeuterated pyrazoles

    OpenAIRE

    Jimeno, María Luisa; Jagerovic, Nadine; Elguero, José; Junk, Thomas; Catallo, W. James

    1997-01-01

    The 1H and 13C chemical shifts as well as the 1H–2H and 2H–13C coupling constants of perdeuterated 3,5-dimethylpyrazole and 3,5-diphenylpyrazole have been measured and the values compared with those of the unlabelled compounds.

  20. Flavonoid glycosides from Persea caerulea. Unraveling their interactions with SDS-micelles through matrix-assisted DOSY, PGSE, mass spectrometry, and NOESY.

    Science.gov (United States)

    Álvarez, Juan M; Raya-Barón, Álvaro; Nieto, Pedro M; Cuca, Luis E; Carrasco-Pancorbo, Alegría; Fernández-Gutiérrez, Alberto; Fernández, Ignacio

    2016-04-13

    Two flavonoid glycosides derived from rhamnopyranoside (1) and arabinofuranoside (2) have been isolated from leaves of Persea caerulea for the first time. The structures of 1 and 2 have been established by (1) H NMR, (13) C NMR, and IR spectroscopy, together with LC-ESI-TOF and LC-ESI-IT MS spectrometry. From the MS and MS/MS data, the molecular weights of the intact molecules as well as those of quercetin and kaempferol together with their sugar moieties were deduced. The NMR data provided information on the identity of the compounds, as well as the α and β configurations and the position of the glycosides on quercetin and kaempferol. We have also explored the application of sodium dodecyl sulfate (SDS) normal micelles in binary aqueous solution, at a range of concentrations, to the diffusion resolution of these two glycosides, by the application of matrix-assisted diffusion ordered spectroscopy (DOSY) and pulse field gradient spin echo (PGSE) methodologies, showing that SDS micelles offer a significant resolution which can, in part, be rationalized in terms of differing degrees of hydrophobicity, amphiphilicity, and steric effects. In addition, intra-residue and inter-residue proton-proton distances using nuclear Overhauser effect build-up curves were used to elucidate the conformational preferences of these two flavonoid glycosides when interacting with the micelles. By the combination of both diffusion and nuclear Overhauser spectroscopy techniques, the average location site of kaempferol and quercetin glycosides has been postulated, with the former exhibiting a clear insertion into the interior of the SDS-micelle, whereas the latter is placed closer to the surface. Copyright © 2016 John Wiley & Sons, Ltd.

  1. 1H NMR Studies of MgH2

    Science.gov (United States)

    Itoh, Yutaka; Kado, Ryoichi

    We report on 1H NMR studies of commercially available powder MgH2 exposed to air and maybe humidity, which has been believed to be a promising material for hydrogen storage. The Fourier transform of the free-induction decay of the protons indicatesd superposition of broad and narrow components in the NMR spectrum, while the Fourier transform of the 1H nuclear spin-echo reproduced the narrow component. With cooling down below room temperature, the ratio of the narrow peak to the broad spectrum decreased. The broad spectrum is associated with direct dipolar coupled protons on an inhomogeneous rigid lattice. The narrow peak is associated with interstitial protons with more inhomogeneous surroundings.

  2. 5-Pentyl-4-phenylsulfonyl-1H-pyrazol-3-ol

    Directory of Open Access Journals (Sweden)

    Tara Shahani

    2010-06-01

    Full Text Available In the title compound, C14H18N2O3S, the 1H-pyrazole ring is approximately planar, with a maximum deviation of 0.005 (1 Å. The dihedral angle formed between the 1H-pyrazole and phenyl rings is 79.09 (5°. Pairs of intermolecular N—H...O and O...H...N hydrogen bonds form dimers between neighboring molecules, generating R22(10 ring motifs. These dimers are further linked byintermolecular N—H...O and O—H...N hydrogen bonds into a two-dimensional array parallel to the ac plane. The crystal structure is also stabilized by C—H...π interactions.

  3. Therapeutic potential of CAMPATH-1H in skeletal tumours

    OpenAIRE

    Fritsche, Raphaela; Grützkau, Andreas; Noske, Aurelia; Melcher, Ingo; Schaser, Klaus-Dieter; Schlag, Peter M.; Kasper, Hans U; Krenn, Veit Jonas; Sers, Christine

    2010-01-01

    Abstract Aim: CD52 is a GPI-anchored glycoprotein that is expressed abundantly on all lymphocytes, monocytes, macrophages, eosinophils and in the male genital tract. To date, the physiological role of CD52 on lymphocytes has not been elucidated. However, an antibody directed to CD52 called CAMPATH-1H has been shown to be capable of depleting lymphocytes. Tissue and cell lines of non-neoplastic bone, cartilage and skeletal tumours were analysed for CD52 expression. Methods and resul...

  4. 7-Iodo-1H-indole-3-carbonitrile

    Directory of Open Access Journals (Sweden)

    Rosanna Meine

    2015-10-01

    Full Text Available The title compound was prepared by a Friedel–Crafts acylation-oxime synthesis-decarboxylation/dehydration sequence starting from commercially available 7-iodoindole with 2-(7-iodo-1H-indol-3-yl-2-oxoacetic acid as isolated intermediate. The structural identity of the title compound was proven by elemental analysis and spectroscopic methods (IR, NMR, EI-MS, and purity was assessed by two independent HPLC methods.

  5. 1-Propyl-1H-indole-2,3-dione

    Directory of Open Access Journals (Sweden)

    Fatima Zahrae Qachchachi

    2016-04-01

    Full Text Available In the title compound, C11H11NO2, the 1H-indole-2,3-dione unit is essentially planar, with an r.m.s. deviation of 0.0387 (13 Å. This plane makes a dihedral angle of 72.19 (17° with the plane of the propyl substituent. In the crystal, chains propagating along the b axis are formed through C—H...O hydrogen bonds.

  6. Quantitative produced water analysis using mobile 1H NMR

    Science.gov (United States)

    Wagner, Lisabeth; Kalli, Chris; Fridjonsson, Einar O.; May, Eric F.; Stanwix, Paul L.; Graham, Brendan F.; Carroll, Matthew R. J.; Johns, Michael L.

    2016-10-01

    Measurement of oil contamination of produced water is required in the oil and gas industry to the (ppm) level prior to discharge in order to meet typical environmental legislative requirements. Here we present the use of compact, mobile 1H nuclear magnetic resonance (NMR) spectroscopy, in combination with solid phase extraction (SPE), to meet this metrology need. The NMR hardware employed featured a sufficiently homogeneous magnetic field, such that chemical shift differences could be used to unambiguously differentiate, and hence quantitatively detect, the required oil and solvent NMR signals. A solvent system consisting of 1% v/v chloroform in tetrachloroethylene was deployed, this provided a comparable 1H NMR signal intensity for the oil and the solvent (chloroform) and hence an internal reference 1H signal from the chloroform resulting in the measurement being effectively self-calibrating. The measurement process was applied to water contaminated with hexane or crude oil over the range 1-30 ppm. The results were validated against known solubility limits as well as infrared analysis and gas chromatography.

  7. Bis{μ-1-[(2-ethyl-1H-imidazol-1-ylmethyl]-1H-benzotriazole}bis(iodidocadmium

    Directory of Open Access Journals (Sweden)

    Xia Wang

    2011-07-01

    Full Text Available The dinuclear title complex, [Cd2I4(C12H13N52], lies on a crystallographic center of inversion. The CdII atom is four-coordinated by two N atoms from two 1-[(2-ethyl-1H-imidazol-1-ylmethyl]-1H-benzotriazole (bmei ligands and two terminal I atoms in a distorted tetrahedral coordination environment. The CdII atoms are connected to each other by two bridging bmei ligands. The benzotriazole rings in adjacent molecules are almost parallel, with an average interplanar distance of 3.3400 (2 Å and a centroid–centroid distance of 4.852 (2 Å.

  8. Complete assignment of NMR data of 22 phenyl-1H-pyrazoles' derivatives.

    Science.gov (United States)

    de Oliveira, Aline Lima; Alves de Oliveira, Carlos Henrique; Mairink, Laura Maia; Pazini, Francine; Menegatti, Ricardo; Lião, Luciano Morais

    2011-08-01

    Complete assignment of (1)H and (13)C NMR chemical shifts and J((1)H/(1)H and (1)H/(19)F) coupling constants for 22 1-phenyl-1H-pyrazoles' derivates were performed using the concerted application of (1)H 1D and (1)H, (13)C 2D gs-HSQC and gs-HMBC experiments. All 1-phenyl-1H-pyrazoles' derivatives were synthesized as described by Finar and co-workers. The formylated 1-phenyl-1H-pyrazoles' derivatives were performed under Duff's conditions.

  9. 2-Methyl-1H-benzimidazol-3-ium hydrogen phthalate

    Directory of Open Access Journals (Sweden)

    YuanQi Yu

    2011-10-01

    Full Text Available The asymmetric unit of the title compound, C8H9N2+·C8H5O4−, contains two independent ion pairs. In each 2-methyl-1H-benzimidazolium ion, an intramolecular O—H...O bond forms an S(7 graph-set motif. In the crystal, the components are linked by N—H...O hydrogen bonds, forming chains along [210]. Further stabilization is provided by weak C—H...O hydrogen bonds.

  10. Decaying Neutralino Dark Matter in Anomalous $U(1)_H$ Models

    CERN Document Server

    Sierra, D Aristizabal; Zapata, Oscar

    2009-01-01

    In supersymmetric models extended with an anomalous $U(1)_H$ different R-parity violating couplings can yield an unstable neutralino. We show that in this context astrophysical and cosmological constraints on neutralino decaying dark matter forbid bilinear R-parity breaking neutralino decays and lead to a class of purely trilinear R-parity violating scenarios in which the neutralino is stable on cosmological scales. We have found that among the resulting models some of them become suitable to explain the observed anomalies in cosmic-ray electron/positron fluxes.

  11. Profiling formulated monoclonal antibodies by (1)H NMR spectroscopy.

    Science.gov (United States)

    Poppe, Leszek; Jordan, John B; Lawson, Ken; Jerums, Matthew; Apostol, Izydor; Schnier, Paul D

    2013-10-15

    Nuclear magnetic resonance (NMR) is arguably the most direct methodology for characterizing the higher-order structure of proteins in solution. Structural characterization of proteins by NMR typically utilizes heteronuclear experiments. However, for formulated monoclonal antibody (mAb) therapeutics, the use of these approaches is not currently tenable due to the requirements of isotope labeling, the large size of the proteins, and the restraints imposed by various formulations. Here, we present a new strategy to characterize formulated mAbs using (1)H NMR. This method, based on the pulsed field gradient stimulated echo (PGSTE) experiment, facilitates the use of (1)H NMR to generate highly resolved spectra of intact mAbs in their formulation buffers. This method of data acquisition, along with postacquisition signal processing, allows the generation of structural and hydrodynamic profiles of antibodies. We demonstrate how variation of the PGSTE pulse sequence parameters allows proton relaxation rates and relative diffusion coefficients to be obtained in a simple fashion. This new methodology can be used as a robust way to compare and characterize mAb therapeutics.

  12. 23Na and 1H NMR Microimaging of Intact Plants

    Science.gov (United States)

    Olt, Silvia; Krötz, Eva; Komor, Ewald; Rokitta, Markus; Haase, Axel

    2000-06-01

    23Na NMR microimaging is described to map, for the first time, the sodium distribution in living plants. As an example, the response of 6-day-old seedlings of Ricinus communis to exposure to sodium chloride concentrations from 5 to 300 mM was observed in vivo using 23Na as well as 1H NMR microimaging. Experiments were performed at 11.75 T with a double resonant 23Na-1H probehead. The probehead was homebuilt and equipped with a climate chamber. T1 and T2 of 23Na were measured in the cross section of the hypocotyl. Within 85 min 23Na images with an in-plane resolution of 156 × 156 μm were acquired. With this spatial information, the different types of tissue in the hypocotyl can be discerned. The measurement time appears to be short compared to the time scale of sodium uptake and accumulation in the plant so that the kinetics of salt stress can be followed. In conclusion, 23Na NMR microimaging promises great potential for physiological studies of the consequences of salt stress on the macroscopic level and thus may become a unique tool for characterizing plants with respect to salt tolerance and salt sensitivity.

  13. Metabolomic insight into soy sauce through (1)H NMR spectroscopy.

    Science.gov (United States)

    Ko, Bong-Kuk; Ahn, Hyuk-Jin; van den Berg, Frans; Lee, Cherl-Ho; Hong, Young-Shick

    2009-08-12

    Soy sauce, a well-known seasoning in Asia and throughout the world, consists of many metabolites that are produced during fermentation or aging and that have various health benefits. However, their comprehensive assessment has been limited due to targeted or instrumentally specific analysis. This paper presents for the first time a metabolic characterization of soy sauce, especially that aged up to 12 years, to obtain a global understanding of the metabolic variations through (1)H NMR spectroscopy coupled with multivariate pattern recognition techniques. Elevated amino acids and organic acids and the consumption of carbohydrate were associated with continuous involvement of microflora in aging for 12 years. In particular, continuous increases in the levels of betaine were found during aging for up to 12 years, demonstrating that microbial- or enzyme-related metabolites were also coupled with osmotolerant or halophilic bacteria present during aging. This work provides global insights into soy sauce through a (1)H NMR-based metabolomic approach that enhances the current understanding of the holistic metabolome and allows assessment of soy sauce quality.

  14. Genetic Variation in Myosin 1H Contributes to Mandibular Prognathism

    Science.gov (United States)

    Tassopoulou-Fishell, Maria; Deeley, Kathleen; Harvey, Erika M.; Sciote, James; Vieira, Alexandre R.

    2013-01-01

    Introduction Several candidate loci have been suggested as influencing mandibular prognathism (1p22.1, 1p22.2, 1p36, 3q26.2, 5p13-p12, 6q25, 11q22.2-q22.3, 12q23, 12q13.13, and 19p13.2). The goal of this study was to replicate these results in a well-characterized homogeneous sample set. Methods Thirty-three single nucleotide polymorphisms spanning all candidate regions were studied in 44 prognathic and 35 Class I subjects from the University of Pittsburgh School of Dental Medicine Dental Registry and DNA Repository. The 44 mandibular prognathism subjects had an average age of 18.4 years, 31 were females and 13 males, and 24 were White, 15 African American, two Hispanic, and three Asian. The 35 Class I subjects had an average age of 17.6 years, 27 were females and 9 males, and 27 were White, six African Americans, one Hispanic, and two Asian. Skeletal mandibular prognathism diagnosis included cephalometric values indicative of Class III such as ANB smaller than two degrees, negative Witts appraisal, and positive A–B plane. Additional mandibular prognathism criteria included negative OJ and visually prognathic (concave) profile as determined by the subject's clinical evaluation. Orthognathic subjects without jaw deformations were used as a comparison group. Mandibular prognathism and orthognathic subjects were matched based on race, sex and age. Genetic markers were tested by polymerase chain reaction using TaqMan chemistry. Chi-square and Fisher exact tests were used to determine overrepresentation of marker allele with alpha of 0.05. Results An association was unveiled between a marker in MYO1H (rs10850110) and the mandibular prognathism phenotype (p=0.03). MYO1H is a Class-I myosin that is in a different protein group than the myosin isoforms of muscle sarcomeres, which are the basis of skeletal muscle fiber typing. Class I myosins are necessary for cell motility, phagocytosis and vesicle transport. Conclusions More strict clinical definitions may increase

  15. Crystal structure of 1H,1'H-[2,2'-biimid-azol]-3-ium hydrogen tartrate hemi-hydrate.

    Science.gov (United States)

    Gao, Xiao-Li; Bian, Li-Fang; Guo, Shao-Wei

    2014-11-01

    In the crystal of the title hydrated salt, C6H7N4 (+)·C4H5O6 (-)·0.5H2O, the bi-imidazole monocation, 1H,1'H-[2,2'-biimidazol]-3-ium, is hydrogen bonded, via N-H⋯O, O-H⋯O and O-H⋯N hydrogen bonds, to the hydrogen tartrate anion and the water mol-ecule, which is located on a twofold rotation axis, forming sheets parallel to (001). The sheets are linked via C-H⋯O hydrogen bonds, forming a three-dimensional structure. There are also C=O⋯π inter-actions present [O⋯π distances are 3.00 (9) and 3.21 (7) Å], involving the carbonyl O atoms and the imidazolium ring, which may help to consolidate the structure. In the cation, the dihedral angle between the rings is 11.6 (2)°.

  16. 4-Methyl-5-phenyl-1H-pyrazol-3-ol

    Directory of Open Access Journals (Sweden)

    Tara Shahani

    2010-07-01

    Full Text Available The title compound, C10H10N2O, crystallizes with two independent molecules in the asymmetric unit, having closely comparable geometries. The dihedral angles between the 1H-pyrazole and benzene rings in the two molecules are 39.57 (14 and 41.95 (13°. The two molecules are each connected to neighbouring molecules by pairs of intermolecular O—H...N hydrogen bonds, forming dimers with R22(8 ring motifs. These dimers are further linked into R44(10 ring motifs by intermolecular N—H...O hydrogen bonds, forming chains along [101]. The crystal structure is further stabilized by a C—H...π interaction.

  17. 海南捕鸟蛛毒素-Ⅰ(HNTX-Ⅰ)的1H-NMR信号归属和二级结构分析%SEQUENCE-SPECIFIC ASSIGNMENT OF 1H-NMR RESONANCE AND DETERMINATION OF THE SECONDARY STRUCTURE OF HAINANTOXIN-Ⅰ

    Institute of Scientific and Technical Information of China (English)

    李冬玲; 梁宋平

    2003-01-01

    Hainantoxin-Ⅰ(HNTX-Ⅰ ) is an insect blocker of voltage-gated sodium channel isolated from the venom of the Chinese bird spider Ornithoctonus hainana (early named Selenocosmia hainana). The three-dimensional conformation of HNTX- Ⅰ in aqueous solution was determined using two-dimensional 1H NMR techniques. The complete sequence-specific assignments of proton resonance in the 1H-NMR spectra of HNTX-Ⅰ were obtained by analyzing a series of 2D spectra, including double-quantum-filtered correlation spectroscopy (DQF-COSY), total correlated spectroscopy (TOCSY) and nuclear overhauser effect spectroscopy (NOESY) in H2O and D2O. All the backbone protons and more than 96% of the side-chain protons were identified by dαN, dαN, dNN and dαδ connectivities in NOESY spectrum. Furthermore, it was found that the main element of the secondary structure of HNTX-Ⅰ is a short triple-stranded antiparallel β-sheet with Lys7-Cys9, Tyr20-Asn23 and Trp28-Val31, based on 3JNH-CαH coupling constants, sequential NOE connectivities and slowly exchanging amide protons. These characters of the secondary structure of HNTX-Ⅰ are similar to those of HWTX-Ⅰ, SHL-Ⅰ and HWTX-Ⅳ, which have known solution structures. These results provide a basis for the further determination of the solution conformation of HNTX-Ⅰ.%海南捕鸟蛛毒素-Ⅰ(HNTX-Ⅰ)是从海南捕鸟蛛(Ornithoctonus hainana)的粗毒中纯化的一种新型神经毒素.应用二维1H-NMR技术研究HNTX-Ⅰ的溶液结构特点,通过分析水和重水中的DQF-COSY、TOCSY和NOESY谱,识别出HNTX-Ⅰ全部33个氨基酸残基自旋体系;通过NOESY谱中的dαN、dβN、dNN和dαδ联系完成了序列专一的谱峰归属,从而确认了HNTX-Ⅰ所有的主链质子和大于96%的侧链质子的化学位移.并通过分析3JNH-CαH耦合常数、序列间的NOE联系以及慢氢交换质子等,确定HNTX-Ⅰ的二级结构主要是由三股反平行的β-折迭组成(Lys7-Cys9,Tyr20-Asn23和Trp28-Val31),

  18. The Conformations and Structures of 1H-NONAFLUOROBUTANE

    Science.gov (United States)

    Fournier, Joseph A.; Bohn, Robert K.; Montgomery, John A.; , Jr.

    2012-06-01

    The all trans conformers of perfluorocarbons, unlike hydrocarbons, are helical with C-C-C-C dihedral angles about 1640. Fluorocarbons with H substitution can replace chlorofluorocarbons as propellants and compressor fluids without the disadvantage of causing ozone depletion in the upper atmosphere. 1H-perfluorobutane, CHF_2CF_2CF_2CF_3, has been studied by pulsed-jet Fourier transform microwave spectroscopy. The spectrum is very rich. Quantum chemical calculations identify five stable conformers with relative energies up to 1.1 kcal/mol. Thus far three conformers have been characterized and many lines remain unassigned. The assigned species have CCCCanti/CCCH gauche as well as the anti/anti and gauche/anti forms. Rotational constant values are 1428.9501(2) MHz, 593.323877(6) MHz, and 546.43578(6) MHz for the anti/gauche species, 1323.664(3) MHz, 617.6051(5) MHz for the ant/anti species, and 1066.9384(4) MHz, 768.4736(4) MHz, and 671.3145(4) MHz for the gauche/anti form.

  19. Tacrine derivatives-acetylcholinesterase interaction: 1H NMR relaxation study.

    Science.gov (United States)

    Delfini, Maurizio; Di Cocco, Maria Enrica; Piccioni, Fabiana; Porcelli, Fernando; Borioni, Anna; Rodomonte, Andrea; Del Giudice, Maria Rosaria

    2007-06-01

    Two acetylcholinesterase (AChE) inhibitors structurally related to Tacrine, 6-methoxytacrine (1a) and 9-heptylamino-6-methoxytacrine (1b), and their interaction with Electrophorus Electricus AChE were investigated. The complete assignment of the 1H and 13C NMR spectra of 1a and 1b was performed by mono-dimensional and homo- and hetero-correlated two-dimensional NMR experiments. This study was undertaken to elucidate the interaction modes between AChE and 1a and 1b in solution, using NMR. The interaction between the two inhibitors and AChE was studied by the analysis of the motional parameters non-selective and selective spin-lattice relaxation times, thereby allowing the motional state of 1a and 1b, both free and bound with AChE, to be defined. The relaxation data pointed out the ligands molecular moiety most involved in the binding with AChE. The relevant ligand/enzyme interaction constants were also evaluated for both compounds and resulted to be 859 and 5412M(-1) for 1a and1b, respectively.

  20. Mapping of prostate cancer by 1H MRSI.

    Science.gov (United States)

    Kobus, Thiele; Wright, Alan J; Scheenen, Tom W J; Heerschap, Arend

    2014-01-01

    In many studies, it has been demonstrated that (1)H MRSI of the human prostate has great potential to aid prostate cancer management, e.g. in the detection and localisation of cancer foci in the prostate or in the assessment of its aggressiveness. It is particularly powerful in combination with T2 -weighted MRI. Nevertheless, the technique is currently mainly used in a research setting. This review provides an overview of the state-of-the-art of three-dimensional MRSI, including the specific hardware required, dedicated data acquisition sequences and information on the spectral content with background on the MR-visible metabolites. In clinical practice, it is important that relevant MRSI results become available rapidly, reliably and in an easy digestible way. However, this functionality is currently not fully available for prostate MRSI, which is a major obstacle for routine use by inexperienced clinicians. Routine use requires more automation in the processing of raw data than is currently available. Therefore, we pay specific attention in this review on the status and prospects of the automated handling of prostate MRSI data, including quality control. The clinical potential of three-dimensional MRSI of the prostate is illustrated with literature examples on prostate cancer detection, its localisation in the prostate, its role in the assessment of cancer aggressiveness and in the selection and monitoring of therapy.

  1. Understanding Reverberation Lags in 1H0707-495

    CERN Document Server

    Zoghbi, A; Fabian, A C

    2010-01-01

    The first reverberation lag from the vicinity of a supermassive black hole was recently detected in the NLS1 galaxy 1H0707-495. We interpreted the lag as being due to reflection from matter close to the black hole, within a few gravitational radii of the event horizon (an inner reflector). It has since been claimed by Miller et al that the lag can be produced by more distant matter, at hundreds of gravitational radii (an outer reflector). Here, we critically explore their interpretation of the lag. The detailed energy dependence of the time lags between soft and hard energy bands is well modelled by an inner reflector using our previously published spectral model. A contrary claim by Miller et al was obtained by neglecting the blackbody component in the soft band. Soft lags can be produced by a large-scale outer reflector if several, implausible, conditions are met. An additional transfer function is required in the soft band corresponding to a region that is physically close to the continuum source, or lies ...

  2. 1H MAS and 1H --> 31P CP/MAS NMR study of human bone mineral.

    Science.gov (United States)

    Kaflak-Hachulska, A; Samoson, A; Kolodziejski, W

    2003-11-01

    Chemical structure of human bone mineral was studied by solid-state nuclear magnetic resonance (NMR) with magic-angle spinning (MAS). Trabecular and cortical bone samples from adult subjects were compared with mineral standards: hydroxyapatite (HA), hydrated and calcined, carbonatoapatite of type B with 9 wt% of CO3(2-) (CHA-B), brushite (BRU) and mixtures of HA with BRU. Proton spectra were acquired with excellent spectral resolution provided by ultra-high speed MAS at 40 kHz. 2D 1H-31P NMR heteronuclear correlation was achieved by cross-polarization (CP) under fast MAS at 12 kHz. 31P NMR was applied with CP from protons under slow MAS at 1 kHz. Appearance of 31P rotational sidebands together with their CP kinetics were analyzed. It was suggested that the sidebands of CP spectra are particularly suitable for monitoring the state of apatite crystal surfaces. The bone samples appeared to be deficient in structural hydroxyl groups analogous to those in HA. We found no direct evidence that the HPO4(2-) brushite-like ions are present in bone mineral. The latter problem is extensively discussed in the literature. The study proves there is a similarity between CHA-B and bone mineral expressed by their similar NMR behavior.

  3. Measurement of {sup 1}H-{sup 15}N and {sup 1}H-{sup 13}C residual dipolar couplings in nucleic acids from TROSY intensities

    Energy Technology Data Exchange (ETDEWEB)

    Ying Jinfa [National Institutes of Health, Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases (United States); Wang Jinbu [National Cancer Institute, National Institutes of Health, Structural Biophysics Laboratory (United States); Grishaev, Alex [National Institutes of Health, Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases (United States); Yu Ping; Wang Yunxing [National Cancer Institute, National Institutes of Health, Structural Biophysics Laboratory (United States); Bax, Ad, E-mail: bax@nih.gov [National Institutes of Health, Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases (United States)

    2011-09-15

    Analogous to the recently introduced ARTSY method for measurement of one-bond {sup 1}H-{sup 15}N residual dipolar couplings (RDCs) in large perdeuterated proteins, we introduce methods for measurement of base {sup 13}C-{sup 1}H and {sup 15}N-{sup 1}H RDCs in protonated nucleic acids. Measurements are based on quantitative analysis of intensities in {sup 1}H-{sup 15}N and {sup 13}C-{sup 1}H TROSY-HSQC spectra, and are illustrated for a 71-nucleotide adenine riboswitch. Results compare favorably with those of conventional frequency-based measurements in terms of completeness and convenience of use. The ARTSY method derives the size of the coupling from the ratio of intensities observed in two TROSY-HSQC spectra recorded with different dephasing delays, thereby minimizing potential resonance overlap problems. Precision of the RDC measurements is limited by the signal-to-noise ratio, S/N, achievable in the 2D TROSY-HSQC reference spectrum, and is approximately given by 30/(S/N) Hz for {sup 15}N-{sup 1}H and 65/(S/N) Hz for {sup 13}C-{sup 1}H. The signal-to-noise ratio of both {sup 1}H-{sup 15}N and {sup 1}H-{sup 13}C spectra greatly benefits when water magnetization during the experiments is not perturbed, such that rapid magnetization transfer from bulk water to the nucleic acid, mediated by rapid amino and hydroxyl hydrogen exchange coupled with {sup 1}H-{sup 1}H NOE transfer, allows for fast repetition of the experiment. RDCs in the mutated helix 1 of the riboswitch are compatible with nucleotide-specifically modeled, idealized A-form geometry and a static orientation relative to the helix 2/3 pair, which differs by ca 6 Degree-Sign relative to the X-ray structure of the native riboswitch.

  4. Synthesis of 1H-indazoles and 1H-pyrazoles via FeBr3/O2 mediated intramolecular C-H amination.

    Science.gov (United States)

    Zhang, Tianshui; Bao, Weiliang

    2013-02-01

    A new synthesis of substituted 1H-indazoles and 1H-pyrazoles from arylhydrazones via FeBr(3)/O(2) mediated C-H activation/C-N bond formation reactions is reported. The corresponding 1,3-diaryl-substituted indazoles and trisubstituted pyrazoles were obtained in moderate to excellent yields under mild conditions.

  5. Synthesis and Characterization of Novel 1H-Indazole Derivatives%1H-吲唑类中间体的合成及表征

    Institute of Scientific and Technical Information of China (English)

    周淑晶; 李长胜; 关文碧; 武晓丽; 刘雪; 马永强

    2013-01-01

    以取代邻甲苯胺为原料经乙酰化、溴化、环合及胺解反应得到1H-吲唑类化合物,再与酸酐、碘乙烷或硝酸反应以较高收率合成了15个1H-吲唑衍生物,其中12个未见文献报道.其结构经1H NMR、IR表征确认.

  6. Weight Management Guides for Pregnant Women with a Body Mass index (BMI) Greater than or Equal to 40kg/m[Superscript 2]: A Qualitative Exploration of Their Use in Maternity Care

    Science.gov (United States)

    Smith, Debbie M.; Ward, Christine; Forbes, Shareen; Reynolds, Rebecca M.; Denison, Fiona C.

    2013-01-01

    Objective: Maternal obesity (Body Mass Index [BMI] greater than or equal to 30kg/m([superscript 2]) is associated with numerous maternal and fetal complications. Recent guidelines have called for advice to be given to women as pregnancy is a good time for intervention as due to women's motivations for change being high and changes may impact on…

  7. Weight Management Guides for Pregnant Women with a Body Mass index (BMI) Greater than or Equal to 40kg/m[Superscript 2]: A Qualitative Exploration of Their Use in Maternity Care

    Science.gov (United States)

    Smith, Debbie M.; Ward, Christine; Forbes, Shareen; Reynolds, Rebecca M.; Denison, Fiona C.

    2013-01-01

    Objective: Maternal obesity (Body Mass Index [BMI] greater than or equal to 30kg/m([superscript 2]) is associated with numerous maternal and fetal complications. Recent guidelines have called for advice to be given to women as pregnancy is a good time for intervention as due to women's motivations for change being high and changes may impact on…

  8. Consecutive C[subscript 60] Fullerene Dissociation from Ir([eta][superscript 2]-C[subscript 60])(CO)(Cl)(PPh[subscript 3])[subscript 2] and the Oxidative Addition of Benzene

    Science.gov (United States)

    Felix, Tamara; Cortes-Figueroa, Jose E.

    2010-01-01

    This laboratory activity is a mechanistic exploration of the interactions between electronically deficient organometallic compounds and solvent molecules. Simple kinetics experiments designed to explore the mechanism of C[subscript 60] fullerene-benzene exchange on Ir(([eta][superscript 2]-C[subscript 60])(CO)(Cl)(PPh[subscript 3])[subscript 2]…

  9. Project h[schwa]li?dx[superscript w]/Healthy Hearts across Generations: Development and Evaluation Design of a Tribally Based Cardiovascular Disease Prevention Intervention for American Indian Families

    Science.gov (United States)

    Walters, Karina L.; LaMarr, June; Levy, Rona L.; Pearson, Cynthia; Maresca, Teresa; Mohammed, Selina A.; Simoni, Jane M.; Evans-Campbell, Teresa; Fredriksen-Goldsen, Karen; Fryberg, Sheryl; Jobe, Jared B.

    2012-01-01

    American Indian and Alaska Native (AIAN) populations are disproportionately at risk for cardiovascular disease (CVD), diabetes, and obesity, compared with the general US population. This article describes the h[schwa]li?dx[superscript w]/Healthy Hearts Across Generations project, an AIAN-run, tribally based randomized controlled trial (January…

  10. Validation of quantitative {sup 1}H NMR method for the analysis of pharmaceutical formulations; Validacao de metodo quantitativo por RMN de {sup 1}H para analises de formulacoes farmaceuticas

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Maiara da S. [Universidade de Sao Paulo (USP), Sao Carlos, SP (Brazil). Instituto de Quimica; Colnago, Luiz Alberto, E-mail: luiz.colnago@embrapa.br [Embrapa Instrumentacao, Sao Carlos, SP (Brazil)

    2013-09-01

    The need for effective and reliable quality control in products from pharmaceutical industries renders the analyses of their active ingredients and constituents of great importance. This study presents the theoretical basis of Superscript-One H NMR for quantitative analyses and an example of the method validation according to Resolution RE N. 899 by the Brazilian National Health Surveillance Agency (ANVISA), in which the compound paracetamol was the active ingredient. All evaluated parameters (selectivity, linearity, accuracy, repeatability and robustness) showed satisfactory results. It was concluded that a single NMR measurement provides structural and quantitative information of active components and excipients in the sample. (author)

  11. Potential and limitations of 2D sup 1 H- sup 1 H spin-exchange CRAMPS experiments to characterize structures of organic solids

    CERN Document Server

    Brus, J; Petrickova, H

    2002-01-01

    A brief overview of our recent results concerning the application of 2D CRAMPS experiments to investigate a wide range of materials is presented. The abilities of the 2D sup 1 H- sup 1 H spin-exchange technique to characterize the structure of organic solids as well as the limitations resulting from segmental mobility and from undesired coherence transfer are discussed. Basic principles of sup 1 H NMR line-narrowing and procedures for analysis of the spin-exchange process are introduced. We focused to the qualitative and quantitative analysis of complex spin-exchange process leading to the determination of domain sizes and morphology in heterogeneous multicomponent systems as well as the characterization of clustering of surface hydroxyl groups in polysiloxane networks. Particular attention is devoted to the determination of the sup 1 H- sup 1 H interatomic distances in the presence of local molecular motion. Finally we discuss limitations of the sup 1 sup 3 C- sup 1 sup 3 C correlation mediated by sup 1 H- s...

  12. Proton-detected 3D (15)N/(1)H/(1)H isotropic/anisotropic/isotropic chemical shift correlation solid-state NMR at 70kHz MAS.

    Science.gov (United States)

    Pandey, Manoj Kumar; Yarava, Jayasubba Reddy; Zhang, Rongchun; Ramamoorthy, Ayyalusamy; Nishiyama, Yusuke

    2016-01-01

    Chemical shift anisotropy (CSA) tensors offer a wealth of information for structural and dynamics studies of a variety of chemical and biological systems. In particular, CSA of amide protons can provide piercing insights into hydrogen-bonding interactions that vary with the backbone conformation of a protein and dynamics. However, the narrow span of amide proton resonances makes it very difficult to measure (1)H CSAs of proteins even by using the recently proposed 2D (1)H/(1)H anisotropic/isotropic chemical shift (CSA/CS) correlation technique. Such difficulties due to overlapping proton resonances can in general be overcome by utilizing the broad span of isotropic chemical shifts of low-gamma nuclei like (15)N. In this context, we demonstrate a proton-detected 3D (15)N/(1)H/(1)H CS/CSA/CS correlation experiment at fast MAS frequency (70kHz) to measure (1)H CSA values of unresolved amide protons of N-acetyl-(15)N-l-valyl-(15)N-l-leucine (NAVL).

  13. Synthesis and anti-TMV activity of novel N-(3-alkyl-1H-pyrazol-4-yl)-3-alkyl-4-substituted- 1H-pyrazole-5-carboxamides

    Institute of Scientific and Technical Information of China (English)

    Da Qiang Zhang; Gao Fei Xu; Zhi Jin Fan; Dao Quan Wang; Xin Ling Yang; De Kai Yuan

    2012-01-01

    In oraer to investigate the biological activity of novel bis-pyrazole compounds,a series of N-(3-alkyl-5-(N-methylcarbamyl)-1H-pyrazol-4-yl)-3-alkyl-4-substituted-1H-pyrazole-5-carboxamides were designed and synthesized with ethyl 3-alkyl-1H-pyrazole-5-carboxylate 1 as starting materials.N-Methyl-3-alkyl-4-amino-1H-pyrazole-5-carboxamides 6 were obtained from 1 via 5 steps.3-Alkyl-4-substitued-1H-pyrazole-5-carboxyl chlorides 4a,4b,11a,11b,11c or 12 were also obtained from 1 via several steps.Target compounds 7a-7g were obtained after the reaction of 6 with the above 1H-pyrazole-5-carboxyl chlorides.Preliminary bioassay showed some compounds possessing good inactivation effect against TMV (tobacco mosaic virus).Compound 7a showed higher activity superior to ningnanmycin at a concentration of 5.0 × 10-4 g/mL and equal acdvity at 1.0 × 10-4 g/nL; 7b and 7c showed equal activity to virazole both at concentrations of 5.0 × 10-4 g/mL and 1.0 × 10-4 g/mL.

  14. Decreased insulin clearance in individuals with elevated 1-h post-load plasma glucose levels.

    Directory of Open Access Journals (Sweden)

    Maria Adelaide Marini

    Full Text Available Reduced insulin clearance has been shown to predict the development of type 2 diabetes. Recently, it has been suggested that plasma glucose concentrations ≥ 8.6 mmol/l (155 mg/dl at 1 h during an oral glucose tolerance test (OGTT can identify individuals at high risk for type 2 diabetes among those who have normal glucose tolerance (NGT 1 h-high. The aim of this study was to examine whether NGT 1 h-high have a decrease in insulin clearance, as compared with NGT individuals with 1-h post-load glucose <8.6 mmol/l (l (155 mg/dl, NGT 1 h-low. To this end, 438 non-diabetic White individuals were subjected to OGTT and euglycemic-hyperinsulinemic clamp to evaluate insulin clearance and insulin sensitivity. As compared with NGT 1 h-low individuals, NGT 1 h-high had significantly higher 1-h and 2-h post-load plasma glucose and 2-h insulin levels as well as higher fasting glucose and insulin levels. NGT 1 h-high exhibited also a significant decrease in both insulin sensitivity (P<0.0001 and insulin clearance (P = 0.006 after adjusting for age, gender, adiposity measures, and insulin sensitivity. The differences in insulin clearance remained significant after adjustment for fasting glucose (P = 0.02 in addition to gender, age, and BMI. In univariate analyses adjusted for gender and age, insulin clearance was inversely correlated with body weight, body mass index, waist, fat mass, 1-h and 2-h post-load glucose levels, fasting, 1-h and 2-h post-load insulin levels, and insulin-stimulated glucose disposal. In conclusion, our data show that NGT 1 h-high have a reduction in insulin clearance as compared with NGT 1 h-low individuals; this suggests that impaired insulin clearance may contribute to sustained fasting and post-meal hyperinsulinemia.

  15. Role of Metallothionein1H in Cisplatin Resistance of Non-Small Cell Lung Cancer Cells

    Institute of Scientific and Technical Information of China (English)

    Xin-fang Hou; Qing-xia Fan; Liu-xing Wang; Shi-xin Lu

    2009-01-01

    Objective: Despite platinum-based adjuvant chemotherapy has improved greatly patients' outcomes, drug resistance poses a major impediment to the successful use of such an effective agent. Metallothioneins(MTs) are known to play putative roles in cancer cell proliferation, apoptosis, differentiation, drug resistance and prognosis. The present studiy was to investigte the role of metallethioein1H(MT1H) in cisplatin resistance of human non-small cell lung cancer(NSCLC) cell lines in vitro or its possible molecular mechanisms. Methods: MT1H mRNA expression in A549 and A549/DDP cells was detected by RT-PCR. A recombinant eukaryotic expression plasmid pcDNA3.1(-)-MT1H was constructed and transfected into A549 cells which express no MT1H. MT1H siRNA was transfected into A549/DDP cells which express MT1H highly. MT1H expression was detected by RT-PCR and Immunoblot. The chemosensitivity to cisplatin was assessed by MTT assay. Apoptosis rate was determined by Tunel and FCM. Bcl-2 and Bax were determined by immunohistochemistry. Results: MT1H mRNA was expressed in A549/DDP but not in A549. After transfection of MT1H, MT1H expression was enhanced and the chemosensitivity to cisplatin was decreased in A549 cells. Inversely, after transfection of MT1H siRNA, MT1H expression was decreased and the chemosensitivity to cisplatin was increased in A549/DDP. The apoptosis rate induced by cisplatin was increased and Bcl-2 was down-regulated but Bax showed little change in A549/DDP cells interferred with MT1H siRNA. Conclusion: MT1H overexpression can promote drug resistance in A549 cells . Down-regulation of MT1H interfered with siRNA can effectively reverses the drug resistance in A549/DDP cells by down-regulating the expression of Bcl-2 and increasing cisplatin induced apoptosis. SiRNA targeting MT1H combined with chemotherapy may be a very promising strategy for treatment of lung cancer.

  16. [Study on derivatives of 5-amino-4-acylamino-1H-pyrazole as inhibitors of furin].

    Science.gov (United States)

    Kibirev, V K; Osadchuk, T V; Vadziuk, O B; Shablykin, O V; Kozachenko, A P; Chumachenko, S A; Popil'nichenko, S V; Brovarets, V S

    2011-01-01

    A series of 5-amino-1H-pyrazoles was synthesized and studied as inhibitors of furin. The most potent compound, 5-amino-4-acetylamino-3-(4-methylphenylamino)1H-pyrazole, was found to retard the activity of furin by mixed-type inhibition with K = 288 microM. These findings permit to plan new ways for chemical modifications of the 5-amino-1H-pyrazole structure and design more potent furin inhibitors of non-peptide nature.

  17. Improved synthesis of 1H-indazole-3-carboxylic acid%1H-吲唑-3-羧酸的合成工艺改进

    Institute of Scientific and Technical Information of China (English)

    张东峰; 王燕; 林紫云; 黄海洪; 饶尔昌

    2006-01-01

    目的 改进1H-吲唑-3-羧酸的合成工艺.方法 以苯甲醛苯腙与草酰氯为原料得到N-亚苄基氨基-N-苯基-草氨酰氯,后者与三氯化铝反应得到关键中间体N-亚苄基氨基靛红,再经水解得到1H-吲唑-3-羧酸.结果与结论 该方法以55.3%的收率简单方便地制备了1H-吲唑-3-羧酸,所用起始原料及试剂的成本低、反应条件温和、易于操作,适合工业化生产.

  18. Vicinal 1H-1H NMR coupling constants from density functional theory as reliable tools for stereochemical analysis of highly flexible multichiral center molecules.

    Science.gov (United States)

    López-Vallejo, Fabian; Fragoso-Serrano, Mabel; Suárez-Ortiz, Gloria Alejandra; Hernández-Rojas, Adriana C; Cerda-García-Rojas, Carlos M; Pereda-Miranda, Rogelio

    2011-08-05

    A protocol for stereochemical analysis, based on the systematic comparison between theoretical and experimental vicinal (1)H-(1)H NMR coupling constants, was developed and applied to a series of flexible compounds (1-8) derived from the 6-heptenyl-5,6-dihydro-2H-pyran-2-one framework. The method included a broad conformational search, followed by geometry optimization at the DFT B3LYP/DGDZVP level, calculation of the vibrational frequencies, thermochemical parameters, magnetic shielding tensors, and the total NMR spin-spin coupling constants. Three scaling factors, depending on the carbon atom hybridizations, were found for the (1)H-C-C-(1)H vicinal coupling constants: f((sp3)-(sp3)) = 0.910, f((sp3)-(sp2)) = 0.929, and f((sp2)-(sp2))= 0.977. A remarkable correlation between the theoretical (J(pre)) and experimental (1)H-(1)H NMR (J(exp)) coupling constants for spicigerolide (1), a cytotoxic natural product, and some of its synthetic stereoisomers (2-4) demonstrated the predictive value of this approach for the stereochemical assignment of highly flexible compounds containing multiple chiral centers. The stereochemistry of two natural 6-heptenyl-5,6-dihydro-2H-pyran-2-ones (14 and 15) containing diverse functional groups in the heptenyl side chain was also analyzed by application of this combined theoretical and experimental approach, confirming its reliability. Additionally, a geometrical analysis for the conformations of 1-8 revealed that weak hydrogen bonds substantially guide the conformational behavior of the tetraacyloxy-6-heptenyl-2H-pyran-2-ones.

  19. Stereospecificity of (1) H, (13) C and (15) N shielding constants in the isomers of methylglyoxal bisdimethylhydrazone: problem with configurational assignment based on (1) H chemical shifts.

    Science.gov (United States)

    Afonin, Andrei V; Pavlov, Dmitry V; Ushakov, Igor A; Keiko, Natalia A

    2012-07-01

    In the (13) C NMR spectra of methylglyoxal bisdimethylhydrazone, the (13) C-5 signal is shifted to higher frequencies, while the (13) C-6 signal is shifted to lower frequencies on going from the EE to ZE isomer following the trend found previously. Surprisingly, the (1) H-6 chemical shift and (1) J(C-6,H-6) coupling constant are noticeably larger in the ZE isomer than in the EE isomer, although the configuration around the -CH═N- bond does not change. This paradox can be rationalized by the C-H⋯N intramolecular hydrogen bond in the ZE isomer, which is found from the quantum-chemical calculations including Bader's quantum theory of atoms in molecules analysis. This hydrogen bond results in the increase of δ((1) H-6) and (1) J(C-6,H-6) parameters. The effect of the C-H⋯N hydrogen bond on the (1) H shielding and one-bond (13) C-(1) H coupling complicates the configurational assignment of the considered compound because of these spectral parameters. The (1) H, (13) C and (15) N chemical shifts of the 2- and 8-(CH(3) )(2) N groups attached to the -C(CH(3) )═N- and -CH═N- moieties, respectively, reveal pronounced difference. The ab initio calculations show that the 8-(CH(3) )(2) N group conjugate effectively with the π-framework, and the 2-(CH(3) )(2) N group twisted out from the plane of the backbone and loses conjugation. As a result, the degree of charge transfer from the N-2- and N-8- nitrogen lone pairs to the π-framework varies, which affects the (1) H, (13) C and (15) N shieldings. Copyright © 2012 John Wiley & Sons, Ltd.

  20. A Classical Approach in Simple Nuclear Fusion Reaction 1H2 + 1H3 using Two-Dimension Granular Molecular Dynamics Model

    CERN Document Server

    Viridi, Sparisoma; Waris, Abdul; Perkasa, Yudha Satya

    2011-01-01

    Molecular dynamics in 2-D accompanied by granular model provides an opportunity to investigate binding between nuclei particles and its properties that arises during collision in a fusion reaction. A fully classical approach is used to observe the influence of initial angle of nucleus orientation to the product yielded by the reaction. As an example, a simplest fusion reaction between 1H2 and 1H3 is observed. Several products of the fusion reaction have been obtained, even the unreported ones, including temporary 2He4 nucleus.

  1. Evaluation of CACNA1H in European patients with childhood absence epilepsy

    NARCIS (Netherlands)

    Chioza, Barry; Everett, Kate; Aschauer, Harald; Brouwer, Oebele; Callenbach, Petra; Covanis, Athanasios; Dulac, Olivier; Durner, Martina; Eeg-Olofsson, Orvar; Feucht, Martha; Friis, Mogens; Heils, Armin; Kjeldsen, Marianne; Larsson, Katrin; Lehesjoki, Anna-Elina; Nabbout, Rima; Olsson, Ingrid; Sander, Thomas; Siren, Auli; Robinson, Robert; Rees, Michele; Gardiner, R. Mark

    2006-01-01

    CACNA1H was evaluated in a resource of Caucasian European patients with childhood absence epilepsy by linkage analysis and typing of sequence variants previously identified in Chinese patients. Linkage analysis of 44 pedigrees provided no evidence for a locus in the CACNA1H region and none of the Ch

  2. An oxazolo[3,2-b]indazole route to 1H-indazolones.

    Science.gov (United States)

    Oakdale, James S; Solano, Danielle M; Fettinger, James C; Haddadin, Makhluf J; Kurth, Mark J

    2009-07-02

    The novel heterocycle 2,3-dihydrooxazolo[3,2-b]indazole has been synthesized and utilized to provide easy access to 1H-indazolones, particularly the previously unreported 2-(2-alkoxyethyl)-1H-indazol-3(2H)-ones. Mechanistic as well as optimization and reaction scope studies are reported.

  3. Reliability of ^1^H NMR analysis for assessment of lipid oxidation at frying temperatures

    Science.gov (United States)

    The reliability of a method using ^1^H NMR analysis for assessment of oil oxidation at a frying temperature was examined. During heating and frying at 180 °C, changes of soybean oil signals in the ^1^H NMR spectrum including olefinic (5.16-5.30 ppm), bisallylic (2.70-2.88 ppm), and allylic (1.94-2.1...

  4. 5-Dimethylamino-1-phenylchromeno[2,3-c]pyrazol-4(1H-one

    Directory of Open Access Journals (Sweden)

    Wolfgang Holzer

    2010-11-01

    Full Text Available The title compound was prepared by treatment of 5-fluoro-1-phenylchromeno [2,3-c]pyrazol-4(1H-one with aqueous dimethylamine. Detailed spectroscopic data (1H NMR, 13C NMR, 15N NMR, IR, MS are presented.

  5. (2E-3-(3-Methoxy-1-phenyl-1H-pyrazol-4-yl-2-propenal

    Directory of Open Access Journals (Sweden)

    Algirdas Šačkus

    2009-12-01

    Full Text Available The palladium-catalyzed reaction of 4-bromo-3-methoxy-1-phenyl-1H-pyrazole with acrolein diethyl acetal gives the title compound in good yield. Detailed spectroscopic data (1H NMR, 13C NMR, 15N NMR, IR, MS are presented.

  6. Complete Genome Sequence of a Bovine Viral Diarrhea Virus Subgenotype 1h Strain Isolated in Italy

    Science.gov (United States)

    Bazzucchi, Moira; Bertolotti, Luigi; Casciari, Cristina; Rossi, Elisabetta; Rosati, Sergio; De Mia, Gian Mario

    2017-01-01

    ABSTRACT We sequenced the complete genome of bovine viral diarrhea virus (BVDV) strain UM/126/07. It belongs to subgenotype 1h. The complete genome is composed of 12,196 nucleotides organized as one open reading frame encoding 3,898 amino acids. This is the first report of a full-length sequence of BVDV-1h. PMID:28232427

  7. Complete Genome Sequence of a Bovine Viral Diarrhea Virus Subgenotype 1h Strain Isolated in Italy.

    Science.gov (United States)

    Bazzucchi, Moira; Bertolotti, Luigi; Giammarioli, Monica; Casciari, Cristina; Rossi, Elisabetta; Rosati, Sergio; De Mia, Gian Mario

    2017-02-23

    We sequenced the complete genome of bovine viral diarrhea virus (BVDV) strain UM/126/07. It belongs to subgenotype 1h. The complete genome is composed of 12,196 nucleotides organized as one open reading frame encoding 3,898 amino acids. This is the first report of a full-length sequence of BVDV-1h.

  8. The complete genome sequence of the Arcobacter butzleri cattle isolate 7h1h

    Science.gov (United States)

    Arcobacter butzleri strain 7h1h was isolated in the UK from a clinically healthy dairy cow. The genome of this isolate was sequenced to completion. Here we present the annotation and analysis of the completed 7h1h genome, as well as comparison of this genome to the existing A. butzleri RM4018 and ED...

  9. Tris{4-[(1,3-diphenyl-1H-pyrazol-4-ylmethylene]-41-aminobiphenyl}amine

    Directory of Open Access Journals (Sweden)

    Sandhya P. Veettil

    2010-04-01

    Full Text Available Tris{4-[(1,3-diphenyl-1H-pyrazol-4-ylmethylene]-41-aminobiphenyl}amine was synthesized from N-(4-bromophenyl-N-[(1,3-diphenyl-1H-pyrazol-4-ylmethylene]amine and tris(4-bromophenylamine based on Ullmann coupling reaction. The synthesized compound was characterized by NMR, IR, MS and elemental analysis.

  10. Synthesis and Molecular Structure of 1,5,1',5'-Tetraphenyl-1H,1H'-3,3'-dialkylthio-bi-1,2,4-triazole

    Institute of Scientific and Technical Information of China (English)

    JIANG Wen-Qing; LIU Tian-Bao; ZOU Jian-Ping; ZHANG Yong

    2007-01-01

    The title compound 1,5,1',5'-tetraphenyl-1H,1H'-3,3'-dialkylthio-bi-1,2,4-triazole (2, C28H20N6S2, Mr=504.62) was prepared by the reaction of 1-benzoyl-3-phenylaminothiourea 1 and Mn(OAc)3·2H2O in acetic acid under microwave irradiation. The crystal is of monoclinic, space group P21/c with a=11.3931(10), b=16.5787(14), c=26.470(2) (A), β=98.274(2)°, Z=8, V=4947.8(8) (A)3, Dc=1.355 g/cm3, μ(MoKα) (A) 0.245 mm-1, F(000)=2096, the final R=0.0583 and Wr=0.1502 for 8705 observed reflections (Ⅰ > 2σ(Ⅰ)). X-ray analysis reveals that the title compound is 1,5,1',5'-tetraphenyl-1H,1H'-3,3'-dialkylthio-bi-1,2,4-triazole, and its formation mechanism was proposed.

  11. Increasing 14N NQR signal by 1H-14N level crossing with small magnetic fields.

    Science.gov (United States)

    Thurber, Kent R; Sauer, Karen L; Buess, Michael L; Klug, Christopher A; Miller, Joel B

    2005-11-01

    NQR detection of materials, such as TNT, is hindered by the low signal-to-noise ratio at low NQR frequencies. Sweeping small (0-26 mT) magnetic fields to shift the (1)H NMR frequency relative to the (14)N NQR frequencies can provide a significant increase of the (14)N NQR signal-to-noise ratio. Three effects of (1)H-(14)N level crossing are demonstrated in diglycine hydrochloride and TNT. These effects are (1) transferring (1)H polarization to one or more of the (14)N transitions, including the use of an adiabatic flip of the (1)H polarization during the field sweep, (2) shortening the effective (14)N T(1) by the interaction of (1)H with the (14)N transitions, (3) "level transfer" effect where the third (14)N (spin 1) energy level or other (14)N sites with different NQR frequency are used as a reservoir of polarization which is transferred to the measured (14)N transition by the (1)H. The (14)N NQR signal-to-noise ratio can be increased by a factor of 2.5 for one (14)N site in diglycine hydrochloride (and 2.2 in TNT), even though the maximum (1)H frequency used in this work, 111 6 kHz, is only 30% larger than the measured (14)N frequencies (834 kHz for diglycine hydrochloride and 843 kHz for TNT).

  12. A common polymorphism in NR1H2 (LXRbeta is associated with preeclampsia

    Directory of Open Access Journals (Sweden)

    Brouillet Jean-Paul

    2011-10-01

    Full Text Available Abstract Background Preeclampsia is a frequent complication of pregnancy and a leading cause of perinatal mortality. Both genetic and environmental risk factors have been identified. Lipid metabolism, particularly cholesterol metabolism, is associated with this disease. Liver X receptors alpha (NR1H3, also known as LXRalpha and beta (NR1H2, also known as LXRbeta play a key role in lipid metabolism. They belong to the nuclear receptor superfamily and are activated by cholesterol derivatives. They have been implicated in preeclampsia because they modulate trophoblast invasion and regulate the expression of the endoglin (CD105 gene, a marker of preeclampsia. The aim of this study was to investigate associations between the NR1H3 and NR1H2 genes and preeclampsia. Methods We assessed associations between single nucleotide polymorphisms of NR1H3 (rs2279238 and rs7120118 and NR1H2 (rs35463555 and rs2695121 and the disease in 155 individuals with preeclampsia and 305 controls. Genotypes were determined by high-resolution melting analysis. We then used a logistic regression model to analyze the different alleles and genotypes for those polymorphisms as a function of case/control status. Results We found no association between NR1H3 SNPs and the disease, but the NR1H2 polymorphism rs2695121 was found to be strongly associated with preeclampsia (genotype C/C: adjusted odds ratio, 2.05; 95% CI, 1.04-4.05; p = 0.039 and genotype T/C: adjusted odds ratio, 1.85; 95% CI, 1.01-3.42; p = 0.049. Conclusions This study provides the first evidence of an association between the NR1H2 gene and preeclampsia, adding to our understanding of the links between cholesterol metabolism and this disease.

  13. Intermolecular Interactions between Eosin Y and Caffeine Using 1H-NMR Spectroscopy

    Directory of Open Access Journals (Sweden)

    Macduff O. Okuom

    2013-01-01

    Full Text Available DETECHIP has been used in testing analytes including caffeine, cocaine, and tetrahydrocannabinol (THC from marijuana, as well as date rape and club drugs such as flunitrazepam, gamma-hydroxybutyric acid (GHB, and methamphetamine. This study investigates the intermolecular interaction between DETECHIP sensor eosin Y (DC1 and the analyte (caffeine that is responsible for the fluorescence and color changes observed in the actual array. Using 1H-NMR, 1H-COSY, and 1H-DOSY NMR methods, a proton exchange from C-8 of caffeine to eosin Y is proposed.

  14. /sup 3/H-/sup 1/H shift correlation NMR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Funke, C.W.; Wagenaars, G.N.; Kaspersen, F.M.

    1986-05-01

    Three two-dimensional /sup 3/H-/sup 1/H chemical shift correlation experiments are described, all using familiar pulse sequences. The experiments reveal the chemical shifts of the /sup 1/H spins which are coupled scalarly to a /sup 3/H spin and, thus, assist in the unambiguous location of this /sup 3/H spin within the molecule. The limitations for molecules involving a /sup 3/H spin which is coupled differently to various /sup 1/H spins are indicated. In practice, the detection limit is of the order of 100 MBq per /sup 3/H-labelling site.

  15. Experience[superscript]2

    Science.gov (United States)

    Barker, Kim

    2011-01-01

    Researching whimsical and spirited artists can inspire new ideas and methods of communicating how art remains a valuable part of people's lives both in and out of the classroom. This instructional resource explores one such contemporary artist who, driven by a curiosity in human interaction, continues to explore the world in fanciful and…

  16. {sup 1}H-MR spectroscopy in anorexia nervosa. Reversible cerebral metabolic changes; {sup 1}H-MR-Spektroskopie bei Anorexia nervosa: Reversible zerebrale Metabolitenaenderungen

    Energy Technology Data Exchange (ETDEWEB)

    Moeckel, R.; Schlemmer, H.P.; Becker, G.; Koepke, J.; Georgi, M. [Heidelberg Univ. (Germany). Inst. fuer Klinische Radiologie; Gueckel, C.; Goepel, C.; Schmidt, M. [Zentralinstitut fuer Seelische Gesundheit, Mannheim (Germany). Klinik fuer Kinder- und Jugendpsychiatrie; Hentschel, F. [Zentralinstitut fuer Seelische Gesundheit, Mannheim (Germany). Neuroradiologie

    1999-04-01

    Purpose: By using localized {sup 1}H-MR spectroscopy in the brain of patients with anorexia nervosa we wanted to verify our preliminary results and to look for a reversibility of the metabolic changes under therapy. Methods: In 22 patients and 17 healthy volunteers (11 follow-up examinations) single voxel {sup 1}H-MR spectroscopy (TE=50 ms, TM=30 ms, TR=1500 ms, voxel (2 cm){sup 3}, acq.: 256) was used in two different localizations (thalamus and parieto-occipital region). The first examination of the patients was performed before therapy, the follow-up examination at the end of therapy. Results: In both regions of the brain we found a statistically significant elevation of the Cho/Cr-ratio in comparison to normal controls. The follow-up examinations revealed reversibility of the metabolic changes under successful therapy. Conclusion: {sup 1}H-MR spectroscopy reveals metabolic changes in the brain of patients with anorexia nervosa, which are reversible under successful therapy. These metabolic changes can be conclusively explained using a biochemical model. (orig.) [Deutsch] Ziel: Im Rahmen dieser weiterfuehrenden Studie sollten die bisherigen Ergebnisse der lokalisierten {sup 1}H-MR-Spektroskopie des Gehirns an Patienten mit Anorexia nervosa verifiziert werden. Weiter sollte ueberprueft werden, ob die von uns nachgewiesenen metabolischen Veraenderungen unter Therapie reversibel sind. Methode: Die {sup 1}H-MR-Spektren wurden bei 22 Patientinnen und 17 Probanden (11 Verlaufskontrollen) in Einzelvolumentechnik (TE=50 ms, TM=30 ms, TR=1500 ms, Voxel: (2 cm){sup 3}, Acq.: 256) in zwei unterschiedlichen Hirnregionen (Thalamus, parieto-okzipitale Region) durchgefuehrt. Die erste Untersuchung der Patienten erfolgte bei Aufnahme und die Verlaufskontrolle zum Abschluss der stationaeren Behandlung. Ergebnisse: Bei den Patienten wurde in beiden Hirnregionen ein statistisch signifikant erhoehter Wert fuer das Cho/Cr-Verhaeltnis im Vergleich zu dem Normalkollektiv nachgewiesen

  17. A novel method for evaluating and improving the 1H-MRSI glioma data quality

    Institute of Scientific and Technical Information of China (English)

    YUAN Kehong; LU Hongyu; BAO Shanglian; CHEN Qiansheng; LI Shaowu; DUAN Chaijie

    2005-01-01

    Metabolic information obtained by proton magnetic resonance spectroscopic imaging (1H-MRSI) has been approved to be a powerful tool to identify either benign or malignant glioma, as well as to confirm the tumor level. However, 1H-MRSI data are affected by various factors, such as the thermal noise, eddy currents, susceptibility artifacts, and rigid body motion. To get accurate quantitative metabolic information, the key problem is to assess the 1H-MRSI data quality. In this paper, we introduce a new evaluating system to filter the data, and a new method, called wavelet denoising method, to improve the data quality under the evaluating system. Experimental results on 1H-MRSI glioma data demonstrate that preprocessing is prerequisite and the proposed algorithm with evaluating system is effective.

  18. On the {sup 1}H NMR spectra of 2-substituted benzoquinones

    Energy Technology Data Exchange (ETDEWEB)

    Tedeschi, E.; Rezende, D.B. [Universidade de Sao Paulo (USP), SP (Brazil). Inst. de Quimica; Arruda Campos, I.P. de, E-mail: ipdacamp@uol.com.br [Universidade Paulista, Sao Paulo, SP (Brazil). Inst. de Ciencias Exatas e Tecnologia. Programa de Pos-Graduacao em Engenharia de Producao

    2009-07-01

    The novel complete analysis of the {sup 1}H NMR spectra of six monosubstituted benzoquinones is reported herein, together with a brief but complete review of the scanty previously published data on benzoquinone and its monosubstituded derivatives. (author)

  19. Synthesis of 2-Substituted Hexahydro-1H-1,4-diazepine Analogues

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    2-substituted hexahydro-1H-1,4-diazepine analogues were synthesized starting from N,N?-dibenzyl-1,3-propylene diamine and methyl-2,3-dibromo propionate through nucleophilic substitution, reduction, chlorination and debenzylation.

  20. catena-Poly[[(diiodidocadmium-μ-{1-[(1H-benzimidazol-2-ylmethyl]-1H-imidazole-κ2N:N′}] N,N-dimethylformamide monosolvate

    Directory of Open Access Journals (Sweden)

    Bingtao Liu

    2011-12-01

    Full Text Available In the title complex, {[CdI2(C11H10N4]·C3H7NO}n, the CdII ion is four-coordinated by two N atoms from two 1-[(1H-benzimidazol-1-ylmethyl]-1H-imidazole (bmi ligands and by two terminal I− anions in a distorted tetrahedral geometry. One of the two I− anions is disordered over two sets of sites, with refined occupancies of 0.66 (5 and 0.34 (5. The CdII ions are bridged by bmi ligands, leading to the formation of a chain along [001]. Dimethylformamide solvent molecules are located between these chains. Classical N—H...O hydrogen bonding between the bmi ligands and the solvent molecules leads to a consolidation of the structure.

  1. Complete 1H, 15N and 13C assignment of trappin-2 and 1H assignment of its two domains, elafin and cementoin.

    Science.gov (United States)

    Loth, Karine; Alami, Soha Abou Ibrahim; Habès, Chahrazed; Garrido, Solène; Aucagne, Vincent; Delmas, Agnès F; Moreau, Thierry; Zani, Marie-Louise; Landon, Céline

    2016-04-01

    Trappin-2 is a serine protease inhibitor with a very narrow inhibitory spectrum and has significant anti-microbial activities. It is a 10 kDa cationic protein composed of two distinct domains. The N-terminal domain (38 residues) named cementoin is known to be intrinsically disordered when it is not linked to the elafin. The C-terminal domain (57 residues), corresponding to elafin, is a cysteine-rich domain stabilized by four disulfide bridges and is characterized by a flat core and a flexible N-terminal part. To our knowledge, there is no structural data available on trappin-2. We report here the complete (1)H, (15)N and (13)C resonance assignment of the recombinant trappin-2 and the (1)H assignments of cementoin and elafin, under the same experimental conditions. This is the first step towards the 3D structure determination of the trappin-2.

  2. Tetraaqua{1-[(1H-1,2,3-benzotriazol-1-ylmethyl]-1H-1,2,4-triazole}sulfatozinc(II dihydrate

    Directory of Open Access Journals (Sweden)

    Yan-Zhi Wang

    2010-11-01

    Full Text Available In the title complex, [Zn(SO4(C9H8N6(H2O4]·2H2O, the ZnII ion is six-coordinated by one N atom from a 1-[(1H-1,2,3-benzotriazol-1-ylmethyl]-1H-1,2,4-triazole ligand and five O atoms from one monodentate sulfate anion and four water molecules in a distorted octahedral geometry. The sulfate tetrahedron is rotationally disordered over two positions in a 0.618 (19:0.382 (19 ratio. In the crystal, adjacent molecules are linked through O—H...O and O—H...N hydrogen bonds involving the cation, the anion, and the coordinated and uncoordinated water molecules into a three-dimensional network.

  3. Tetraaqua{1-[(1H-1,2,3-benzotriazol-1-ylmethyl]-1H-1,2,4-triazole}sulfatocadmium dihydrate

    Directory of Open Access Journals (Sweden)

    Yu-xian Li

    2011-09-01

    Full Text Available In the title complex, [Cd(SO4(C9H8N6(H2O4]·2H2O, the CdII ion is six-coordinated by one N atom from a 1-[(1H-1,2,3-benzotriazol-1-ylmethyl]-1H-1,2,4-triazole ligand and by five O atoms from four water molecules and one monodentate sulfate anion in a distorted octahedral geometry. The sulfate tetrahedron is rotationally disordered over two positions in a 0.651 (12:0.349 (12 ratio. In the crystal, adjacent molecules are linked through O—H...O and O—H...N hydrogen bonds into a three-dimensional network.

  4. Comparative analysis of fecal fat quantitation via nuclear magnetic resonance spectroscopy (1H NMR) and gravimetry.

    Science.gov (United States)

    Korpi-Steiner, Nichole L; Ward, Jennie N; Kumar, Vivek; McConnell, Joseph P

    2009-02-01

    Fecal-fat is typically measured by extracting lipid from homogenized feces with subsequent gravimetric/titrimetric analyses that are time-consuming and involve toxic solvents. Accordingly, an efficient and more safe method to quantitate fecal-fat is needed. The present objective was to adapt CEM SmartTrac technology (i.e. (1)H NMR) to rapidly (fecal-fat and compare (1)H NMR and gravimetric performance characteristics. (1)H NMR and gravimetric measurements of stool-fat were conducted using excess stool samples (72 h collection; n=107) homogenized to semi-liquid consistency prior to analyses. The (1)H NMR method demonstrated acceptable linearity (R(2)=0.9999) and recovery (mean=105%) with imprecision (intra-assay CV=1.2-6.5%; inter-assay CV=1.8-5.8%) comparable to or better than gravimetry (intra-assay CV=1.0-17.2%; inter-assay CV=3.8-6.5%). Excellent correlation between fecal-fat quantitation by (1)H NMR and gravimetry (n=107; R(2)=0.983; y=1.0173x-0.6859) was exhibited; moreover, (1)H NMR demonstrated good sensitivity (92.3%), specificity (94.5%), negative-predictive value (92.9%) and positive-predictive value (94.1%) for malabsorption using the reference cut-off of fat/24 h. These data demonstrate that (1)H NMR permits rapid and safe quantitation of fecal-fat while maintaining acceptable performance characteristics, thereby supporting the utility of (1)H NMR as an alternative method to gravimetry for fecal-fat quantitation.

  5. Supramolecular assemblies based on 2-ureido-4[1H]-pyrimidinone building block

    Institute of Scientific and Technical Information of China (English)

    WANG Sumin; WU Lizhu; ZHANG Liping; TUNG Chenho

    2006-01-01

    With high association constants in nonpolar solvents, the quadruple hydrogen bonding arrays of 2-ureido-4[1H]-pyrimidinones are recently considered to be one of the ideal building blocks to construct the complicated and functional supramole- cular systems. In this paper, we review the latest achievements of the supramolecular assemblies based on 2-ureido-4[1H]-pyrimidinone AADD quadruple hydrogen bonding building blocks.

  6. Regioselective Synthesis and Base Catalyzed Transacylation of Substituted 1H-Pyrazole-4-carboxamides

    Institute of Scientific and Technical Information of China (English)

    REN,Jun(任军); ZHANG,Xiao-Hong(张晓弘); LIU,Ying(刘莹); CHEN,Wei-Qiang(陈卫强); JIN,Gui-Yu(金桂玉)

    2002-01-01

    New type of substituted 1H-pyrazole-4-carboxamides were obtained by regioselective synthesis under the catalysis of different bases. The structures of the title compounds were confirmed by elemental analysis, 1H NMR, IR, MS and X-ray crystallogaphy. Compounds 1 were transacylated into their corresponding amides 3 in the presence of sodium hydride.Preliminary bioassays indicated that some compounds showed fungicidal activities against Rhizoctonia solani and Sclerotinia sclerotiorum.

  7. Proton-detected 3D {sup 1}H/{sup 13}C/{sup 1}H correlation experiment for structural analysis in rigid solids under ultrafast-MAS above 60 kHz

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Rongchun; Ramamoorthy, Ayyalusamy, E-mail: ramamoor@umich.edu [Biophysics and Department of Chemistry, The University of Michigan, Ann Arbor, Michigan 48109-1055 (United States); Nishiyama, Yusuke [JEOL RESONANCE Inc., Musashino, Akishima, Tokyo 196-8558 (Japan); RIKEN CLST-JEOL Collaboration Center, RIKEN, Yokohama, Kanagawa 230-0045 (Japan)

    2015-10-28

    A proton-detected 3D {sup 1}H/{sup 13}C/{sup 1}H chemical shift correlation experiment is proposed for the assignment of chemical shift resonances, identification of {sup 13}C-{sup 1}H connectivities, and proximities of {sup 13}C-{sup 1}H and {sup 1}H-{sup 1}H nuclei under ultrafast magic-angle-spinning (ultrafast-MAS) conditions. Ultrafast-MAS is used to suppress all anisotropic interactions including {sup 1}H-{sup 1}H dipolar couplings, while the finite-pulse radio frequency driven dipolar recoupling (fp-RFDR) pulse sequence is used to recouple dipolar couplings among protons and the insensitive nuclei enhanced by polarization transfer technique is used to transfer magnetization between heteronuclear spins. The 3D experiment eliminates signals from non-carbon-bonded protons and non-proton-bonded carbons to enhance spectral resolution. The 2D (F1/F3) {sup 1}H/{sup 1}H and 2D {sup 13}C/{sup 1}H (F2/F3) chemical shift correlation spectra extracted from the 3D spectrum enable the identification of {sup 1}H-{sup 1}H proximity and {sup 13}C-{sup 1}H connectivity. In addition, the 2D (F1/F2) {sup 1}H/{sup 13}C chemical shift correlation spectrum, incorporated with proton magnetization exchange via the fp-RFDR recoupling of {sup 1}H-{sup 1}H dipolar couplings, enables the measurement of proximities between {sup 13}C and even the remote non-carbon-bonded protons. The 3D experiment also gives three-spin proximities of {sup 1}H-{sup 1}H-{sup 13}C chains. Experimental results obtained from powder samples of L-alanine and L-histidine ⋅ H{sub 2}O ⋅ HCl demonstrate the efficiency of the 3D experiment.

  8. Bulk magnetization and {sup 1}H NMR spectra of magnetically heterogeneous model systems

    Energy Technology Data Exchange (ETDEWEB)

    Levin, E.M., E-mail: levin@iastate.edu [Division of Materials Sciences and Engineering, Ames Laboratory of US DOE (United States); Department of Physics and Astronomy, Iowa State University, Iowa, IA 50011-3020 (United States); Bud' ko, S.L. [Division of Materials Sciences and Engineering, Ames Laboratory of US DOE (United States); Department of Physics and Astronomy, Iowa State University, Iowa, IA 50011-3020 (United States)

    2011-10-15

    Bulk magnetization and {sup 1}H static and magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectra of two magnetically heterogeneous model systems based on laponite (LAP) layered silicate or polystyrene (PS) with low and high proton concentration, respectively, and ferrimagnetic Fe{sub 2}O{sub 3} nano- or micro-particles have been studied. In LAP+Fe{sub 2}O{sub 3}, a major contribution to the NMR signal broadening is due to the dipolar coupling between the magnetic moments of protons and magnetic particles. In PS+Fe{sub 2}O{sub 3}, due to the higher proton concentration in polystyrene and stronger proton-proton dipolar coupling, an additional broadening is observed, i.e. {sup 1}H MAS NMR spectra of magnetically heterogeneous systems are sensitive to both proton-magnetic particles and proton-proton dipolar couplings. An increase of the volume magnetization by {approx}1 emu/cm{sup 3} affects the {sup 1}H NMR signal width in a way that is similar to an increase of the proton concentration by {approx}2x10{sup 22}/cm{sup 3}. {sup 1}H MAS NMR spectra, along with bulk magnetization measurements, allow the accurate determination of the hydrogen concentration in magnetically heterogeneous systems. - Highlights: > {sup 1}H NMR and magnetization allow study of dipolar interactions in magnetically heterogeneous systems. > Both the proton-proton and proton-magnetic particle dipolar interactions affect {sup 1}H NMR spectra. > {sup 1}H NMR and magnetization can be used for the accurate determination of the hydrogen concentration.

  9. 1H magnetic resonance spectroscopy studies on subclinical neurocysticercosis%脑实质囊虫病亚临床期的1H-MRS成像研究

    Institute of Scientific and Technical Information of China (English)

    王青; 张承志; 李信响; 徐鲲; 苏洁

    2016-01-01

    Objective: To evaluate the clinical application of single voxel 1H magnetic resonance spectroscopy in diagnosis of subclinical neurocysticercosis. Materials and Methods: One hundred and ten cases of subclinical neurocysticercosis and 130 cases of cerebral cysticercosis (live worms stage) with contrast enhanced single voxel 1H magnetic resonance spectroscopy were screened for this study. Observation of the change in ratio of the lesions of the subclinical neurocysticercosis and some trace metabolites around the lesions was done. Results: The group of subclinical neurocysticercosis has no significant difference with normal control group in various biochemical metabolites. The ratios of NAA/Cho, Cho/Cr and Lip/Cr have statistical significance in the analysis and evaluation of subclinical neurocysticercosis group and live worms stage group. The ratio of NAA/Cho in subclinical neurocysticercosis group is higher than live worms stage group. The ratios of Cho/Cr and Lip/Cr of the former are lower than that of the latter. The ratios of NAA/Cho and Lip/Cr evaluate the differential diagnosis efficiency between subclinical neurocysticercosis stage and live worms stage on ROC curve. Conclusions: 1H-MRS reveals the changes in characteristics of subclinical neurocysticercosis stage and live worms stage so as to evaluate the corresponding diagnosis index of the ratios of NAA/Cho and Lip/Cr, which are of great value to early diagnosis and treatment of the neurocysticercosis.%目的:应用单体素1H-MRS波谱成像前瞻性研究对其脑实质囊虫病亚临床期的诊断价值。材料与方法筛选110例脑实质囊虫病亚临床期为研究对象,并与130例脑实质囊虫病活虫期为对照,进行单体素1H-MRS波谱成像检查,观测脑实质囊虫(亚临床期)病灶及其周围区域某些微量代谢产物比值的变化,并进行对照评价。结果脑实质囊虫病亚临床期与正常镜像区组各生化代谢物比值结果均无显著性差异

  10. Design, synthesis and anticancer activity of new 3-cyano-2 (1H -pyridone and 3-cyanopyridine-2-(1H-thione derivatives

    Directory of Open Access Journals (Sweden)

    E. A. Abdel Motaal

    2015-06-01

    Full Text Available The main objective of the present research study is to synthesize some novel chalcone, cyanoacetohydrazone, enaminone, 3-cyano-2(1H-pyridone and 3-cyanopyridine-2-(1H-thione derivatives and evaluate them for their anticancer effect. The novel chalcones 2a-c were achieved by Claisen-Schmidt condensation of appropriate benzaldehydes with ethanone derivative 1. Treatment of cyanoacetic acid hydrazide with ethanone derivative 1 yielded the correspondinghydrazone derivative 3. Condensation of ethanone derivative 1 with DMF-DMA afforded (E-3-(dimethylamino-1- (4- morpholinophenylprop-2-en-1-one 4. Heterocyclization of chalcones 2a-c with cyanothioacetamide yielded 2-thioxo-1,2-dihydropyridine-3-carbonitriles 7a-c. In a similar manner, cyclocondensation of chalcones 2a,b with cyanoacetamide afforded the corresponding 2-oxo-1,2-dihydropyridine-3-carbonitriles 8a,b. The Reaction of compound 2a with ethyl cyanoacetate furnished 2-oxo-1,2-dihydropyridine-3-carboxylate 12. The 2-oxo-4-phenyl-1,2-dihydro-pyridine-3,5-dicarbonitriles 14a,b were obtained by cyclization of cyano-acetohydrazone 3 with cinnamonitriles. The structures of the synthesized compounds were confirmed by elemental analysis, mass spectrometry, IR and 1H-NMR spectroscopy. The anticancer activity of the newly synthesized compounds was screened in vitro against Human lung carcinoma (A 549 cell line indicating that compounds 7b and 8a possess the most potent inhibitory effect against the human lung carcinoma cell line (A549.

  11. Transformation of 1H-benzotriazole by ozone in aqueous solution.

    Science.gov (United States)

    Mawhinney, Douglas B; Vanderford, Brett J; Snyder, Shane A

    2012-07-01

    Recent studies have shown that 1H-benzotriazole is a widespread contaminant of wastewater and surface water. Although disinfection by ozone has been shown to efficiently remove this compound, the transformation products have not been identified. To that end, the reaction of ozone with 1H-benzotriazole in aqueous solution has been studied in real time employing quadrupole time-of-flight mass spectrometry (Q-TOF MS) and negative electrospray ionization. The transformation products have been identified by calculating their empirical formulas using accurate mass measurements, and further confirmed by performing the reaction with stable isotope-labeled 1H-benzotriazole and measuring product ion spectra. Stable reaction products were distinguished from transient species by plotting their extracted mass profiles. The products that resulted from ozone and hydroxyl radicals in the reaction were qualitatively identified by modifying the conditions to either promote the formation of hydroxyl radicals, or to scavenge them. Based on experimental evidence, a mechanism for the direct reaction between ozone and 1H-benzotriazole is proposed that results in the formation of 1H-1,2,3-triazole-4,5-dicarbaldehyde, which has an empirical formula of C(4)H(3)O(2)N(3). Lastly, it was confirmed that the same transformation products formed in surface water and tertiary-treated wastewater, although they were observed to degrade at higher ozone doses.

  12. A disc wind interpretation of the strong Fe Kα features in 1H 0707-495

    Science.gov (United States)

    Hagino, Kouichi; Odaka, Hirokazu; Done, Chris; Tomaru, Ryota; Watanabe, Shin; Takahashi, Tadayuki

    2016-10-01

    1H 0707-495 is the most convincing example of a supermassive black hole with an X-ray spectrum being dominated by extremely smeared, relativistic reflection, with the additional requirement of strongly supersolar iron abundance. However, here we show that the iron features in its 2-10 keV spectrum are rather similar to the archetypal wind dominated source, PDS 456. We fit all the 2-10 keV spectra from 1H 0707-495 using the same wind model as used for PDS 456, but viewed at higher inclination so that the iron absorption line is broader but not so blueshifted. This gives a good overall fit to the data from 1H 0707-495, and an extrapolation of this model to higher energies also gives a good match to the NuSTAR data. Small remaining residuals indicate that the iron line emission is stronger than in PDS 456. This is consistent with the wider angle wind expected from a continuum-driven wind from the super-Eddington mass accretion rate in 1H 0707-495, and/or the presence of residual reflection from the underlying disc though the presence of the absorption line in the model removes the requirement for highly relativistic smearing, and highly supersolar iron abundance. We suggest that the spectrum of 1H 0707-495 is sculpted more by absorption in a wind than by extreme relativistic effects in strong gravity.

  13. 1H relaxation dispersion in solutions of nitroxide radicals: Influence of electron spin relaxation

    Science.gov (United States)

    Kruk, D.; Korpała, A.; Kubica, A.; Kowalewski, J.; Rössler, E. A.; Moscicki, J.

    2013-03-01

    The work presents a theory of nuclear (1H) spin-lattice relaxation dispersion for solutions of 15N and 14N radicals, including electron spin relaxation effects. The theory is a generalization of the approach presented by Kruk et al. [J. Chem. Phys. 137, 044512 (2012)], 10.1063/1.4736854. The electron spin relaxation is attributed to the anisotropic part of the electron spin-nitrogen spin hyperfine interaction modulated by rotational dynamics of the paramagnetic molecule, and described by means of Redfield relaxation theory. The 1H relaxation is caused by electron spin-proton spin dipole-dipole interactions which are modulated by relative translational motion of the solvent and solute molecules. The spectral density characterizing the translational dynamics is described by the force-free-hard-sphere model. The electronic relaxation influences the 1H relaxation by contributing to the fluctuations of the inter-molecular dipolar interactions. The developed theory is tested against 1H spin-lattice relaxation dispersion data for glycerol solutions of 4-oxo-TEMPO-d16-15N and 4-oxo-TEMPO-d16-14N covering the frequency range of 10 kHz-20 MHz. The studies are carried out as a function of temperature starting at 328 K and going down to 290 K. The theory gives a consistent overall interpretation of the experimental data for both 14N and 15N systems and explains the features of 1H relaxation dispersion resulting from the electron spin relaxation.

  14. Localized 1H-MR spectroscopy in moyamoya disease before and after revascularization surgery

    Energy Technology Data Exchange (ETDEWEB)

    Lim, Soo Mee; Choi, Hye Young; Suh, Jung Soo [Ewha Womans University Hospital, Seoul (Korea, Republic of); Lee, Jung Hee; Lim, Keun Ho; Suh, Dae Chul; Lee, Ho Kyu; Lim, Tae Hwan; Ra, Young Shin [Ulsan University College of Medicine, Seoul (Korea, Republic of)

    2003-06-01

    To evaluate, using localized proton magnetic resonance spectroscopy (1H-MRS), the cerebral metabolic change apparent after revascularization surgery in patients with moyamoya disease. Sixteen children with moyamoya disease and eight age-matched normal controls underwent MR imaging, MR angiography, conventional angiography, and {sup 99m}Tc- ECD SPECT. Frontal white matter and the basal ganglia of both hemispheres were subjected to localized {sup 1}H-MRS, and after revascularization surgery, four patients underwent follow-up {sup 1}H-MRS. Decreased NAA/Cr ratios (1.35{+-}0.14 in patients vs. 1.55{+-}0.24 in controls) and Cho/Cr ratios (0.96{+-}0.13 in patients vs. 1.10{+-}0.11 in controls) were observed in frontal white matter. After revascularization surgery, NAA/Cr and Cho/Cr ratios in this region increased. In the basal ganglia, there is no abnormal metabolic ratios. Localized 1H-MRS revealed abnormal metabolic change in both hemispheres of children with moyamoya disease. Because of its non-invasive nature, {sup 1}H-MRS is potentially useful for the preoperative evaluation of metabolic abnormalities and their postoperative monitoring.

  15. Sequence-specific Assignment of 1H-NMR Resonance and Determination of the Secondary Structure of HWTX-II%虎纹捕鸟蛛毒素HWTX-II的1H-NMR信号归属和二级结构分析

    Institute of Scientific and Technical Information of China (English)

    舒芹; 吕善运; 顾孝诚; 梁宋平

    2001-01-01

    虎纹捕鸟蛛毒素HWTX-II是从虎纹捕鸟蛛Selenocosmia huwena的毒液中分离出的一种新型杀虫肽。应用2D-NMR技术研究该毒素分子的溶液结构特点, 通过分析水及重水DQF-COSY、COSY、TOCSY和NOESY等1H-NMR谱, 识别出HWTX-II全部37个氨基酸残基自旋体系; 通过NOESY谱中的dαN、dαδ、dβN和dNN联系完成了序列专一的谱峰归属, 确认了所有主链质子和除了Lys侧链εNH2质子外的所有侧链质子的化学位移, 为完全解析HWTX-II的溶液三维构象奠定了基础。 并且通过核磁数据分析, 确定HWTX-II的二级结构特点是含有较多的伸展构象, 尤其是C端有一个典型的双股反平行的β折叠(Trp27~Cys29和Cys34~Lys36), 分子中缺乏螺旋结构。 这些二级结构特点与已探明结构的其他蜘蛛毒素的基本相同。%Huwentoxin-II (HWTX-II) is an insecticidal peptide purified from the venom of spider Selenocosmia huwena. The structure of this toxin in solution was investigated using 2D-NMR. The complete sequence-specific assignments of proton resonance in the 1H-NMR spectra of HWTX-II were obtained by analyzing a series of 2D spectrum, including COSY, DQF-COSY, TOCSY and NOESY. All the backbone protons and side chain protons, except εNH2 protons of Lys residues, were identified by dαN, dαδ, dNN and dβN connectivities. The results provide a basis for further determination of the solution conformation of HWTX-II. Furthermore the secondary structure of HWTX-II was determined from NMR data. It contained mainly extended conformation, especially a double-stranded anti-parallel β-sheet with Trp27—Cys29 and Cys34—Lys36 at the C terminal, and it lacked helix. These characters of the secondary structure of HWTX-II were similar to those spider toxins which structure in solution had been reported.

  16. Effect of fertilizers on galanthamine and metabolite profiles in Narcissus bulbs by 1H NMR.

    Science.gov (United States)

    Lubbe, Andrea; Choi, Young Hae; Vreeburg, Peter; Verpoorte, Robert

    2011-04-13

    Narcissus bulbs contain the biologically active alkaloid galanthamine, and Narcissus is being developed as a natural source of the molecule for the pharmaceutical industry. The effect of fertilizer on galanthamine production was investigated in a field study using a (1)H nuclear magnetic resonance (NMR) metabolite profiling approach. Galanthamine was quantitated and major metabolites in the bulbs were identified. The application of standard fertilization levels of nitrogen and potassium caused a significant increase in galanthamine as compared to a control. Multivariate data analysis of the (1)H NMR data revealed that applying double the standard level of nitrogen fertilizer resulted in production of more amino acids and citric acid cycle intermediates, but not more galanthamine. The results indicated that standard levels of fertilizer currently applied in The Netherlands are sufficient for optimal galanthamine accumulation in the bulbs. This study shows how (1)H NMR-based metabolic profiling can provide insight into the response of plant metabolism to agricultural practices.

  17. Approximation methods of mixed l 1/H2 optimization problems for MIMO discrete-time systems

    Institute of Scientific and Technical Information of China (English)

    李昇平

    2004-01-01

    The mixed l1/H2 optimization problem for MIMO (multiple input-multiple output) discrete-time systems is eonsidered. This problem is formulated as minimizing the l1-norm of a dosed-loop transfer matrix while maintaining the H2-norm of another closed-loop transfer matrix at prescribed level. The continuity property of the optimal value in respect to changes in the H2-norm constraint is studied. The existence of the optimal solutions of mixed l1/H2 problem is proved. Becatse the solution of the mixed l1/H2 problem is based on the scaled-Q method, it avoids the zero interpolation difficulties. The convergent upper and lower bounds can be obtained by solving a sequence of finite dimensional nonlinear programming for which many efficient numerical optimization algorithms exist.

  18. Double-tuned radiofrequency coil for (19)F and (1)H imaging.

    Science.gov (United States)

    Otake, Yosuke; Soutome, Yoshihisa; Hirata, Koji; Ochi, Hisaaki; Bito, Yoshitaka

    2014-01-01

    We developed a double-tuned radiofrequency (RF) coil using a novel circuit method to double tune for fluorine-19 (19F) and 1H magnetic resonance imaging, whose frequencies are very close to each other. The RF coil consists of 3 parallel-connected series inductor capacitor circuits. A computer simulation for our double-tuned RF coil with a phantom demonstrated that the coil has tuned resonant frequency and high sensitivity for both 19F and 1H. Drug distribution was visualized at 7 tesla using this RF coil and a rat administered perfluoro 15-crown-5-ether emulsion. The double-tune RF coil we developed may be a powerful tool for 19F and 1H imaging.

  19. Relativistic Force Field: Parametrization of (13)C-(1)H Nuclear Spin-Spin Coupling Constants.

    Science.gov (United States)

    Kutateladze, Andrei G; Mukhina, Olga A

    2015-11-01

    Previously, we reported a reliable DU8 method for natural bond orbital (NBO)-aided parametric scaling of Fermi contacts to achieve fast and accurate prediction of proton-proton spin-spin coupling constants (SSCC) in (1)H NMR. As sophisticated NMR experiments for precise measurements of carbon-proton SSCCs are becoming more user-friendly and broadly utilized by the organic chemistry community to guide and inform the process of structure determination of complex organic compounds, we have now developed a fast and accurate method for computing (13)C-(1)H SSCCs. Fermi contacts computed with the DU8 basis set are scaled using selected NBO parameters in conjunction with empirical scaling coefficients. The method is optimized for inexpensive B3LYP/6-31G(d) geometries. The parametric scaling is based on a carefully selected training set of 274 ((3)J), 193 ((2)J), and 143 ((1)J) experimental (13)C-(1)H spin-spin coupling constants reported in the literature. The DU8 basis set, optimized for computing Fermi contacts, which by design had evolved from optimization of a collection of inexpensive 3-21G*, 4-21G, and 6-31G(d) bases, offers very short computational (wall) times even for relatively large organic molecules containing 15-20 carbon atoms. The most informative SSCCs for structure determination, i.e., (3)J, were computed with an accuracy of 0.41 Hz (rmsd). The new unified approach for computing (1)H-(1)H and (13)C-(1)H SSCCs is termed "DU8c".

  20. Protein conformational exchange measured by 1H R1ρ relaxation dispersion of methyl groups.

    Science.gov (United States)

    Weininger, Ulrich; Blissing, Annica T; Hennig, Janosch; Ahlner, Alexandra; Liu, Zhihong; Vogel, Hans J; Akke, Mikael; Lundström, Patrik

    2013-09-01

    Activated dynamics plays a central role in protein function, where transitions between distinct conformations often underlie the switching between active and inactive states. The characteristic time scales of these transitions typically fall in the microsecond to millisecond range, which is amenable to investigations by NMR relaxation dispersion experiments. Processes at the faster end of this range are more challenging to study, because higher RF field strengths are required to achieve refocusing of the exchanging magnetization. Here we describe a rotating-frame relaxation dispersion experiment for (1)H spins in methyl (13)CHD2 groups, which improves the characterization of fast exchange processes. The influence of (1)H-(1)H rotating-frame nuclear Overhauser effects (ROE) is shown to be negligible, based on a comparison of R 1ρ relaxation data acquired with tilt angles of 90° and 35°, in which the ROE is maximal and minimal, respectively, and on samples containing different (1)H densities surrounding the monitored methyl groups. The method was applied to ubiquitin and the apo form of calmodulin. We find that ubiquitin does not exhibit any (1)H relaxation dispersion of its methyl groups at 10 or 25 °C. By contrast, calmodulin shows significant conformational exchange of the methionine methyl groups in its C-terminal domain, as previously demonstrated by (1)H and (13)C CPMG experiments. The present R 1ρ experiment extends the relaxation dispersion profile towards higher refocusing frequencies, which improves the definition of the exchange correlation time, compared to previous results.

  1. Elevated glutamatergic compounds in pregenual anterior cingulate in pediatric autism spectrum disorder demonstrated by 1H MRS and 1H MRSI.

    Directory of Open Access Journals (Sweden)

    Anthony Bejjani

    Full Text Available Recent research in autism spectrum disorder (ASD has aroused interest in anterior cingulate cortex and in the neurometabolite glutamate. We report two studies of pregenual anterior cingulate cortex (pACC in pediatric ASD. First, we acquired in vivo single-voxel proton magnetic resonance spectroscopy ((1H MRS in 8 children with ASD and 10 typically developing controls who were well matched for age, but with fewer males and higher IQ. In the ASD group in midline pACC, we found mean 17.7% elevation of glutamate + glutamine (Glx (p<0.05 and 21.2% (p<0.001 decrement in creatine + phosphocreatine (Cr. We then performed a larger (26 subjects with ASD, 16 controls follow-up study in samples now matched for age, gender, and IQ using proton magnetic resonance spectroscopic imaging ((1H MRSI. Higher spatial resolution enabled bilateral pACC acquisition. Significant effects were restricted to right pACC where Glx (9.5%, p<0.05, Cr (6.7%, p<0.05, and N-acetyl-aspartate + N-acetyl-aspartyl-glutamate (10.2%, p<0.01 in the ASD sample were elevated above control. These two independent studies suggest hyperglutamatergia and other neurometabolic abnormalities in pACC in ASD, with possible right-lateralization. The hyperglutamatergic state may reflect an imbalance of excitation over inhibition in the brain as proposed in recent neurodevelopmental models of ASD.

  2. Electrowetting Performances of Novel Fluorinated Polymer Dielectric Layer Based on Poly(1H,1H,2H,2H-perfluoroctylmethacrylate Nanoemulsion

    Directory of Open Access Journals (Sweden)

    Jiaxin Hou

    2017-06-01

    Full Text Available In electrowetting devices, hydrophobic insulating layer, namely dielectric layer, is capable of reversibly switching surface wettability through applied electric field. It is critically important but limited by material defects in dielectricity, reversibility, film forming, adhesiveness, price and so on. To solve this key problem, we introduced a novel fluorinated polyacrylate—poly(1H,1H,2H,2H-perfluoroctylmethacrylate (PFMA to construct micron/submicron-scale dielectric layer via facile spray coating of nanoemulsion for replacing the most common Teflon AF series. All the results illustrated that, continuous and dense PFMA film with surface relief less than 20 nm was one-step fabricated at 110 °C, and exhibited much higher static water contact angle of 124°, contact angle variation of 42°, dielectric constant of about 2.6, and breakdown voltage of 210 V than Teflon AF 1600. Particularly, soft and highly compatible polyacrylate mainchain assigned five times much better adhesiveness than common adhesive tape, to PFMA layer. As a promising option, PFMA dielectric layer may further facilitate tremendous development of electrowetting performances and applications.

  3. (1)H-NMR, (1)H-NMR T2-edited, and 2D-NMR in bipolar disorder metabolic profiling.

    Science.gov (United States)

    Sethi, Sumit; Pedrini, Mariana; Rizzo, Lucas B; Zeni-Graiff, Maiara; Mas, Caroline Dal; Cassinelli, Ana Cláudia; Noto, Mariane N; Asevedo, Elson; Cordeiro, Quirino; Pontes, João G M; Brasil, Antonio J M; Lacerda, Acioly; Hayashi, Mirian A F; Poppi, Ronei; Tasic, Ljubica; Brietzke, Elisa

    2017-12-01

    The objective of this study was to identify molecular alterations in the human blood serum related to bipolar disorder, using nuclear magnetic resonance (NMR) spectroscopy and chemometrics. Metabolomic profiling, employing (1)H-NMR, (1)H-NMR T2-edited, and 2D-NMR spectroscopy and chemometrics of human blood serum samples from patients with bipolar disorder (n = 26) compared with healthy volunteers (n = 50) was performed. The investigated groups presented distinct metabolic profiles, in which the main differential metabolites found in the serum sample of bipolar disorder patients compared with those from controls were lipids, lipid metabolism-related molecules (choline, myo-inositol), and some amino acids (N-acetyl-L-phenyl alanine, N-acetyl-L-aspartyl-L-glutamic acid, L-glutamine). In addition, amygdalin, α-ketoglutaric acid, and lipoamide, among other compounds, were also present or were significantly altered in the serum of bipolar disorder patients. The data presented herein suggest that some of these metabolites differentially distributed between the groups studied may be directly related to the bipolar disorder pathophysiology. The strategy employed here showed significant potential for exploring pathophysiological features and molecular pathways involved in bipolar disorder. Thus, our findings may contribute to pave the way for future studies aiming at identifying important potential biomarkers for bipolar disorder diagnosis or progression follow-up.

  4. A practical, metal-free synthesis of 1H-indazoles.

    Science.gov (United States)

    Counceller, Carla M; Eichman, Chad C; Wray, Brenda C; Stambuli, James P

    2008-03-06

    The synthesis of 1H-indazoles is achieved from o-aminobenzoximes by the selective activation of the oxime in the presence of the amino group. The reaction occurs with a variety of substituted o-aminobenzoximes using a slight excess of methanesulfonyl chloride and triethylamine at 0-23 degrees C and is amenable to scale-up. The synthesis of 1H-indazoles under these conditions is extremely mild compared with previous synthetic approaches and affords the desired compounds in good to excellent yields.

  5. A novel approach for the synthesis of 5-substituted-1H-tetrazoles

    Energy Technology Data Exchange (ETDEWEB)

    Akhlaghinia, Batool; Rezazadeh, Soodabeh, E-mail: akhlaghinia@um.ac.ir [Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad (Iran, Islamic Republic of)

    2012-12-15

    A series of 5-substituted-1H-tetrazoles (RCN{sub 4}H) have been synthesized by cycloaddition reaction of different aryl and alkyl nitriles with sodium azide in DMSO using CuSO{sub 4}{center_dot}5H{sub 2}O as catalyst. A wide variety of aryl nitriles underwent [3+2] cycloaddition to afford tetrazoles under mild reaction conditions in good to excellent yields. The catalyst used is readily available and environmentally friendly. Short reaction times, good to excellent yields, safe process and simple workup make this method an attractive and useful contribution to present organic synthesis of 5-substituted-1H-tetrazoles. (author)

  6. Synthesis of 2-azetidinone derivatives of 6-nitro-1H-indazole and their biological importance

    Directory of Open Access Journals (Sweden)

    Pushkal Samadhiya

    2012-01-01

    Full Text Available A new series of 3-chloro-1-{[2-(6-nitro-1H-indazol-1-ylethyl]amino}-4-(substituted phenyl-2-azetidinones (4a-j was synthesized in four steps from 6-nitro-1H-indazole and characterized by IR, ¹H NMR, 13C NMR, FAB-mass spectrometry and chemical methods. Compounds 4(a-j were screened in vitro for their antibacterial, antifungal and antitubercular activities against some selected microorganism and for their antiinflammatory activity (in vivo against albino rats (either sex. All above activities of compounds 4(a-j showed acceptable results.

  7. Copper-Promoted Oxidative C-H Bond Amination of Hydrazones: Synthesis of 1H-Indazoles and 1H-Pyrazoles%铜促进下腙的氧化胺化反应:1H-吲唑和1H-吡唑的合成

    Institute of Scientific and Technical Information of China (English)

    丁正伟; 谭启涛; 刘秉新; 张可; 许斌

    2015-01-01

    吲唑和吡唑是两类重要的含氮杂环化合物,具有广泛的生物活性.发展了一类铜促进下腙的C(sp2)-H键氧化胺化反应,简便、高效地构建了一系列1H-吲唑和1H-吡唑衍生物.该反应条件温和,具有广泛的底物适用范围和较好的官能团兼容性.

  8. Methylation of 5-Amino-3-methylthio-1H-pyrazole Derivatives and Two Related Crystal Structures

    Institute of Scientific and Technical Information of China (English)

    REN, Xue-Ling(任雪玲); WU, Chao(吴超); HU, Fang-Zhong(胡方中); ZOU, Xiao-Mao(邹小毛); YANG, Hua-Zheng(杨华铮)

    2004-01-01

    5-Amino-3-methylthio-1H-pyrazoles are very important building blocks from which a wide variety of pyrazole derivatives can be prepared. When substituted 5-amino-3-methylthio-1H-pyrazole was treated with CH3I, the methylation occurres at endocyclic two nitrogens at the same time. The ratio of isomers in products was depended upon the nature of 4-position substituent in the pyrazole ring. The products were characterized by X-ray diffraction analysis, and the ratios of isomer were explained by means of the results of ab inito calculation.

  9. Spiroheterocyclization of Methyl 1-Aryl-3-cinnamoyl-4,5-dioxo-4,5-dihydro-1H-pyrrole-2-carboxylates by the Action of 3-(Arylamino-1H-inden-1-ones

    Directory of Open Access Journals (Sweden)

    Аndrey N. Maslivets

    2012-11-01

    Full Text Available Methyl 1-aryl-3-cinnamoyl-4,5-dioxo-4,5-dihydro-1H-pyrrole-2-carboxylates interact with 3-(arylamino-1H-inden-1-ones to give the corresponding 1,1'-diaryl-3'-cinnamoyl-4'-hydroxy-1H-spiro[indeno[1,2-b]pyrrole-3,2'-pyrrole]-2,4,5'(1'H-triones in good yields.

  10. Evaluation of 1H NMR relaxometry for the assessment of pore size distribution in soil samples

    NARCIS (Netherlands)

    Jaeger, F.; Bowe, S.; As, van H.; Schaumann, G.E.

    2009-01-01

    1H NMR relaxometry is used in earth science as a non-destructive and time-saving method to determine pore size distributions (PSD) in porous media with pore sizes ranging from nm to mm. This is a broader range than generally reported for results from X-ray computed tomography (X-ray CT) scanning, wh

  11. Aminosilanes derived from 1H-benzimidazole-2(3H)-thione

    Energy Technology Data Exchange (ETDEWEB)

    Palomo-Molina, Juliana [Facultad de Ciencias Químicas, Universidad de Colima, Carretera Coquimatlán-Colima, Coquimatlán Colima 28400 (Mexico); García-Báez, Efrén V. [Unidad Profesional Interdisciplinaria de Biotecnología, Instituto Politécnico Nacional, Avenida Acueducto s/n, Barrio La Laguna Ticomán, México DF 07340 (Mexico); Contreras, Rosalinda [Departamento de Química, Centro de Investigación y de Estudios Avanzados del IPN, Apartado Postal 14-740, México DF 07000 (Mexico); Barrio La Laguna Ticomán, México DF 07340 (Mexico); Pineda-Urbina, Kayim; Ramos-Organillo, Angel, E-mail: aaramos@ucol.mx [Facultad de Ciencias Químicas, Universidad de Colima, Carretera Coquimatlán-Colima, Coquimatlán Colima 28400 (Mexico)

    2015-08-12

    In two trimethylsilyl-substituted 1H-benzimidazole-2(3H)-thiones, noncovalent C—H⋯π interactions between the centroid of the benzmidazole system and the SiMe{sub 3} groups form helicoidal arrangements in one, and dimerization results in the formation of R{sub s} {sup 2}(8) rings via N—H⋯S interactions, along with parallel π–π interactions between imidazole and benzene rings, in the second compound. Two new molecular structures, namely 1,3-bis(trimethylsilyl)-1H-benzimidazole-2(3H)-thione, C{sub 13}H{sub 22}N{sub 2}SSi{sub 2}, (2), and 1-trimethylsilyl-1H-benzimidazole-2(3H)-thione, C{sub 10}H{sub 14}N{sub 2}SSi, (3), are reported. Both systems were derived from 1H-benzimidazole-2(3H)-thione. Noncovalent C—H⋯π interactions between the centroid of the benzmidazole system and the SiMe{sub 3} groups form helicoidal arrangements in (2). Dimerization of (3) results in the formation of R{sub 2}{sup 2}(8) rings via N—H⋯S interactions, along with parallel π–π interactions between imidazole and benzene rings.

  12. Synthesis, antimicrobial and cytotoxic activity of novel azetidine-2-one derivatives of 1H-benzimidazole

    Directory of Open Access Journals (Sweden)

    Malleshappa Noolvi

    2014-04-01

    Full Text Available A series of 1-methyl-N-[(substituted-phenylmethylidene-1H-benzimidazol-2-amines (4a–4g were prepared via the formation of 1-methyl-1H-benzimidazol-2-amine (3, which was prepared by the cycloaddition of o-phenylenediamine (1 with cyanogen bromide in the presence of aqueous base followed by N-methylation with methyl iodide in the presence of anhydrous potassium carbonate in dry acetonitrile. Moreover, the four-membered β-lactam ring was introduced by the cycloaddition of 4a–4g and chloroacetyl chloride in the presence of triethylamine catalyst to give 3-chloro-1-(1-methyl-1H-benzimidazol-2-yl-(4′-substituted-phenylazetidin-2-one 5a–5g. A total of 14 compounds were synthesized and characterized by IR, 1H NMR, 13C NMR and Mass spectral technique, in addition they were evaluated for anti-bacterial and cytotoxic properties. Among the chemicals tested 4a, 4b, 5a, 5b, 5g exhibited good antibacterial activity and 5f, 5g shown good cytotoxic activity in vitro.

  13. Wild salmon authenticity can be predicted by 1H-NMR spectroscopy

    NARCIS (Netherlands)

    Capuano, E.; Lommen, A.; Heenan, S.P.; Dura, de la A.; Rozijn, M.; Ruth, van S.M.

    2012-01-01

    The combination of 1H NMR fingerprinting of muscle lipids from fresh and processed (frozen, canned and smoked) Atlantic salmon (Salmo salar) with supervised multivariate analysis was applied to differentiate wild and farmed fish. Soft Independent Modelling of Class Analogy (SIMCA) allowed classifica

  14. One-pot synthesis of novel 2,3-dihydro-1H-indazoles.

    Science.gov (United States)

    Breton, Gary W; Lepore, Antonio J

    2011-11-16

    A copper(I)-mediated one-pot synthesis of 2,3-dihydro-1H-indazole heterocycles has been developed. This synthetic route provides the desired indazoles in moderate to good yields (55%-72%) which are substantially better than those achievable with an alternative two-step reaction sequence. The reaction is tolerant of functionality on the aromatic ring.

  15. Synthesis of 1H-Indazoles from Imidates and Nitrosobenzenes via Synergistic Rhodium/Copper Catalysis.

    Science.gov (United States)

    Wang, Qiang; Li, Xingwei

    2016-05-06

    Nitrosobenzenes have been used as a convenient aminating reagent for the efficient synthesis of 1H-indazoles via rhodium and copper catalyzed C-H activation and C-N/N-N coupling. The reaction occurred under redox-neutral conditions with high efficiency and functional group tolerance. Moreover, a rhodacyclic imidate complex has been identified as a key intermediate.

  16. The neutron star soft X-ray transient 1H 1905+000 in quiescence

    NARCIS (Netherlands)

    Jonker, P.G.; Bassa, C.G.; Nelemans, G.; Juett, A.M.; Brown, E.F.; Chakrabarty, D.

    2006-01-01

    In this paper, we report on our analysis of a ~25ks. Chandra X-ray observation of the neutron star soft X-ray transient (SXT) 1H 1905+000 in quiescence. Furthermore, we discuss our findings of the analysis of optical photometric observations which we obtained using the Magellan telescope and photome

  17. Quantitative Analysis of Chemically Modified Starches by 1H-NMR Spectroscopy

    NARCIS (Netherlands)

    Graaf, R.A. de; Lammers, G.; Janssen, L.P.B.M.; Beenackers, A.A.C.M.

    1995-01-01

    A quantitative 1H-NMR method for the determination of the Molar Substitution (MS) of acetylated and hydroxypropylated starches was developed and tested for MS ranging from 0.09 to 0.5. Results were checked using the Johnson method and a titration method for hydroxypropylated and acetylated starch, r

  18. Conformational analysis of MBBA fluorinated analogues by 1H and 13C - NMR

    Science.gov (United States)

    Pivovarova, N. S.; Boldeskul, I. E.; Shelyagenko, S. V.; Fialkov, Yu. A.

    1988-05-01

    1H- 13C -chemical shifts correlation analysis for MBBA and a series of its fluorinated analogues have been carried out. The azomethine proton chemical shift is shown to be sensitive to the aniline ring torsion angle and can be used for its approximate estimation.

  19. Bulk magnetization and 1H NMR spectra of magnetically heterogeneous model systems

    Science.gov (United States)

    Levin, E. M.; Bud'ko, S. L.

    2011-10-01

    Bulk magnetization and 1H static and magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectra of two magnetically heterogeneous model systems based on laponite (LAP) layered silicate or polystyrene (PS) with low and high proton concentration, respectively, and ferrimagnetic Fe2O3 nano- or micro-particles have been studied. In LAP+Fe2O3, a major contribution to the NMR signal broadening is due to the dipolar coupling between the magnetic moments of protons and magnetic particles. In PS+Fe2O3, due to the higher proton concentration in polystyrene and stronger proton-proton dipolar coupling, an additional broadening is observed, i.e. 1H MAS NMR spectra of magnetically heterogeneous systems are sensitive to both proton-magnetic particles and proton-proton dipolar couplings. An increase of the volume magnetization by ∼1 emu/cm3 affects the 1H NMR signal width in a way that is similar to an increase of the proton concentration by ∼2×1022/cm3. 1H MAS NMR spectra, along with bulk magnetization measurements, allow the accurate determination of the hydrogen concentration in magnetically heterogeneous systems.

  20. An Efficient Approach to 6, 7-Disubstituted-1H-quinoxalin-2-ones

    Institute of Scientific and Technical Information of China (English)

    Xun LI; Qing Ping HU; Xue Gui CUI; Dong Hua WANG

    2004-01-01

    A novel approach to the synthesis of 6, 7-disubstituted-1H-quinoxalin-2-ones is described.The title compounds were regioselectively prepared by starting from substituted phenylamines and chloroacetyl chloride through the efficient sequence ofacylation, nitration, reduction, intramolecular alkylation, and oxidation.

  1. Wine analysis to check quality and authenticity by fully-automated 1H-NMR

    Directory of Open Access Journals (Sweden)

    Spraul Manfred

    2015-01-01

    Full Text Available Fully-automated high resolution 1H-NMR spectroscopy offers unique screening capabilities for food quality and safety by combining non-targeted and targeted screening in one analysis (15–20 min from acquisition to report. The advantage of high resolution 1H-NMR is its absolute reproducibility and transferability from laboratory to laboratory, which is not equaled by any other method currently used in food analysis. NMR reproducibility allows statistical investigations e.g. for detection of variety, geographical origin and adulterations, where smallest changes of many ingredients at the same time must be recorded. Reproducibility and transferability of the solutions shown are user-, instrument- and laboratory-independent. Sample prepara- tion, measurement and processing are based on strict standard operation procedures which are substantial for this fully automated solution. The non-targeted approach to the data allows detecting even unknown deviations, if they are visible in the 1H-NMR spectra of e.g. fruit juice, wine or honey. The same data acquired in high-throughput mode are also subjected to quantification of multiple compounds. This 1H-NMR methodology will shortly be introduced, then results on wine will be presented and the advantages of the solutions shown. The method has been proven on juice, honey and wine, where so far unknown frauds could be detected, while at the same time generating targeted parameters are obtained.

  2. Effect of fertilizers on galanthamine and metabolite profiles in narcissus bulbs by 1H NMR

    NARCIS (Netherlands)

    Lubbe, A.; Choi, Y.H.; Vreeburg, P.J.M.; Verpoorte, R.

    2011-01-01

    Narcissus bulbs contain the biologically active alkaloid galanthamine, and Narcissus is being developed as a natural source of the molecule for the pharmaceutical industry. The effect of fertilizer on galanthamine production was investigated in a field study using a 1H nuclear magnetic resonance (NM

  3. Co-III-Carbene Radical Approach to Substituted 1H-Indenes

    NARCIS (Netherlands)

    Das, B.G.; Chirila, A.; Tromp, M.; Reek, J.N.H.; de Bruin, B.

    2016-01-01

    A new strategy for the catalytic synthesis of substituted 1H-indenes via metalloradical activation of o-cinnamyl N-tosyl hydrazones is presented, taking advantage of the intrinsic reactivity of a Co-III carbene radical intermediate. The reaction uses readily available starting materials and is

  4. An Efficient Green Synthesis of 3-Amino-1H-chromenes Catalyzed ...

    African Journals Online (AJOL)

    NICO

    disorder.18. Traditional methods have been reported for the synthesis of ... vantages and potentially explore industrial applications.38 ... sol-gel, hydrothermal, thermal evaporation, oxidation and anodization.39–45 Although the use of ZnO nanoparticles (NPs) ... 1aryl-1H-benzo[f]chromene-2-carbonitriles (4) via a three-.

  5. Effect of fertilizers on galanthamine and metabolite profiles in narcissus bulbs by 1H NMR

    NARCIS (Netherlands)

    Lubbe, A.; Choi, Y.H.; Vreeburg, P.J.M.; Verpoorte, R.

    2011-01-01

    Narcissus bulbs contain the biologically active alkaloid galanthamine, and Narcissus is being developed as a natural source of the molecule for the pharmaceutical industry. The effect of fertilizer on galanthamine production was investigated in a field study using a 1H nuclear magnetic resonance (NM

  6. NMR resonance splitting of urea in stretched hydrogels: proton exchange and (1)H/(2)H isotopologues.

    Science.gov (United States)

    Kuchel, Philip W; Naumann, Christoph; Chapman, Bogdan E; Shishmarev, Dmitry; Håkansson, Pär; Bacskay, George; Hush, Noel S

    2014-10-01

    Urea at ∼12 M in concentrated gelatin gel, that was stretched, gave (1)H and (2)H NMR spectral splitting patterns that varied in a predictable way with changes in the relative proportions of (1)H2O and (2)H2O in the medium. This required consideration of the combinatorics of the two amide groups in urea that have a total of four protonation/deuteration sites giving rise to 16 different isotopologues, if all the atoms were separately identifiable. The rate constant that characterized the exchange of the protons with water was estimated by back-transformation analysis of 2D-EXSY spectra. There was no (1)H NMR spectral evidence that the chiral gelatin medium had caused in-equivalence in the protons bonded to each amide nitrogen atom. The spectral splitting patterns in (1)H and (2)H NMR spectra were accounted for by intra-molecular scalar and dipolar interactions, and quadrupolar interactions with the electric field gradients of the gelatin matrix, respectively.

  7. Synthesis of 1H-indazoles from N-tosylhydrazones and nitroaromatic compounds.

    Science.gov (United States)

    Liu, Zhenxing; Wang, Long; Tan, Haocheng; Zhou, Shiyi; Fu, Tianren; Xia, Ying; Zhang, Yan; Wang, Jianbo

    2014-05-21

    A new method for the synthesis of 1H-indazoles from readily available N-tosylhydrazones and nitroaromatic compounds has been developed. This transformation occurs under transition-metal-free conditions and shows a wide substrate scope. The method has been successfully applied to the formal synthesis of a bioactive compound, WAY-169916.

  8. [Brain metabolism alterations in patients with anorexia nervosa observed in 1H-MRS

    NARCIS (Netherlands)

    Grzelak, P.; Gajewicz, W.; Wyszogrodzka-Kucharska, A.; Rotkiewicz, A.; Stefanczyk, L.; Goraj, B.M.; Rabe-Jablonska, J.

    2005-01-01

    The causes of metabolic brain changes in patients with anorexia nervosa are still not fully explained. The purpose of this study was to use the 1H-MRS method in investigating metabolic changes in the brain of patients with anorexia nervosa. We studied 10 patients for visible alternations in brain me

  9. Amyloidogenicity and aggregate cytotoxicity of human glucagon-like peptide-1 (hGLP-1).

    Science.gov (United States)

    Poon, S; Birkett, N R; Fowler, S B; Luisi, B F; Dobson, C M; Zurdo, J

    2009-01-01

    The potential of human glucagon-like peptide-1 (hGLP-1) as a therapeutic agent is limited by its high aggregation propensity. We show that hGLP-1 forms amyloid-like structures that are preceded by cytotoxic aggregates, suggesting that aggregation of biopharmaceuticals could present a cytotoxic risk to patients besides the reported increased risk in immunogenicity.

  10. Glycosylation intermediates studied using low temperature 1H- and 19F-DOSY NMR

    DEFF Research Database (Denmark)

    Qiao, Yan; Ge, Wenzhi; Jia, Lingyu

    2016-01-01

    Low temperature 1H- and 19F-DOSY have been used for analyzing reactive intermediates in glycosylation reactions, where a glycosyl trichloroacetimidate donor has been activated using different catalysts. The DOSY protocols have been optimized for low temperature experiments and provided new insight...

  11. MICROWAVE-ASSISTED SYNTHESIS OF SOME 5(6)-NITRO-1H ...

    African Journals Online (AJOL)

    Preferred Customer

    reagents for the synthesis of 2-substitued benzimidazoles [5-9]. ... study, we wish to report the synthesis of 5-nitro-1H-benzimidazoles and their ... Diethyl Ether ... iminoester hydrochloride 1(a-d) (0.013 mol) in methanol (30 mL) were stirred at ...

  12. Effect of paramagnetic manganese cations on (1)H MRS of the brain

    DEFF Research Database (Denmark)

    Madsen, Kathrine Skak; Holm, David Alberg; Vejby Søgaard, Lise

    2008-01-01

    Manganese cations (Mn(2+)) can be used as an intracellular contrast agent for structural, functional and neural pathway imaging applications. However, at high concentrations, Mn(2+) is neurotoxic and may influence the concentration of (1)H MR-detectable metabolites. Furthermore, the paramagnetic Mn...

  13. 1H NMR spectroscopy-based interventional metabolic phenotyping: a cohort study of rheumatoid arthritis patients

    DEFF Research Database (Denmark)

    Lauridsen, Michael Brændgaard; Bliddal, Henning; Christensen, Robin Daniel Kjersgaard;

    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...

  14. Refined structure of a flexible heptasaccharide using {sup 1}H-{sup 13}C and {sup 1}H-{sup 1}H NMR residual dipolar couplings in concert with NOE and long range scalar coupling constants

    Energy Technology Data Exchange (ETDEWEB)

    Martin-Pastor, Manuel; Bush, C. Allen [University of Maryland-Baltimore County, Department of Chemistry and Biochemistry (United States)

    2001-02-15

    The heptasaccharide isolated from the cell wall polysaccharide of Streptococcus mitis J22 serves as an important model for the dynamics and conformation of complex polysaccharides, illustrating the nature of flexibility with rigid epitopes joined by flexible hinges. One-bond C-H residual dipolar couplings ({sup 1}D{sub CH}) and long-range H-H residual dipolar couplings ({sup n}D{sub HH}) were measured for the heptasaccharide in a cetylpyridinium chloride/hexanol/brine lamellar liquid crystal medium. A method is proposed to determine the {sup n}D{sub HH} in natural abundance based on a {sup 13}C resolved {sup 1}H TOCSY pulse sequence previously published to determine the homonuclear scalar couplings. Different methods for interpretation of the {sup 1}D{sub CH} and the {sup n}D{sub HH} residual dipolar coupling data obtained were compared and combined with the NOE and long-range H,C and C,C scalar couplings available for this heptasaccharide. A flexible model of the heptasaccharide was determined in which two structurally well-defined regions involving four and two sugar residues, respectively are joined by a flexible hinge which involves two 1{sup {yields}}6 glycosidic linkages.

  15. Crystal structures of the two salts 2-methyl-1H-imidazol-3-ium nitrate-2-methyl-1H-imidazole (1/1) and 2-methyl-1H-imidazol-3-ium nitrate.

    Science.gov (United States)

    Diop, Mouhamadou Birame; Diop, Libasse; Maris, Thierry

    2016-04-01

    The title salts, C4H7N2 (+)·NO3 (-)·C4H6N2, (I), and C4H7N2 (+)·NO3 (-), (II), were obtained from solutions containing 2-methyl-imidazole and nitric acid in different concentrations. In the crystal structure of salt (I), one of the -NH H atoms of the imidazole ring shows half-occupancy, hence only every second mol-ecule is in its cationic form. The nitrate anion in this structure lies on a twofold rotation axis. The neutral 2-methyl-imidazole mol-ecule and the 2-methyl-1H-imidazol-3-ium cation inter-act through N-H⋯N hydrogen bonds to form [(C4H6N2)⋯(C4H7N2)(+)] pairs. These pairs are linked with two nitrate anions on both sides through bifurcated N-H⋯(O,O) hydrogen bonds into chains running parallel to [001]. In the crystal structure of salt (II), the C4H7N2 (+) cation and the NO3 (-) anion are both located on a mirror plane, leading to a statistical disorder of the methyl H atoms. The cations and anions again inter-act through bifurcated N-H⋯(O,O) hydrogen bonds, giving rise to the formation of chains consisting of alternating anions and cations parallel to [100].

  16. Crystal structures of the two salts 2-methyl-1H-imidazol-3-ium nitrate–2-methyl-1H-imidazole (1/1) and 2-methyl-1H-imidazol-3-ium nitrate

    Science.gov (United States)

    Diop, Mouhamadou Birame; Diop, Libasse; Maris, Thierry

    2016-01-01

    The title salts, C4H7N2 +·NO3 −·C4H6N2, (I), and C4H7N2 +·NO3 −, (II), were obtained from solutions containing 2-methyl­imidazole and nitric acid in different concentrations. In the crystal structure of salt (I), one of the –NH H atoms of the imidazole ring shows half-occupancy, hence only every second mol­ecule is in its cationic form. The nitrate anion in this structure lies on a twofold rotation axis. The neutral 2-methyl­imidazole mol­ecule and the 2-methyl-1H-imidazol-3-ium cation inter­act through N—H⋯N hydrogen bonds to form [(C4H6N2)⋯(C4H7N2)+] pairs. These pairs are linked with two nitrate anions on both sides through bifurcated N—H⋯(O,O) hydrogen bonds into chains running parallel to [001]. In the crystal structure of salt (II), the C4H7N2 + cation and the NO3 − anion are both located on a mirror plane, leading to a statistical disorder of the methyl H atoms. The cations and anions again inter­act through bifurcated N—H⋯(O,O) hydrogen bonds, giving rise to the formation of chains consisting of alternating anions and cations parallel to [100]. PMID:27375869

  17. Refined structure of a flexible heptasaccharide using 1H-13C and 1H-1H NMR residual dipolar couplings in concert with NOE and long range scalar coupling constants.

    Science.gov (United States)

    Martin-Pastor, M; Bush, C A

    2001-02-01

    The heptasaccharide isolated from the cell wall polysaccharide of Streptococcus mitis J22 serves as an important model for the dynamics and conformation of complex polysaccharides, illustrating the nature of flexibility with rigid epitopes joined by flexible hinges. One-bond C-H residual dipolar couplings (1D(CH)) and long-range H-H residual dipolar couplings (nD(HH)) were measured for the heptasaccharide in a cetylpyridinium chloride/hexanol/brine lamellar liquid crystal medium. A method is proposed to determine the nD(HH) in natural abundance based on a 13C resolved 1H TOCSY pulse sequence previously published to determine the homonuclear scalar couplings. Different methods for interpretation of the 1D(CH) and the nD(HH) residual dipolar coupling data obtained were compared and combined with the NOE and long-range H,C and C,C scalar couplings available for this heptasaccharide. A flexible model of the heptasaccharide was determined in which two structurally well-defined regions involving four and two sugar residues, respectively are joined by a flexible hinge which involves two 1-->6 glycosidic linkages.

  18. Synthesis and Biological Activities of Schiff Bases of 3-Amino-1H-1,2,4-triazole

    Institute of Scientific and Technical Information of China (English)

    SUN,Xiaohong; LIU,Yuanfa; CHEN,Shuzhe; CHEN,Bang; JIA,Yingqi; ZENG,Zhengfang

    2009-01-01

    Eight Schiff bases of 3-amino-1H-1,2,4-triazole have been synthesized by glacial acetic acid catalyzed conden- sation of 3-amino-1H-1,2,4-triazole with substituted benzaldehyde and structurally confirmed by IR, 1H NMR and elemental analysis. The preliminary bioassay showed that the title compounds exhibited good fungicidal activities.

  19. Brief synthesis of 1H-indazole-3-carbaldehyde%1H-吲唑-3-甲醛的简便合成

    Institute of Scientific and Technical Information of China (English)

    朱五福; 王海燕; 曹云云; 白玫; 宫平

    2012-01-01

    1H-Indazole-3-carbaldehyde was obtained by the ring opening of indole in acid condition, and the followed di-azotization with.sodium nitrite,then cyclization,with the yield 36% . This method has the advantage of low cost,simple operation, short reaction time and it is. Also suitable for industrial production.%以吲哚为原料,酸性条件下与亚硝酸钠发生重氮化反应,重氮盐环合得到标题化合物,收率36%,该方法原料易得、操作简单、反应时间短,适合工业化生产.

  20. Study of 1H-MR spectroscopy in the peritumoral area of gliomas%脑胶质瘤周围区的1H-MRS研究

    Institute of Scientific and Technical Information of China (English)

    王佳; 范国光

    2010-01-01

    目的应用多体素氢质子磁共振波谱(1H-MRS)探讨胶质瘤周围区脑代谢改变的特点,评价多体素1H-MRS在胶质瘤周围区的应用价值.方法23例病理证实的脑胶质瘤病人分为低级别组(WHO Ⅰ~Ⅱ级)13例和高级别组(WHOⅢ~Ⅳ级)10例.所有病例术前均行多体素1H-MRS检查,测量肿瘤实质区、周围区及对侧正常脑组织区代谢产物的相对定量,进行统计学比较.结果多体素1H-MRS显示高级别胶质瘤的周围区与实质区NAA/Cr、Cho/Cr、NAA/Cho值差异有统计学意义(P值均为0.00).高级别胶质瘤周围区与对侧正常脑组织区NAA/Cr、Cho/Cr、NAA/Cho、Glx/Cr值差异均有统计学意义(P值均为0.00);低级别胶质瘤周围区与实质区NAA/Cr、Cho/Cr、NAA/Cho值差异均有统计学意义(P值均为0.00);低级别胶质瘤周围区与对侧正常脑组织区Cho/Cr、NAA/Cho值差异均有统计学意义(P值分别为0.02、0.00);高级别与低级别胶质瘤实质区NAA/Cr、NAA/Cho、Cho/Cr、Glx/Cr值差异均有统计学意义(P值分别为0.00、0.00、0.03、0.00);高级别与低级别胶质瘤周嗣区NAA/Cr、NAA/Cho、Cho/Cr、Glx/Cr值差异均有统计学意义(P值均为0.00).结论脑胶质瘤周围区代谢物的改变反映了肿瘤向瘤周组织浸润,对确定胶质瘤的分级及预测侵袭性病变的浸润范围有帮助.

  1. Investigation of Coating Performance of UV-Curable Hybrid Polymers Containing 1H,1H,2H,2H-Perfluorooctyltriethoxysilane Coated on Aluminum Substrates

    Directory of Open Access Journals (Sweden)

    Mustafa Çakır

    2017-03-01

    Full Text Available This study describes preparation and characterization of fluorine-containing organic-inorganic hybrid coatings. The organic part consists of bisphenol-A glycerolate (1 glycerol/phenol diacrylate resin and 1,6-hexanediol diacrylate reactive diluent. The inorganically rich part comprises trimethoxysilane-terminated urethane, 1H,1H,2H,2H-perfluorooctyltriethoxysilane, 3-(trimethoxysilyl propyl methacrylate and sol–gel precursors that are products of hydrolysis and condensation reactions. Bisphenol-A glycerolate (1 glycerol/phenol diacrylate resin was added to the inorganic part in predetermined amounts. The resultant mixture was utilized in the preparation of free films as well as coatings on aluminum substrates. Thermal and mechanical tests such as DSC, thermo-gravimetric analysis (TGA, and tensile and shore D hardness tests were performed on free films. Water contact angle, gloss, Taber abrasion test, cross-cut and tubular impact tests were conducted on the coated samples. SEM examination and EDS analysis was performed on the fractured surfaces of free films. The hybrid coatings on the aluminum sheets gave rise to properties such as moderately glossed surface; low wear rate and hydrophobicity. Tensile strength of free films increased with up to 10% inorganic content in the hybrid structure and this increase was approximately three times that of the control sample. As expected; the % strain value decreased by 17.3 with the increase in inorganic content and elastic modulus values increased by a factor of approximately 6. Resistance to ketone-based solvents was proven and an increase in hardness was observed as the ratio of the inorganic part increased. Samples which contain 10% sol–gel content were observed to provide optimal properties.

  2. 1H NMR spectra. Part 30(+): 1H chemical shifts in amides and the magnetic anisotropy, electric field and steric effects of the amide group.

    Science.gov (United States)

    Abraham, Raymond J; Griffiths, Lee; Perez, Manuel

    2013-03-01

    The (1)H spectra of 37 amides in CDCl(3) solvent were analysed and the chemical shifts obtained. The molecular geometries and conformational analysis of these amides were considered in detail. The NMR spectral assignments are of interest, e.g. the assignments of the formamide NH(2) protons reverse in going from CDCl(3) to more polar solvents. The substituent chemical shifts of the amide group in both aliphatic and aromatic amides were analysed using an approach based on neural network data for near (≤3 bonds removed) protons and the electric field, magnetic anisotropy, steric and for aromatic systems π effects of the amide group for more distant protons. The electric field is calculated from the partial atomic charges on the N.C═O atoms of the amide group. The magnetic anisotropy of the carbonyl group was reproduced with the asymmetric magnetic anisotropy acting at the midpoint of the carbonyl bond. The values of the anisotropies Δχ(parl) and Δχ(perp) were for the aliphatic amides 10.53 and -23.67 (×10(-6) Å(3)/molecule) and for the aromatic amides 2.12 and -10.43 (×10(-6) Å(3)/molecule). The nitrogen anisotropy was 7.62 (×10(-6) Å(3)/molecule). These values are compared with previous literature values. The (1)H chemical shifts were calculated from the semi-empirical approach and also by gauge-independent atomic orbital calculations with the density functional theory method and B3LYP/6-31G(++) (d,p) basis set. The semi-empirical approach gave good agreement with root mean square error of 0.081 ppm for the data set of 280 entries. The gauge-independent atomic orbital approach was generally acceptable, but significant errors (ca. 1 ppm) were found for the NH and CHO protons and also for some other protons.

  3. Structural, electronic and vibrational properties of N,N'-1H,1H-perfluorobutyl dicyanoperylenecarboxydiimide (PDI-FCN2) crystal

    Science.gov (United States)

    Colle, Renato; Grosso, Giuseppe; Cassinese, Antonio; Centore, Roberto

    2013-09-01

    We present a theoretical and experimental investigation of the crystalline structure of N,N'-1H,1H-perfluorobutyl dicyanoperylenecarboxydiimide (PDI-FCN2) that has been deduced combining experimental XRD data, obtained from powders, with global-optimization algorithms which allow to identify Bravais lattice, primitive cell parameters, and space group of the crystal. The XRD spectrum calculated for the proposed crystalline structure very well reproduces the measured XRD data. Our results suggest the triclinic lattice structure of spatial groups Poverline{1} and P1, respectively, for the crystalline PDI-FCN2-1,7 and PDI-FCN2-1,6 isomers. In both cases, the primitive cell contains a single molecule. On the proposed crystalline structures, KS-DFT cell energy calculations, including van der Waals interactions, have been performed to assign the minimum energy geometrical structure and orientation of the molecule inside the corresponding primitive cell. These calculations evidence the molecular packing that characterizes the strong anisotropy of the PDI-FCN2 crystal. Electronic band-structures calculated for both isomers within the Kohn-Sham density-functional theory indicate that the crystalline Poverline{1} structure is an indirect gap semiconductor, while the P1 structure is a direct gap semiconductor. The electronic band structure calculations on the optimized crystal geometries highlight strong anisotropy in the dispersion curves E(k), which roots at the molecular packing in the crystal. Finally, the vibrational spectrum of both crystalline isomers has been calculated in the harmonic approximation and the dominant vibrational frequencies have been associated to collective motions of selected atoms in the molecules.

  4. Structural, electronic and vibrational properties of N,N'-1H,1H-perfluorobutyl dicyanoperylenecarboxydiimide (PDI-FCN2) crystal.

    Science.gov (United States)

    Colle, Renato; Grosso, Giuseppe; Cassinese, Antonio; Centore, Roberto

    2013-09-21

    We present a theoretical and experimental investigation of the crystalline structure of N,N'-1H,1H-perfluorobutyl dicyanoperylenecarboxydiimide (PDI-FCN2) that has been deduced combining experimental XRD data, obtained from powders, with global-optimization algorithms which allow to identify Bravais lattice, primitive cell parameters, and space group of the crystal. The XRD spectrum calculated for the proposed crystalline structure very well reproduces the measured XRD data. Our results suggest the triclinic lattice structure of spatial groups P1 and P1, respectively, for the crystalline PDI-FCN2-1,7 and PDI-FCN2-1,6 isomers. In both cases, the primitive cell contains a single molecule. On the proposed crystalline structures, KS-DFT cell energy calculations, including van der Waals interactions, have been performed to assign the minimum energy geometrical structure and orientation of the molecule inside the corresponding primitive cell. These calculations evidence the molecular packing that characterizes the strong anisotropy of the PDI-FCN2 crystal. Electronic band-structures calculated for both isomers within the Kohn-Sham density-functional theory indicate that the crystalline P1 structure is an indirect gap semiconductor, while the P1 structure is a direct gap semiconductor. The electronic band structure calculations on the optimized crystal geometries highlight strong anisotropy in the dispersion curves E(k), which roots at the molecular packing in the crystal. Finally, the vibrational spectrum of both crystalline isomers has been calculated in the harmonic approximation and the dominant vibrational frequencies have been associated to collective motions of selected atoms in the molecules.

  5. Translational diffusion in paramagnetic liquids by 1H NMR relaxometry: nitroxide radicals in solution.

    Science.gov (United States)

    Kruk, D; Korpała, A; Kubica, A; Meier, R; Rössler, E A; Moscicki, J

    2013-01-14

    For nitroxide radicals in solution one can identify three frequency regimes in which (1)H spin-lattice relaxation rate of solvent molecules depend linearly on square root of the (1)H resonance frequency. Combining a recently developed theory of nuclear (proton) spin-lattice relaxation in solutions of nitroxide radicals [D. Kruk et al., J. Chem. Phys. 137, 044512 (2012)] with properties of the spectral density function associated with translational dynamics, relationships between the corresponding linear changes of the relaxation rate (for (14)N spin probes) and relative translational diffusion coefficient of the solvent and solute molecules have been derived (in analogy to (15)N spin probes [E. Belorizky et al., J. Phys. Chem. A 102, 3674 (1998)]). This method allows a simple and straightforward determination of diffusion coefficients in spin-labeled systems, by means of (1)H nuclear magnetic resonance (NMR) relaxometry. The approach has thoroughly been tested by applying to a large set of experimental data-(1)H spin-lattice relaxation dispersion results for solutions of different viscosity (decalin, glycerol, propylene glycol) of (14)N and (15)N spin probes. The experiments have been performed versus temperature (to cover a broad range of translational diffusion coefficients) using field cycling spectrometer which covers three decades in (1)H resonance frequency, 10 kHz-20 MHz. The limitations of NMR relaxometry caused by the time scale of the translational dynamics as well as electron spin relaxation have been discussed. It has been shown that for spin-labeled systems NMR relaxometry gives access to considerably faster diffusion processes than for diamagnetic systems.

  6. Translational diffusion in paramagnetic liquids by 1H NMR relaxometry: Nitroxide radicals in solution

    Science.gov (United States)

    Kruk, D.; Korpała, A.; Kubica, A.; Meier, R.; Rössler, E. A.; Moscicki, J.

    2013-01-01

    For nitroxide radicals in solution one can identify three frequency regimes in which 1H spin-lattice relaxation rate of solvent molecules depend linearly on square root of the 1H resonance frequency. Combining a recently developed theory of nuclear (proton) spin-lattice relaxation in solutions of nitroxide radicals [D. Kruk et al., J. Chem. Phys. 137, 044512 (2012)], 10.1063/1.4736854 with properties of the spectral density function associated with translational dynamics, relationships between the corresponding linear changes of the relaxation rate (for 14N spin probes) and relative translational diffusion coefficient of the solvent and solute molecules have been derived (in analogy to 15N spin probes [E. Belorizky et al., J. Phys. Chem. A 102, 3674 (1998)], 10.1021/jp980397h). This method allows a simple and straightforward determination of diffusion coefficients in spin-labeled systems, by means of 1H nuclear magnetic resonance (NMR) relaxometry. The approach has thoroughly been tested by applying to a large set of experimental data—1H spin-lattice relaxation dispersion results for solutions of different viscosity (decalin, glycerol, propylene glycol) of 14N and 15N spin probes. The experiments have been performed versus temperature (to cover a broad range of translational diffusion coefficients) using field cycling spectrometer which covers three decades in 1H resonance frequency, 10 kHz-20 MHz. The limitations of NMR relaxometry caused by the time scale of the translational dynamics as well as electron spin relaxation have been discussed. It has been shown that for spin-labeled systems NMR relaxometry gives access to considerably faster diffusion processes than for diamagnetic systems.

  7. Sequential acquisition of multi-dimensional heteronuclear chemical shift correlation spectra with 1H detection

    Science.gov (United States)

    Bellstedt, Peter; Ihle, Yvonne; Wiedemann, Christoph; Kirschstein, Anika; Herbst, Christian; Görlach, Matthias; Ramachandran, Ramadurai

    2014-03-01

    RF pulse schemes for the simultaneous acquisition of heteronuclear multi-dimensional chemical shift correlation spectra, such as {HA(CA)NH & HA(CACO)NH}, {HA(CA)NH & H(N)CAHA} and {H(N)CAHA & H(CC)NH}, that are commonly employed in the study of moderately-sized protein molecules, have been implemented using dual sequential 1H acquisitions in the direct dimension. Such an approach is not only beneficial in terms of the reduction of experimental time as compared to data collection via two separate experiments but also facilitates the unambiguous sequential linking of the backbone amino acid residues. The potential of sequential 1H data acquisition procedure in the study of RNA is also demonstrated here.

  8. Inclusion complex of benzocaine and β-cyclodextrin: 1H NMR and isothermal titration calorimetry studies

    Science.gov (United States)

    Mic, Mihaela; Pırnǎu, Adrian; Bogdan, Mircea; Turcu, Ioan

    2013-11-01

    The supramolecular structure of the inclusion complex of β-cyclodextrin with benzocaine in aqueous solution has been investigated by 1H NMR spectroscopy and isothermal titration nanocalorimetry (ITC). Analysis of 1H NMR data by continuous variation method indicates that the benzocaine: β-cyclodextrin inclusion complex occurs and has a 1:1 stoichiometry. Rotating frame NOE spectroscopy (ROESY) was used to ascertain the solution geometry of the host-guest complex which indicates that the benzocaine molecule was included with the aromatic ring into the cyclodextrin cavity. Although the affinity of benzocaine for cyclodextrin is relatively high, the association constant cannot be measured using ITC due to the low solubility of benzocaine in water.

  9. A sup 1 H nuclear magnetic resonance study of structural and organisational changes in the cell

    CERN Document Server

    Tunnah, S K

    2000-01-01

    Increasing importance is being placed on understanding the role of membrane lipids in many different areas of biochemistry. It is of interest to determine what interactions may occur between membrane lipids and drug species. Furthermore, an increasing body of evidence suggests that membrane lipids are involved in the pathology of numerous diseases such as rheumatoid arthritis, cancer and HIV. Clearly, the more information available on the mechanisms involved in diseases, the greater the potential for identifying a cure or even a prevention. sup 1 H nuclear magnetic resonance (NMR) spectroscopy was used to study the alterations in membrane lipid organisation and structure in intact, viable cultured cells. Changes in the sup 1 H NMR spectra and the spin-lattice relaxation measurements of the human K562 and the rat FRTL-5 cell lines were observed on the addition of the fatty acid species: triolein, evening primrose oil, arachidonic acid and ITF 1779. Results indicate that the membrane lipids are reorganised to a...

  10. Amplitude-integrated electroencephalogram 1 h after birth in a preterm infant with cystic periventricular leukomalacia.

    Science.gov (United States)

    Kato, Toru; Okumura, Akihisa; Hayakawa, Fumio; Tsuji, Takeshi; Hayashi, Seiji; Natsume, Jun

    2013-01-01

    We report a preterm infant, who showed abnormal amplitude-integrated electroencephalogram (aEEG) findings 1 h after birth and later developed cystic periventricular leukomalacia (PVL). The patient was a girl with a gestational age of 29 weeks. She was delivered by emergency cesarean section because of placental abruption and intrauterine co-twin demise. Artificial ventilation and administration of surfactant were needed to treat respiratory distress syndrome. Her cardiovascular condition was stable with artificial ventilation. Cranial ultrasonography showed extended cystic PVL after 11 days of age. aEEG 1 h after birth showed a consistently inactive pattern that resolved completely 28 h after birth. The neurophysiological findings of this patient suggest that aEEG findings during the very early period after birth provide significant information for predicting PVL.

  11. Shaft Sinking at the Nevada Test Site, U1h Shaft Project

    Energy Technology Data Exchange (ETDEWEB)

    B. Briggs; R. Musick

    2001-03-01

    The U1h Shaft Project is a design/build subcontract to construct one 6.1 meter (m) (20 feet (ft)) finished diameter shaft to a depth of 321.6 m (1,055 ft.) at the Nevada Test Site. Atkinson Construction was subcontracted by Bechtel Nevada to construct the U1h Shaft for the U.S. Department of Energy. The project consists of furnishing and installing the sinking plant, construction of the 321.6 m (1,055 ft.) of concrete lined shaft, development of a shaft station at a depth of 297.5 m (976 ft.), and construction of a loading pocket at the station. The outfitting of the shaft and installation of a new hoist may be incorporated into the project at a later date. This paper will describe the design phase, the excavation and lining operation, shaft station construction and the contractual challenges encountered on this project.

  12. Evaluation of saffron (Crocus sativus L.) adulteration with plant adulterants by (1)H NMR metabolite fingerprinting.

    Science.gov (United States)

    Petrakis, Eleftherios A; Cagliani, Laura R; Polissiou, Moschos G; Consonni, Roberto

    2015-04-15

    In the present work, a preliminary study for the detection of adulterated saffron and the identification of the adulterant used by means of (1)H NMR and chemometrics is reported. Authentic Greek saffron and four typical plant-derived materials utilised as bulking agents in saffron, i.e., Crocus sativus stamens, safflower, turmeric, and gardenia were investigated. A two-step approach, relied on the application of both OPLS-DA and O2PLS-DA models to the (1)H NMR data, was adopted to perform authentication and prediction of authentic and adulterated saffron. Taking into account the deficiency of established methodologies to detect saffron adulteration with plant adulterants, the method developed resulted reliable in assessing the type of adulteration and could be viable for dealing with extensive saffron frauds at a minimum level of 20% (w/w).

  13. GFT projection NMR for efficient (1)H/ (13)C sugar spin system identification in nucleic acids.

    Science.gov (United States)

    Atreya, Hanudatta S; Sathyamoorthy, Bharathwaj; Jaipuria, Garima; Beaumont, Victor; Varani, Gabriele; Szyperski, Thomas

    2012-12-01

    A newly implemented G-matrix Fourier transform (GFT) (4,3)D HC(C)CH experiment is presented in conjunction with (4,3)D HCCH to efficiently identify (1)H/(13)C sugar spin systems in (13)C labeled nucleic acids. This experiment enables rapid collection of highly resolved relay 4D HC(C)CH spectral information, that is, shift correlations of (13)C-(1)H groups separated by two carbon bonds. For RNA, (4,3)D HC(C)CH takes advantage of the comparably favorable 1'- and 3'-CH signal dispersion for complete spin system identification including 5'-CH. The (4,3)D HC(C)CH/HCCH based strategy is exemplified for the 30-nucleotide 3'-untranslated region of the pre-mRNA of human U1A protein.

  14. Data of 1H/13C NMR spectra and degree of substitution for chitosan alkyl urea

    Directory of Open Access Journals (Sweden)

    Jing Wang

    2016-06-01

    Full Text Available The data shown in this article are related to the subject of an article in Carbohydrate Polymers, entitled “Synthesis and characterization of chitosan alkyl urea” [1]. 1H NMR and 13C NMR spectra of chitosan n-octyl urea, chitosan n-dodecyl urea and chitosan cyclohexyl urea are displayed. The chemical shifts of proton and carbon of glucose skeleton in these chitosan derivatives are designated in detail. Besides, 1H NMR spectra of chitosan cyclopropyl urea, chitosan tert-butyl urea, chitosan phenyl urea and chitosan N,N-diethyl urea and the estimation of the degree of substitution are also presented. The corresponding explanations can be found in the above-mentioned article.

  15. Efficient dipolar double quantum filtering under magic angle spinning without a (1)H decoupling field.

    Science.gov (United States)

    Courtney, Joseph M; Rienstra, Chad M

    2016-08-01

    We present a systematic study of dipolar double quantum (DQ) filtering in (13)C-labeled organic solids over a range of magic-angle spinning rates, using the SPC-n recoupling sequence element with a range of n symmetry values from 3 to 11. We find that efficient recoupling can be achieved for values n⩾7, provided that the (13)C nutation frequency is on the order of 100kHz or greater. The decoupling-field dependence was investigated and explicit heteronuclear decoupling interference conditions identified. The major determinant of DQ filtering efficiency is the decoupling interference between (13)C and (1)H fields. For (13)C nutation frequencies greater than 75kHz, optimal performance is observed without an applied (1)H field. At spinning rates exceeding 20kHz, symmetry conditions as low as n=3 were found to perform adequately.

  16. Exploring the 3-piperidin-4-yl-1H-indole scaffold as a novel antimalarial chemotype.

    Science.gov (United States)

    Santos, Sofia A; Lukens, Amanda K; Coelho, Lis; Nogueira, Fátima; Wirth, Dyann F; Mazitschek, Ralph; Moreira, Rui; Paulo, Alexandra

    2015-09-18

    A series of 3-piperidin-4-yl-1H-indoles with building block diversity was synthesized based on a hit derived from an HTS whole-cell screen against Plasmodium falciparum. Thirty-eight compounds were obtained following a three-step synthetic approach and evaluated for anti-parasitic activity. The SAR shows that 3-piperidin-4-yl-1H-indole is intolerant to most N-piperidinyl modifications. Nevertheless, we were able to identify a new compound (10d) with lead-like properties (MW = 305; cLogP = 2.42), showing antimalarial activity against drug-resistant and sensitive strains (EC50 values ∼ 3 μM), selectivity for malaria parasite and no cross-resistance with chloroquine, thus representing a potential new chemotype for further optimization towards novel and affordable antimalarial drugs.

  17. 4(1H)-Quinolones with liver stage activity against Plasmodium berghei.

    Science.gov (United States)

    Lacrue, Alexis N; Sáenz, Fabián E; Cross, R Matthew; Udenze, Kenneth O; Monastyrskyi, Andrii; Stein, Steven; Mutka, Tina S; Manetsch, Roman; Kyle, Dennis E

    2013-01-01

    With the exception of primaquine, tafenoquine, and atovaquone, there are very few antimalarials that target liver stage parasites. In this study, a transgenic Plasmodium berghei parasite (1052Cl1; PbGFP-Luc(con)) that expresses luciferase was used to assess the anti-liver stage parasite activity of ICI 56,780, a 7-(2-phenoxyethoxy)-4(1H)-quinolone (PEQ), as well as two 3-phenyl-4(1H)-quinolones (P4Q), P4Q-146 and P4Q-158, by using bioluminescent imaging (BLI). Results showed that all of the compounds were active against liver stage parasites; however, ICI 56,780 and P4Q-158 were the most active, with low nanomolar activity in vitro and causal prophylactic activity in vivo. This potent activity makes these compounds ideal candidates for advancement as novel antimalarials.

  18. Surface enhanced Raman spectroscopic studies of 1H-indazole on silver sols.

    Science.gov (United States)

    Pergolese, B; Bigotto, A

    2001-05-01

    The SER spectra of 1H-indazole adsorbed on silver hydrosol were recorded in the 1800-100 cm(-1) and in the 3200-2800 cm(-1) regions. The SERS data were interpreted on the basis of previous vibrational assignments, with the help of the results of DFT calculations carried out using the 6-31G** basis. From the comparison of SER and normal Raman spectra it can be deduced that 1H-indazole is non-dissociatively adsorbed on metal surface and that it interacts with silver sol via nitrogen atoms and ring pi-system. The molecular plane assumes a tilted orientation with respect to the silver surface. The effect of varying the concentration of adsorbate was also evaluated. The observed changes of the relative intensities of some enhanced bands suggest that the molecule assumes a more tilted orientation upon lowering the concentration of the adsorbate.

  19. 1H MAS NMR spectra of hy- droxyl species on diatomite surface

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    High spinning speed 1H magic-angle spinning nuclear magnetic resonance (1H MAS NMR) was used to detect surface hydroxyl groups of diatomite, which include isolated hydroxyl groups and hydrogen-bonded hydroxyl groups, and water adsorbed on diatomite surface that include pore water and hydrogen-bonded water. The corresponding proton chemical shifts of above species are ca. 2.0, 6.0-7.1, 4.9 and 3.0 respectively. Accompanied by thermal treatment temperature ascending, the pore water and hydrogen-bonded water are desorbed successively. As a result, the relative intensities of the peaks assigned to protons of isolat-ed hydroxyl groups and hydrogen-bonded hydroxyl groups increase gradually and reach their maxima at 1000℃. After 1100℃ calcination, the hydroxyl groups that classified to strongly hydrogen-bonded ones and the isolated hydroxyl groups condense basically. But some weakly hydrogen-bonded hydroxyl groups may still persist in the micropores.

  20. Discrimination of sugarcane according to cultivar by 1H NMR and chemometric analyses

    Energy Technology Data Exchange (ETDEWEB)

    Alves Filho, Elenilson G.; Silva, Lorena M.A.; Choze, Rafael; Liao, Luciano M. [Laboratorio de Ressonancia Magnetica Nuclear, Instituto de Quimica, Universidade Federal de Goias (UFG), Goiania, GO (Brazil); Honda, Neli K.; Alcantara, Glaucia B. [Departamento de Quimica, Universidade Federal de Mato Grosso do Sul (UFMS), Campo Grande, MS (Brazil)

    2012-07-01

    Several technologies for the development of new sugarcane cultivars have mainly focused on the increase in productivity and greater disease resistance. Sugarcane cultivars are usually identified by the organography of the leaves and stems, the analysis of peroxidase and esterase isoenzyme activities and the total soluble protein as well as soluble solid content. Nuclear magnetic resonance (NMR) associated with chemometric analysis has proven to be a valuable tool for cultivar assessment. Thus, this article describes the potential of chemometric analysis applied to 1H high resolution magic angle spinning (HRMAS) and NMR in solution for the investigation of sugarcane cultivars. For this purpose, leaves from eight different cultivars of sugarcane were investigated by {sup 1}H NMR spectroscopy in combination with chemometric analysis. The approach shows to be a useful tool for the distinction and classification of different sugarcane cultivars as well as to access the differences on its chemical composition. (author)

  1. (1)H-(13)C NMR-Based Profiling of Biotechnological Starch Utilization.

    Science.gov (United States)

    Sundekilde, Ulrik K; Meier, Sebastian

    2016-10-04

    Starch is used in food- and nonfood applications as a renewable and degradable source of carbon and energy. Insight into the chemical detail of starch degradation remains challenging as the starch constituents amylose and amylopectin are homopolymers. We show that considerable molecular detail of starch fragmentation can be obtained from multivariate analysis of spectral features in optimized (1)H-(13)C NMR spectroscopy of starch fragments to identify relevant features that distinguish processes in starch utilization. As a case study, we compare the profiles of starch fragments in commercial beer samples. Spectroscopic profiles of homooligomeric starch fragments can be excellent indicators of process conditions. In addition, differences in the structure and composition of starch fragments have predictive value for downstream process output such as ethanol production from starch. Thus, high-resolution (1)H-(13)C NMR spectroscopic profiles of homooligomeric fragment mixtures in conjunction with chemometric methods provide a useful addition to the analytical chemistry toolbox of biotechnological starch utilization.

  2. N-Carbethoxy-N′-(3-phenyl-1H-1,2,4-triazol-5-ylthiourea

    Directory of Open Access Journals (Sweden)

    Anton V. Dolzhenko

    2010-02-01

    Full Text Available The title compound {systematic name: ethyl N-[N-(3-phenyl-1H-1,2,4-triazol-5-ylcarbamothioyl]carbamate}, C12H13N5O2S, exists in the 3-phenyl-5-thioureido-1H-1,2,4-triazole tautomeric form stabilized by intramolecular hydrogen bonding between the endocyclic NH H atom and the thioureido S atom. The molecular structure is also stabilized by intramolecular N—H...O=C hydrogen bonds arranged in an S(6 graph-set motif within the carbethoxythiourea moiety. The mean planes of the phenyl and 1,2,4-triazole rings make a dihedral angle of 7.61 (11°. In the crystal, the molecules form two types of inversion dimers. Intermolecular hydrogen bonds are arranged in R22(6 and R22(8 graph-set motifs, together forming a network parallel to (111.

  3. Digital NMR Profiles as Building Blocks: Assembling 1H Fingerprints of Steviol Glycosides

    Science.gov (United States)

    Napolitano, José G.; Simmler, Charlotte; McAlpine, James B.; Lankin, David C.; Chen, Shao-Nong; Pauli, Guido F.

    2015-01-01

    This report describes a fragment-based approach to the examination of congeneric organic compounds by NMR spectroscopy. The method combines the classic interpretation of 1D- and 2D-NMR data sets with contemporary computer-assisted NMR analysis. Characteristic NMR profiles of key structural motifs were generated by 1H iterative full spin analysis and then joined together as building blocks to recreate the 1H NMR spectra of increasingly complex molecules. To illustrate the methodology described, a comprehensive analysis of steviol (1), seven steviol glycosides (2–8) and two structurally related isosteviol compounds (9, 10) was carried out. The study also assessed the potential impact of this method on relevant aspects of natural product research including structural verification, chemical dereplication, and mixture analysis. PMID:25714117

  4. Microwave-enhanced transition metal-catalyzed decoration of 2(1H)-pyrazinone scaffolds.

    Science.gov (United States)

    Kaval, Nadya; Bisztray, Katalin; Dehaen, Wim; Kappe, C Oliver; Van der Eycken, Erik

    2003-01-01

    The 2(1H)-pyrazinones have been demonstrated to be versatile building blocks for the synthesis of biologically active compounds. Here, an efficient method is described for the decoration of these interesting scaffolds. Microwave-assisted palladium catalyzed reactions allow the easy introduction of different substituents at the C3- and even at the rather unreactive C5-position of the pyrazinones. Stille, Suzuki, Heck, Sonogashira reactions, in addition to reductive dechlorinations, and cyanation reactions are investigated.

  5. Multicomponent assembly of diverse pyrazin-2(1H)-one chemotypes.

    Science.gov (United States)

    Azuaje, Jhonny; El Maatougui, Abdelaziz; Pérez-Rubio, José M; Coelho, Alberto; Fernández, Franco; Sotelo, Eddy

    2013-05-03

    An expedient and concise Ugi-based approach for the rapid assembly of pyrazin-2(1H)-one-based frameworks has been developed. This convergent approach encompasses skeletal, functional and stereochemical diversity, exhibiting an unusually high bond-forming efficiency as well as high structure and step economies. The method involves the use of readily available commercial reagents and is an example of the reconciliation of structural complexity with operational simplicity in a time- and cost-effective manner.

  6. Synthesis and antileishmanial activity of new 1-Aryl-1H-Pyrazole-4- carboximidamides derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Mauricio S. dos; Gomes, Adriana O.; Bernardino, Alice M.R.; Souza, Marcos C. de, E-mail: alicerolim@globo.co [Universidade Federal Fluminense (UFF), Niteroi, RJ (Brazil). Programa de Pos-Graduacao em Quimica Organica; Khan, Misbahul A. [The Islamia University of Bahawalpur (Pakistan). Chemistry Dept.; Brito, Monique A. de [Universidade Federal Fluminense (UFF), Niteroi, RJ (Brazil). Fac. de Farmacia. Lab. de Quimica Medicinal Computacional; Castro, Helena C.; Abreu, Paula A. [Universidade Federal Fluminense (LABioMol/GCM/UFF), Niteroi, RJ (Brazil). Inst. de Biologia. Lab. de Antibioticos, Bioquimica e Modelagem Molecular; Rodrigues, Carlos R. [Universidade Federal do Rio de Janeiro (ModMol/UFRJ), RJ (Brazil). Fac. de Farmacia. Lab. de Modelagem Molecular e QSAR; Leo, Rosa M.M. de; Leon, Leonor L.; Canto-Cavalheiro, Marilene M. [Fundacao Oswaldo Cruz (IOC/FIOCRUZ), Rio de Janeiro, RJ (Brazil). Instituto Oswaldo Cruz. Lab. de Bioquimica de Tripanosomatideos

    2011-07-01

    Chemotherapy for leishmaniasis, diseases caused by protozoa of the genus Leishmania, remains inefficient in several treatments. So there is a need to search for new drugs. In this work, we have synthesized 1-aryl-1H-pyrazole-4-carboximidamides derivatives and evaluated antileishmanial activities in vitro, as well as cytotoxic effects. Structure-activity relationship (SAR) studies were carried out with all the compounds of the series. Compound 2 showed an activity profile that can be improved through medicinal chemistry strategies. (author)

  7. One-Pot Synthesis of Novel 2,3-Dihydro-1H-indazoles

    Directory of Open Access Journals (Sweden)

    Antonio J. Lepore

    2011-11-01

    Full Text Available A copper(I-mediated one-pot synthesis of 2,3-dihydro-1H-indazole heterocycles has been developed. This synthetic route provides the desired indazoles in moderate to good yields (55%–72% which are substantially better than those achievable with an alternative two-step reaction sequence. The reaction is tolerant of functionality on the aromatic ring.

  8. Search for the Halo Effect in the 1H(6He, 6Li)n Peaction

    Institute of Scientific and Technical Information of China (English)

    李志宏; 柳卫平; 白希祥; 王友宝; 连钢; 李志常; 申庆彪; 林承键; 曾晟; 符长波

    2002-01-01

    The angular distributions of the charge exchange reaction 1 H(6He, 6Li)n were measured in reverse kinematics with a secondary 6He beam at the energy of4.17 AMeV. The data were analysed in the context ora microscopic calculation. It is shown that both the ground state of6He and the second excited state of6Li (3.563 MeV, 0+) have a halo structure.

  9. 1H-MRS metabolites in adults with Down syndrome: Effects of dementia

    Directory of Open Access Journals (Sweden)

    A.-L. Lin

    2016-01-01

    Full Text Available To determine if proton magnetic resonance spectroscopy (1H-MRS detect differences in dementia status in adults with Down syndrome (DS, we used 1H-MRS to measure neuronal and glial metabolites in the posterior cingulate cortex in 22 adults with DS and in 15 age- and gender-matched healthy controls. We evaluated associations between 1H-MRS results and cognition among DS participants. Neuronal biomarkers, including N-acetylaspartate (NAA and glutamate-glutamine complex (Glx, were significantly lower in DS patients with Alzheimer's should probably be changed to Alzheimer (without ' or s through ms as per the new naming standard disease (DSAD when compared to non-demented DS (DS and healthy controls (CTL. Neuronal biomarkers therefore appear to reflect dementia status in DS. In contrast, all DS participants had significantly higher myo-inositol (MI, a putative glial biomarker, compared to CTL. Our data indicate that there may be an overall higher glial inflammatory component in DS compared to CTL prior to and possibly independent of developing dementia. When computing the NAA to MI ratio, we found that presence or absence of dementia could be distinguished in DS. NAA, Glx, and NAA/MI in all DS participants were correlated with scores from the Brief Praxis Test and the Severe Impairment Battery. 1H-MRS may be a useful diagnostic tool in future longitudinal studies to measure AD progression in persons with DS. In particular, NAA and the NAA/MI ratio is sensitive to the functional status of adults with DS, including prior to dementia.

  10. PepsNMR for the 1H-NMR metabolomic data pre-processing

    OpenAIRE

    Martin, Manon; Legat, Benoît; Leenders, Justine; Vanwinsberghe, Julien; Rousseau, Réjane; Boulanger, Bruno; Eilers, Paul H. C.; De Tullio, Pascal; Govaerts, Bernadette

    2017-01-01

    In the analysis of complex biological samples, control over experimental design and data acquisition procedures cannot ensure alone well-conditioned 1H-NMR spectra with maximal information recovery for data analysis. A third major element affects the accuracy and robustness of the results: the data pre-processing/pre-treatment for which not enough attention is usually devoted, in particular in the metabolomic studies. The usual approach is to use proprietary software provided by the analytica...

  11. (E-1-Diphenylmethylidene-2-[(1H-indol-3-ylmethylidene]hydrazine

    Directory of Open Access Journals (Sweden)

    R. Archana

    2010-07-01

    Full Text Available In the title compound, C22H17N3, the 1H-indole unit is essentially planar, with a dihedral angle of 0.95 (10° between the pyrrole ring and the fused benzene ring. The dihedral angle between the two phenyl rings is 65.09 (10°. In the crystal, an intermolecular N—H...N hydrogen bond forms an infinite chain in the b-axis direction.

  12. MR diffusion imaging and 1H spectroscopy in a child with medulloblastoma: A case report

    Energy Technology Data Exchange (ETDEWEB)

    Wilke, M. [Max-Planck-Institute of Psychiatry, Muenchen (Germany). NMR Study Group; Eidenschink, A.; Mueller-Weihrich, S. [Technical Univ. of Muenchen, (Germany). Childrens' Hospital; Auer, D.P. [Max-Planck-Institute of Psychiatry, Muenchen (Germany). NMR Study Group

    2000-01-01

    We report on a child with a metastasising medulloblastoma which was assessed by MR diffusion imaging and 1H MR spectroscopy (MRS). Reduced mean apparent diffusion coefficients and a high amount of taurine could be demonstrated. This is the first reported case of high taurine in medulloblastoma in vivo and confirms earlier in vitro findings. It is suggested that the changes on diffusion imaging, possibly reflecting the small-cell histology of the tumour and high taurine in MRS, are indicative of medulloblastoma.

  13. 1H-13C NMR-based profiling of biotechnological starch utilization

    DEFF Research Database (Denmark)

    Sundekilde, Ulrik K.; Meier, Sebastian

    2016-01-01

    Starch is used in food-and non-food applications as a renewable and degradable source of carbon and energy. Insight into the chemical detail of starch degradation remains challenging as the starch constituents amylose and amylopectin are homopolymers. We show that considerable molecular detail......-resolution 1H-13C NMR spectroscopic profiles of homooligomeric fragment mixtures in conjunction with chemometric methods provide a useful addition to the analytical chemistry toolbox of biotechnologi-cal starch utilization....

  14. Authentication of beef versus horse meat using 60 MHz 1H NMR spectroscopy

    OpenAIRE

    Jakes, W.; Gerdova, A.; Defernez, M.; Watson, A. D.; McCallum, C.; Limer, E.; Colquhoun, I. J.; Williamson, D. C.; Kemsley, E.K.

    2015-01-01

    This work reports a candidate screening protocol to distinguish beef from horse meat based upon comparison of triglyceride signatures obtained by 60 MHz 1H NMR spectroscopy. Using a simple chloroform-based extraction, we obtained classic low-field triglyceride spectra from typically a 10 min acquisition time. Peak integration was sufficient to differentiate samples of fresh beef (76 extractions) and horse (62 extractions) using Naïve Bayes classification. Principal component analysis gave a t...

  15. The neurochemical profile quantified by in vivo(1)H NMR spectroscopy

    OpenAIRE

    João M N Duarte; Lei, Hongxia; Mlynárik, Vladimír; Gruetter, Rolf

    2012-01-01

    Proton NMR spectroscopy is emerging from translational and preclinical neuroscience research as an important tool for evidence based diagnosis and therapy monitoring. It provides biomarkers that offer fingerprints of neurological disorders even in cases where a lesion is not yet observed in MR images. The collection of molecules used as cerebral biomarkers that are detectable by (1)H NMR spectroscopy define the so-called "neurochemical profile". The non-invasive quality of this technique make...

  16. Synthesis and Biological Activity of 3-Methyl-1H-pyrazole-4-carboxylic Ester Derivatives

    Institute of Scientific and Technical Information of China (English)

    ZHAO Wei-Guang; LI Zheng-Ming; YUAN Ping-Wei; WANG Wen-Yan

    2001-01-01

    In search of novel pyrazole derivatives with bioactivity,a se-ries of 3-methyl- 1H-pyrazole-4-caboxylic ester derivatives were synthesized via α-oxoketene dithioacetals as starting ma-terial.The structures of al1 compounds prepared were con-firmed by 1HNMR, IR, MS and elemental analyses.Prelimi-nary bioassays indicated that some compounds showed fungici-dal activity against wheat rust,phoma asparagi and antiviral activity against TMV.

  17. Characterisation of human embryonic stem cells conditioning media by 1H-nuclear magnetic resonance spectroscopy.

    Directory of Open Access Journals (Sweden)

    David A MacIntyre

    Full Text Available BACKGROUND: Cell culture media conditioned by human foreskin fibroblasts (HFFs provide a complex supplement of protein and metabolic factors that support in vitro proliferation of human embryonic stem cells (hESCs. However, the conditioning process is variable with different media batches often exhibiting differing capacities to maintain hESCs in culture. While recent studies have examined the protein complement of conditioned culture media, detailed information regarding the metabolic component of this media is lacking. METHODOLOGY/PRINCIPAL FINDINGS: Using a (1H-Nuclear Magnetic Resonance ((1H-NMR metabonomics approach, 32 metabolites and small compounds were identified and quantified in media conditioned by passage 11 HFFs (CMp11. A number of metabolites were secreted by HFFs with significantly higher concentration of lactate, alanine, and formate detected in CMp11 compared to non-conditioned media. In contrast, levels of tryptophan, folate and niacinamide were depleted in CMp11 indicating the utilisation of these metabolites by HFFs. Multivariate statistical analysis of the (1H-NMR data revealed marked age-related differences in the metabolic profile of CMp11 collected from HFFs every 24 h over 72 h. Additionally, the metabolic profile of CMp11 was altered following freezing at -20°C for 2 weeks. CM derived from passage 18 HFFs (CMp18 was found to be ineffective at supporting hESCs in an undifferentiated state beyond 5 days culture. Multivariate statistical comparison of CMp11 and CMp18 metabolic profiles enabled rapid and clear discrimination between the two media with CMp18 containing lower concentrations of lactate and alanine as well as higher concentrations of glucose and glutamine. CONCLUSIONS/SIGNIFICANCE: (1H-NMR-based metabonomics offers a rapid and accurate method of characterising hESC conditioning media and is a valuable tool for monitoring, controlling and optimising hESC culture media preparation.

  18. Quantitative analysis of amygdalin and prunasin in Prunus serotina Ehrh. using (1) H-NMR spectroscopy.

    Science.gov (United States)

    Santos Pimenta, Lúcia P; Schilthuizen, Menno; Verpoorte, Robert; Choi, Young Hae

    2014-01-01

    Prunus serotina is native to North America but has been invasively introduced in Europe since the seventeenth century. This plant contains cyanogenic glycosides that are believed to be related to its success as an invasive plant. For these compounds, chromatographic- or spectrometric-based (targeting on HCN hydrolysis) methods of analysis have been employed so far. However, the conventional methods require tedious preparation steps and a long measuring time. To develop a fast and simple method to quantify the cyanogenic glycosides, amygdalin and prunasin in dried Prunus serotina leaves without any pre-purification steps using (1) H-NMR spectroscopy. Extracts of Prunus serotina leaves using CH3 OH-d4 and KH2 PO4 buffer in D2 O (1:1) were quantitatively analysed for amygdalin and prunasin using (1) H-NMR spectroscopy. Different internal standards were evaluated for accuracy and stability. The purity of quantitated (1) H-NMR signals was evaluated using several two-dimensional NMR experiments. Trimethylsilylpropionic acid sodium salt-d4 proved most suitable as the internal standard for quantitative (1) H-NMR analysis. Two-dimensional J-resolved NMR was shown to be a useful tool to confirm the structures and to check for possible signal overlapping with the target signals for the quantitation. Twenty-two samples of P. serotina were subsequently quantitatively analysed for the cyanogenic glycosides prunasin and amygdalin. The NMR method offers a fast, high-throughput analysis of cyanogenic glycosides in dried leaves permitting simultaneous quantification and identification of prunasin and amygdalin in Prunus serotina. Copyright © 2013 John Wiley & Sons, Ltd.

  19. Anti-Toxoplasma Activity of 2-(Naphthalene-2-γlthiol-1H Indole.

    Directory of Open Access Journals (Sweden)

    Qasem Asgari

    2015-06-01

    Full Text Available This study was undertaken to evaluate the viability, infectivity and immunity of Toxoplasma gondii tachyzoites exposed to 2-(naphthalene-2-ylthio-1H-indole.Tachyzoites of RH strain were incubated in various concentrations of 2-(naphthalene-2-ylthio-1H-indole (25-800 μM for 1.5 hours. Then, they were stained by PI and analyzed by Fluorescence-activated cell sorting (FACS. To evaluate the infectivity, the tachyzoites exposed to the different concentrations of the compound were inoculated to 10 BALB/c mice groups. For Control, parasites exposed to DMSO (0.2% v/v were also intraperitoneally inoculated into two groups of mice. The immunity of the exposed tachyzoites was evaluated by inoculation of the naïve parasite to the survived mice.The LD50 of 2-(naphthalene-2-ylthio-1H-indole was 57 μmol. The longevity of mice was dose dependent. Five mice out of group 400μmol and 3 out of group 800μmol showed immunization to the parasite.Our findings demonstrated the toxoplasmocidal activity of the compound. The presence of a well-organized transporter mechanism for indole compounds within the parasite in conjunction with several effective mechanisms of these compounds on Toxoplasma viability would open a window for production of new drugs and vaccines.

  20. Stereoelectronic effects on 1H nuclear magnetic resonance chemical shifts in methoxybenzenes

    DEFF Research Database (Denmark)

    Lambert, Maja; Olsen, Lars; Jaroszewski, Jerzy W

    2006-01-01

    the Ar-OCH3 torsion out of the ring plane, resulting in large stereoelectronic effects on the chemical shift of Hpara. Conformational searches and geometry optimizations for 3-16 at the B3LYP/6-31G** level, followed by B3LYP/6-311++G(2d,2p) calculations for all low-energy conformers, gave excellent......Investigation of all O-methyl ethers of 1,2,3-benzenetriol and 4-methyl-1,2,3-benzenetriol (3-16) by 1H NMR spectroscopy and density-functional calculations disclosed practically useful conformational effects on 1H NMR chemical shifts in the aromatic ring. While the conversion of phenol (2......) to anisole (1) causes only small positive changes of 1H NMR chemical shifts (Delta delta Hmeta > Hpara, the experimental O-methylation induced shifts in ortho-disubstituted phenols are largest for Hpara, Delta delta equals; 0.19 +/- 0.02 ppm (n = 11...

  1. Sudan dyes in adulterated saffron (Crocus sativus L.): Identification and quantification by (1)H NMR.

    Science.gov (United States)

    Petrakis, Eleftherios A; Cagliani, Laura R; Tarantilis, Petros A; Polissiou, Moschos G; Consonni, Roberto

    2017-02-15

    Saffron, the dried red stigmas of Crocus sativus L., is considered as one of the most expensive spices worldwide, and as such, it is prone to adulteration. This study introduces an NMR-based approach to identify and determine the adulteration of saffron with Sudan I-IV dyes. A complete (1)H and (13)C resonance assignment for Sudan I-IV, achieved by two-dimensional homonuclear and heteronuclear NMR experiments, is reported for the first time. Specific different proton signals for the identification of each Sudan dye in adulterated saffron can be utilised for quantitative (1)H NMR (qHNMR), a well-established method for quantitative analysis. The quantification of Sudan III, as a paradigm, was performed in varying levels (0.14-7.1g/kg) by considering the NMR signal occurring at 8.064ppm. The high linearity, accuracy and rapidity of investigation enable high resolution (1)H NMR spectroscopy to be used for evaluation of saffron adulteration with Sudan dyes.

  2. Theoretical study of an energetic material di-1H-1,3,4-triazole derivatives

    Directory of Open Access Journals (Sweden)

    Hua Zhou

    2014-12-01

    Full Text Available Computations by density functional theory (DFT method are performed on a series of di-1H-1,3,4-triazole derivatives with different substituents and linkages. The heat of formation (HOF is predicted by the designed isodesmic reactions. The predicted results reveal that –N3 and –NN– groups are effective structural units for increasing the HOF values of the di-1H-1,3,4-triazole derivatives. The HOMO–LUMO gap is affected by the substituents and linkage groups. Detonation performance is evaluated using the Kamlet–Jacobs approach based on the calculated density and HOF. The results indicate that –NO2, –NF2, –NH–, –NH–NH– and –NN– groups are helpful for enhancing the detonation properties of di-1H-1,3,4-triazole derivatives. The bond dissociation energy and bond order of the weakest bonds are analyzed to investigate their stability. It is observed that the –CH2–, –CH2–CH2– and –CHCH– groups are effective structural units for improving the stabilities of these derivatives. Considering the detonation performance and the stability, five compounds are screened as the potential candidates for high energy density materials.

  3. Theoretical study of an energetic material di-1H-1,3,4-triazole derivatives

    Institute of Scientific and Technical Information of China (English)

    Hua ZHOU; Zhong-liang MA; Jian-long WANG; Dong WANG

    2014-01-01

    Computations by density functional theory (DFT) method are performed on a series of di-1H-1,3,4-triazole derivatives with different sub-stituents and linkages. The heat of formation (HOF ) is predicted by the designed isodesmic reactions. The predicted results reveal that eN3 and eN]Ne groups are effective structural units for increasing the HOF values of the di-1H-1,3,4-triazole derivatives. The HOMOeLUMO gap is affected by the substituents and linkage groups. Detonation performance is evaluated using the KamleteJacobs approach based on the calculated density and HOF. The results indicate that eNO2, eNF2, eNHe, eNHeNHe and eN]Ne groups are helpful for enhancing the detonation properties of di-1H-1,3,4-triazole derivatives. The bond dissociation energy and bond order of the weakest bonds are analyzed to investigate their stability. It is observed that the eCH2e, eCH2eCH2e and eCH]CHe groups are effective structural units for improving the stabilities of these derivatives. Considering the detonation performance and the stability, five compounds are screened as the potential candidates for high energy density materials.

  4. Discriminating binding and positioning of amphiphiles to lipid bilayers by {sup 1}H NMR

    Energy Technology Data Exchange (ETDEWEB)

    Evanics, F. [Department of Chemistry, University of Toronto, UTM, 3359 Mississauga Rd. North Mississauga, Ont., L5L 1C6 (Canada); Prosser, R.S. [Department of Chemistry, University of Toronto, UTM, 3359 Mississauga Rd. North Mississauga, Ont., L5L 1C6 (Canada)]. E-mail: sprosser@utm.utoronto.ca

    2005-04-04

    The binding and positioning in lipid bilayers of three well-known drugs--imipramine, nicotine, and caffeine--have been studied using {sup 1}H NMR. The membrane model system consisted of 'fast-tumbling' lipid bicelles, in which a bilayered lipid domain, composed of the unsaturated lipid, 1,2-dimyristelaidoyl-sn-glycero-3-phosphocholine (DMLPC) was surrounded by a rim of deuterated detergent-like lipids, consisting of 1,2-dihexanoyl-sn-glycero-3-phosphocholine (DHPC-d22). Binding and immersion depth information was obtained by three experiments. (1) {sup 1}H chemical shift perturbations, upon transfer of the amphiphiles from water to a bicelle mixture, were used to estimate regions of the amphiphiles that interact with the membrane. (2) Water contact to resolvable protons was measured through a Nuclear Overhauser Effect (NOE) between water and resolvable drug and lipid resonances. In the case of both lipids and membrane bound drugs, positive NOEs with large cross-relaxation rates were measured for most resonances originating from the membrane hydrophilic region, while negative NOEs were observed predominantly to resonances in the hydrophobic region of the membrane. (3) {sup 1}H NMR measurements of oxygen-induced (paramagnetic) spin-lattice relaxation rates, which are known to increase with membrane immersion depth, were used to corroborate conclusions based on chemical shift perturbations and water-ligand NOEs.

  5. Improving Assessment of Lipoprotein Profile in Type 1 Diabetes by 1H NMR Spectroscopy

    Science.gov (United States)

    Brugnara, Laura; Mallol, Roger; Ribalta, Josep; Vinaixa, Maria; Murillo, Serafín; Casserras, Teresa; Guardiola, Montse; Vallvé, Joan Carles; Kalko, Susana G.; Correig, Xavier; Novials, Anna

    2015-01-01

    Patients with type 1 diabetes (T1D) present increased risk of cardiovascular disease (CVD). The aim of this study is to improve the assessment of lipoprotein profile in patients with T1D by using a robust developed method 1H nuclear magnetic resonance spectroscopy (1H NMR), for further correlation with clinical factors associated to CVD. Thirty patients with T1D and 30 non-diabetes control (CT) subjects, matched for gender, age, body composition (DXA, BMI, waist/hip ratio), regular physical activity levels and cardiorespiratory capacity (VO2peak), were analyzed. Dietary records and routine lipids were assessed. Serum lipoprotein particle subfractions, particle sizes, and cholesterol and triglycerides subfractions were analyzed by 1H NMR. It was evidenced that subjects with T1D presented lower concentrations of small LDL cholesterol, medium VLDL particles, large VLDL triglycerides, and total triglycerides as compared to CT subjects. Women with T1D presented a positive association with HDL size (plipoprotein profile as compared to control counterparts. In addition, slight alterations in BMI and/or body fat composition showed to be relevant to provoking alterations in lipoproteins profiles. Finally, body fat composition appears to be a determinant for cardioprotector lipoprotein profile. PMID:26317989

  6. Permissivity of the NCI-60 cancer cell lines to oncolytic Vaccinia Virus GLV-1h68

    Directory of Open Access Journals (Sweden)

    Bedognetti Davide

    2011-10-01

    Full Text Available Abstract Background Oncolytic viral therapy represents an alternative therapeutic strategy for the treatment of cancer. We previously described GLV-1h68, a modified Vaccinia Virus with exclusive tropism for tumor cells, and we observed a cell line-specific relationship between the ability of GLV-1h68 to replicate in vitro and its ability to colonize and eliminate tumor in vivo. Methods In the current study we surveyed the in vitro permissivity to GLV-1h68 replication of the NCI-60 panel of cell lines. Selected cell lines were also tested for permissivity to another Vaccinia Virus and a vesicular stomatitis virus (VSV strain. In order to identify correlates of permissity to viral infection, we measured transcriptional profiles of the cell lines prior infection. Results We observed highly heterogeneous permissivity to VACV infection amongst the cell lines. The heterogeneity of permissivity was independent of tissue with the exception of B cell derivation. Cell lines were also tested for permissivity to another Vaccinia Virus and a vesicular stomatitis virus (VSV strain and a significant correlation was found suggesting a common permissive phenotype. While no clear transcriptional pattern could be identified as predictor of permissivity to infection, some associations were observed suggesting multifactorial basis permissivity to viral infection. Conclusions Our findings have implications for the design of oncolytic therapies for cancer and offer insights into the nature of permissivity of tumor cells to viral infection.

  7. An elevated 1-h post- load glucose level during the oral glucose tolerance test detects prediabetes.

    Science.gov (United States)

    Buysschaert, Martin; Bergman, Michael; Yanogo, Donald; Jagannathan, Ram; Buysschaert, Benoit; Preumont, Vanessa

    The objective of the study was to compare the diagnosis of dysglycemic states by conventional oral glucose tolerance test (OGTT) criteria (fasting and 2-h plasma glucose) with the 1-h post-load plasma glucose level. 34 individuals (mean age: 55±13years; BMI: 27.7±6.3kg/m(2)) at risk for prediabetes were administered a 75g OGTT. Individuals with normal glucose tolerance (NGT) or prediabetes were identified according to fasting and/or 2-h plasma glucose (PG) concentrations. Subsequently, subjects were divided in 2 groups: group 1 (n=21) with a 1-h PGh PG≥155mg/dl. HOMA was performed to assess β-cell function and insulin sensitivity. NGT or prediabetes based on conventional criteria correlated with the 1-h PGh PG≥155mg/dl was associated with higher HbA1c levels (6.1±0.5 vs. 5.5±0.3%, ph PGh post-load plasma glucose value ≥155mg/dl is strongly associated with conventional criteria for (pre)diabetes and alterations of β-cell function. Copyright © 2016 Diabetes India. Published by Elsevier Ltd. All rights reserved.

  8. Synthesis and antiproliferative activity of 3-amino-N-phenyl-1H-indazole-1-carboxamides.

    Science.gov (United States)

    Raffa, Demetrio; Maggio, Benedetta; Cascioferro, Stella; Raimondi, Maria Valeria; Schillaci, Domenico; Gallo, Giorgio; Daidone, Giuseppe; Plescia, Salvatore; Meneghetti, Fiorella; Bombieri, Gabriella; Di Cristina, Antonietta; Pipitone, Rosaria M; Grimaudo, Stefania; Tolomeo, Manlio

    2009-01-01

    A series of new 3-amino-N-phenyl-1H-indazole-1-carboxamides 10 have been prepared from commercially available phenyl isocyanate precursors 8 and 3-aminoindazole 9. Some of the synthesized compounds were evaluated for their in vitro antineoplastic activity against 60 human cell lines derived from seven clinically isolated cancer types (lung, colon, melanoma, renal, ovarian, brain, and leukemia) according to the NCI standard protocol. The test results indicated that 3-amino-1H-indazole-1-carboxamides 10 were endowed with an interesting antiproliferative activity. The most active compounds of this series, 10d,e, were able to inhibit cell growth of many neoplastic cell lines at concentrations lower than 1 microM (0.0153 microM in SR leukemia) causing a block in G0-G1 phase of cell cycle. Analysis of pRb expression showed that these two compounds increased the ratio between underphosphorylated pRb and total pRb. The X-ray structure of 10w, confirmed the 3-amino-N-phenyl-1H-indazole-1-carboxamide structure of compounds 10.

  9. {sup 1}H NMR spectroscopic studies establish that heparanase is a retaining glycosidase

    Energy Technology Data Exchange (ETDEWEB)

    Wilson, Jennifer C., E-mail: jennifer.wilson@griffith.edu.au [Institute for Glycomics, Griffith University Gold Coast Campus, QLD 4222 (Australia); Laloo, Andrew Elohim [School of Chemistry and Molecular Biosciences, The University of Queensland, Brisbane, QLD 4072 (Australia); Singh, Sanjesh [Institute for Glycomics, Griffith University Gold Coast Campus, QLD 4222 (Australia); Ferro, Vito, E-mail: v.ferro@uq.edu.au [School of Chemistry and Molecular Biosciences, The University of Queensland, Brisbane, QLD 4072 (Australia)

    2014-01-03

    Highlights: •{sup 1}H and {sup 13}C NMR chemical shifts of fondaparinux were fully assigned by 1D and 2D NMR techniques. •Hydrolysis of fondaparinux by heparanase was monitored by {sup 1}H NMR spectroscopy. •Heparanase is established to be a retaining glycosidase. -- Abstract: Heparanase is an endo-β-glucuronidase that cleaves heparan sulfate side chains of proteoglycans in basement membranes and the extracellular matrix (ECM). Heparanase is implicated in several diverse pathological processes associated with ECM degradation such as metastasis, inflammation and angiogenesis and is thus an important target for anti-cancer and anti-inflammatory drug discovery. Heparanase has been classed as belonging to the clan A glycoside hydrolase family 79 based on sequence analysis, secondary structure predictions and mutagenic analysis, and thus it has been inferred that it is a retaining glycosidase. However, there has been no direct experimental evidence to support this conclusion. Herein we describe {sup 1}H NMR spectroscopic studies of the hydrolysis of the pentasaccharide substrate fondaparinux by heparanase, and provide conclusive evidence that heparanase hydrolyses its substrate with retention of configuration and is thus established as a retaining glycosidase. Knowledge of the mechanism of hydrolysis may have implications for future design of inhibitors for this important drug target.

  10. Artefacts in 1H NMR-based metabolomic studies on cell cultures.

    Science.gov (United States)

    Madhu, Basetti; Dadulescu, Madalina; Griffiths, John

    2015-04-01

    Metabolomic studies on cultured cells involve assays of cell extracts and culture medium, both of which are often performed by (1)H NMR. Cell culture is nowadays performed in plastic dishes or flasks, and the extraction of metabolites from the cells is typically performed with perchloric acid, methanol-chloroform, or acetonitrile, ideally while the cells are still adherent to the culture dish. We conducted this investigation to identify contaminants from cell culture plasticware in metabolomic studies. Human diploid fibroblasts (IMR90) (n = 6), HeLa cells (n = 6), and transformed astrocytes with HIF-1 knockout (Astro-KO) (n = 6) were cultured. Cells were seeded in 100 mm Petri dishes with 10 ml complete growth medium (Dulbecco's minimum essential medium) containing 10 % foetal bovine serum (FBS). Cell cultures were incubated at 37 °C in 5 % CO2 for approximately 3 days. Metabolites were extracted by use of a perchloric acid procedure. (1)H NMR spectroscopy was used for metabolite analysis. "Null sample" (i.e. cell-free) experiments were performed by either rinsing dishes with medium or incubating the medium in Petri dishes from five different manufacturers for 72 h and then by performing a dummy "extraction" of each Petri dish by the perchloric acid, methanol-chloroform, or acetonitrile procedures. Principal components analysis was used for classification of samples and to determine the contaminants arising from plasticware. We found that even brief rinsing of cell culture plasticware with culture medium elutes artefactual chemicals, the (1)H NMR signals of which could confound assays of acetate, succinate, and glycolate. Incubation of culture medium in cell-culture dishes for 72 h (as in a typical cell-culture experiment) followed by perchloric extraction in the dishes enhanced elution of the artefacts. These artefacts were present, but somewhat less pronounced, in the (1)H NMR spectra of null samples extracted with methanol and acetonitrile. Ethanol, lactate

  11. New pseudan (2-alkyl-4(1H)-quinolinone) alkaloids from Boronia ternata var. elongata and Boronia alulata (Rutaceae).

    Science.gov (United States)

    Agier, Catherine; Bury, Michele; Aquette, Jacqueline; Hocquemiller, Reynald; Waterman, Peter G

    2007-07-10

    The aerial parts of Boronia ternata var. elongata from western Australia has yielded three new 2-acyl-4(1H)-quinolinone alkaloids, characterised as 2-n-pentyl-4(1H)-quinolinone, 1-methyl-2-n-pentyl-4(1H)-quinolinone and 1-methyl-2-(1 xi-methyl)-propyl-4(1H)-quinolinone, as well as known alkaloids of this class and a furoquinoline alkaloid. Boronia alulata, from northeast Queensland, also yielded 2-n-pentyl-4(1H)-quinolinone together with the known 2-n-propyl-4(1H)-quinolinone. Both species are assigned to Boronia section Valvatae which, alone among the sections of Boronia, appears to be characterised by the presence of alkaloids.

  12. Experimental design and environmental parameters affect Rhodospirillum rubrum S1H response to space flight.

    Science.gov (United States)

    Mastroleo, Felice; Van Houdt, Rob; Leroy, Baptiste; Benotmane, M Abderrafi; Janssen, Ann; Mergeay, Max; Vanhavere, Filip; Hendrickx, Larissa; Wattiez, Ruddy; Leys, Natalie

    2009-12-01

    In view of long-haul space exploration missions, the European Space Agency initiated the Micro-Ecological Life Support System Alternative (MELiSSA) project targeting the total recycling of organic waste produced by the astronauts into oxygen, water and food using a loop of bacterial and higher plant bioreactors. In that purpose, the alpha-proteobacterium, Rhodospirillum rubrum S1H, was sent twice to the International Space Station and was analyzed post-flight using a newly developed R. rubrum whole genome oligonucleotide microarray and high throughput gel-free proteomics with Isotope-Coded Protein Label technology. Moreover, in an effort to identify a specific response of R. rubrum S1H to space flight, simulation of microgravity and space-ionizing radiation were performed on Earth under identical culture set-up and growth conditions as encountered during the actual space journeys. Transcriptomic and proteomic data were integrated and permitted to put forward the importance of medium composition and culture set-up on the response of the bacterium to space flight-related environmental conditions. In addition, we showed for the first time that a low dose of ionizing radiation (2 mGy) can induce a significant response at the transcriptomic level, although no change in cell viability and only a few significant differentially expressed proteins were observed. From the MELiSSA perspective, we could argue the effect of microgravity to be minimized, whereas R. rubrum S1H could be more sensitive to ionizing radiation during long-term space exploration mission.

  13. Identification of fucans from four species of sea cucumber by high temperature 1H NMR

    Science.gov (United States)

    Wu, Nian; Chen, Shiguo; Ye, Xingqian; Li, Guoyun; Yin, Li'ang; Xue, Changhu

    2014-10-01

    Acidic polysaccharide, which has various biological activities, is one of the most important components of sea cucumber. In the present study, crude polysaccharide was extracted from four species of sea cucumber from three different geographical zones, Pearsonothuria graeffei ( Pg) from Indo-Pacific, Holothuria vagabunda ( Hv) from Norwegian Coast, Stichopus tremulu ( St) from Western Indian Ocean, and Isostichopus badionotu ( Ib) from Western Atlantic. The polysaccharide extract was separated and purified with a cellulose DEAE anion-exchange column to obtain corresponding sea cucumber fucans (SC-Fucs). The chemical property of these SC-Fucs, including molecular weight, monosaccharide composition and sulfate content, was determined. Their structure was compared simply with fourier infrared spectrum analyzer and identified with high temperature 1H nuclear magnetic resonance spectrum analyzer (NMR) and room temperature 13C NMR. The results indicated that Fuc- Pg obtained from the torrid zone mainly contained 2,4-O-disulfated and non-sulfated fucose residue, whereas Fuc- Ib from the temperate zone contained non-, 2-O- and 2,4-O-disulfated fucose residue; Fuc- St from the frigid zone and Fuc- Hv from the torrid zone contained mainly non-sulfated fucose residue. The proton of SC-Fucs was better resolved via high temperature 1H NMR than via room temperature 1H NMR. The fingerprint of sea cucumber in different sea regions was established based on the index of anomer hydrogen signal in SC-Fucs. Further work will help to understand whether there exists a close relationship between the geographical area of sea cucumber and the sulfation pattern of SC-Fucs.

  14. (1)H-(2)H cross-polarization NMR in fast spinning solids by adiabatic sweeps.

    Science.gov (United States)

    Wi, Sungsool; Schurko, Robert; Frydman, Lucio

    2017-03-14

    Cross-polarization (CP) experiments employing frequency-swept radiofrequency (rf) pulses have been successfully used in static spin systems for obtaining broadband signal enhancements. These experiments have been recently extended to heteronuclear I, S = spin-1/2 nuclides under magic-angle spinning (MAS), by applying adiabatic inversion pulses along the S (low-γ) channel while simultaneously applying a conventional spin-locking pulse on the I-channel ((1)H). This study explores an extension of this adiabatic frequency sweep concept to quadrupolar nuclei, focusing on CP from (1)H (I = 1/2) to (2)H spins (S = 1) undergoing fast MAS (νr = 60 kHz). A number of new features emerge, including zero- and double-quantum polarization transfer phenomena that depend on the frequency offsets of the swept pulses, the rf pulse powers, and the MAS spinning rate. An additional mechanism found operational in the (1)H-(2)H CP case that was absent in the spin-1/2 counterpart, concerns the onset of a pseudo-static zero-quantum CP mode, driven by a quadrupole-modulated rf/dipolar recoupling term arising under the action of MAS. The best CP conditions found at these fast spinning rates correspond to double-quantum transfers, involving weak (2)H rf field strengths. At these easily attainable (ca. 10 kHz) rf field conditions, adiabatic level-crossings among the {|1⟩,|0⟩,|-1⟩} mS energy levels, which are known to complicate the CP MAS of quadrupolar nuclei, are avoided. Moreover, the CP line shapes generated in this manner are very close to the ideal (2)H MAS spectral line shapes, facilitating the extraction of quadrupolar coupling parameters. All these features were corroborated with experiments on model compounds and justified using numerical simulations and average Hamiltonian theory models. Potential applications of these new phenomena, as well as extensions to higher spins S, are briefly discussed.

  15. Metabolomic changes in CSF of migraine patients measured with (1)H-NMR spectroscopy.

    Science.gov (United States)

    Zielman, Ronald; Postma, Rudmer; Verhoeven, Aswin; Bakels, Floor; van Oosterhout, Willebrordus P J; Meissner, Axel; van den Maagdenberg, Arn M J M; Terwindt, Gisela M; Mayboroda, Oleg A; Ferrari, Michel D

    2016-11-15

    Migraine is a common episodic brain disorder. Treatment options and diagnosis are hampered by an incomplete understanding of disease pathophysiology and the lack of objective diagnostic markers. The aim of this study was to identify biochemical differences characteristic for different subtypes of migraine in cerebrospinal fluid (CSF) of migraine patients using an exploratory (1)H-NMR-based metabolomics approach. CSF was obtained, in between migraine attacks, via lumbar puncture from patients with hemiplegic migraine, migraine with aura, migraine without aura, and healthy controls. Metabolite concentrations were measured by quantitative (1)H-NMR spectroscopy. Multivariate data analysis was used to find the optimal set of predictors, generalized linear models (GLM) were used to ascertain the differential significance of individual metabolites. In CSF samples from 18 patients with hemiplegic migraine, 38 with migraine with aura, 27 migraine without aura, and 43 healthy controls, nineteen metabolites were identified and quantified. Hemiplegic migraine patients could be discriminated from healthy controls using supervised multivariate modelling with 2-hydroxybutyrate and 2-hydroxyisovalerate as the most discriminant metabolites. Univariate GLM analysis showed 2-hydroxybutyrate to be lower in hemiplegic migraine compared with healthy controls; no significant differences were observed for other metabolites. It was not possible to discriminate migraine with and without aura from healthy controls based on their metabolic profile. Using an exploratory (1)H-NMR metabolomics analysis we identified metabolites that were able to discriminate hemiplegic migraine patients from healthy controls. The lower levels of 2-hydroxybutyrate found in patients with hemiplegic migraine could indicate a dysregulation of the brain's energy metabolism. An experimental confirmation in vitro or in animal models will be required to confirm or discard this hypothesis. Migraine with and migraine

  16. Untargeted 1H-NMR metabolomics in CSF: toward a diagnostic biomarker for motor neuron disease.

    Science.gov (United States)

    Blasco, Hélène; Nadal-Desbarats, Lydie; Pradat, Pierre-François; Gordon, Paul H; Antar, Catherine; Veyrat-Durebex, Charlotte; Moreau, Caroline; Devos, David; Mavel, Sylvie; Emond, Patrick; Andres, Christian R; Corcia, Philippe

    2014-04-01

    To develop a CSF metabolomics signature for motor neuron disease (MND) using (1)H-NMR spectroscopy and to evaluate the predictive value of the profile in a separate cohort. We collected CSF from patients with MND and controls and analyzed the samples using (1)H-NMR spectroscopy. We divided the total patient sample in a 4:1 ratio into a training cohort and a test cohort. First, a metabolomics signature was created by statistical modeling in the training cohort, and then the analyses tested the predictive value of the signature in the test cohort. We conducted 10 independent trials for each step. Finally, we identified the compounds that contributed most consistently to the metabolome profile. Analysis of CSF from 95 patients and 86 controls identified a diagnostic profile for MND (R(2)X > 22%, R(2)Y > 93%, Q(2) > 66%). The best model selected the correct diagnosis with mean probability of 99.31% in the training cohort. The profile discriminated between diagnostic groups with 78.9% sensitivity and 76.5% specificity in the test cohort. Metabolites linked to pathophysiologic pathways in MND (i.e., threonine, histidine, and molecules related to the metabolism of branched amino acids) were among the discriminant compounds. CSF metabolomics using (1)H-NMR spectroscopy can detect a reproducible metabolic signature for MND with reasonable performance. To our knowledge, this is the first metabolomics study that shows that a validation in separate cohorts is feasible. These data should be considered in future biomarker studies. This study provides Class III evidence that CSF metabolomics accurately distinguishes MNDs from other neurologic diseases.

  17. 1H NMR relaxometry, viscometry, and PFG NMR studies of magnetic and nonmagnetic ionic liquids.

    Science.gov (United States)

    Daniel, Carla I; Chávez, Fabián Vaca; Feio, Gabriel; Portugal, Carla A M; Crespo, João G; Sebastião, Pedro J

    2013-10-03

    A study is presented of the molecular dynamics and of the viscosity in pure [Aliquat][Cl] ionic liquid and in a mixture of [Aliquat][Cl] with 1% (v/v) of [Aliquat][FeCl4]. The (1)H spin-lattice relaxation rate, R1, was measured by NMR relaxometry between 8 and 300 MHz. In addition, the translation self-diffusion, D, was measured by pulse field gradient NMR. The ILs' viscosity was measured as a function of an applied magnetic field, B, and it was found that the IL mixture's viscosity decreased with increasing B, whereas the [Aliquat][Cl] viscosity is independent of B. All experimental results were analyzed taking into account the viscosity's magnetic field dependence, assuming a modified Stokes-Einstein diffusion/viscosity relation. The main difference between the relaxation mechanisms responsible for R1 in the two IL systems is related to the additional paramagnetic relaxation contribution associated with the (1)H spins-[FeCl4] paramagnetic moments' interactions. Cross-relaxation cusps in the R1 dispersion, associated with (35)Cl and (1)H nuclear spins in the IL systems, were detected. The R1 model considered was successfully fitted to the experimental results, and it was possible to estimate the value of D at zero field in the case of the IL mixture which was consistent with the values of D measured at 7 and 14.1 T and with the magnetic field dependence estimated from the viscosity measurements. It was observed that a small concentration of [Aliquat][FeCl4] in the [Aliquat][Cl] was enough to produce a "superparamagnetic"-like effect and to change the IL mixture's molecular dynamics and viscosity and to allow for their control with an external magnetic field.

  18. Co(III)-Carbene Radical Approach to Substituted 1H-Indenes.

    Science.gov (United States)

    Das, Braja Gopal; Chirila, Andrei; Tromp, Moniek; Reek, Joost N H; Bruin, Bas de

    2016-07-20

    A new strategy for the catalytic synthesis of substituted 1H-indenes via metalloradical activation of o-cinnamyl N-tosyl hydrazones is presented, taking advantage of the intrinsic reactivity of a Co(III) carbene radical intermediate. The reaction uses readily available starting materials and is operationally simple, thus representing a practical method for the construction of functionalized 1H-indene derivatives. The cheap and easy to prepare low spin cobalt(II) complex [Co(II)(MeTAA)] (MeTAA = tetramethyltetraaza[14]annulene) proved to be the most active catalyst among those investigated, which demonstrates catalytic carbene radical reactivity for a nonporphyrin cobalt(II) complex, and for the first time catalytic activity of [Co(II)(MeTAA)] in general. The methodology has been successfully applied to a broad range of substrates, producing 1H-indenes in good to excellent yields. The metallo-radical catalyzed indene synthesis in this paper represents a unique example of a net (formal) intramolecular carbene insertion reaction into a vinylic C(sp(2))-H bond, made possible by a controlled radical ring-closure process of the carbene radical intermediate involved. The mechanism was investigated computationally, and the results were confirmed by a series of supporting experimental reactions. Density functional theory calculations reveal a stepwise process involving activation of the diazo compound leading to formation of a Co(III)-carbene radical, followed by radical ring-closure to produce an indanyl/benzyl radical intermediate. Subsequent indene product elimination involving a 1,2-hydrogen transfer step regenerates the catalyst. Trapping experiments using 2,2,6,6-tetra-methylpiperidine-1-oxyl (TEMPO) radical or dibenzoylperoxide (DBPO) confirm the involvement of cobalt(III) carbene radical intermediates. Electron paramagnetic resonance spectroscopic spin-trapping experiments using phenyl N-tert-butylnitrone (PBN) reveal the radical nature of the reaction.

  19. Synthesis of Ruthenium Complex Based on 2,6-Bis(1-(phenyl)-1H-benzo[d]imidazol-2-yl)pyridine and 2-(1-Phenyl-1H-benzo[d]imidazol-2-yl)benzoate and Catalytical Oxidation Property of 1-(1H-Benzo[d]imidazol-2-yl)ethanol to 1-(1H-Benzo[d]imidazol-2-yl)ethanone with H2O2

    OpenAIRE

    Shenggui Liu; Rongkai Pan; Guobi Li; Wenyi Su; Chunlin Ni

    2017-01-01

    A new ruthenium complex, Ru(bpbp)(pbb)Cl, based on 2,6-bis(1-(phenyl)-1H-benzo[d]imidazol-2-yl)pyridine (bpbp) and 2-(1-phenyl-1H-benzo[d]imidazol-2-yl)benzoate (pbb) was synthesized. The complex Ru(bpbp)(pbb)Cl could catalytically oxidize 1-(1H-benzo[d]imidazol-2-yl)ethanol to 1-(1H-benzo[d]imidazol-2-yl)ethanone with H2O2 as oxidant. Influence of temperature and catalyst amount on the oxidation reaction was evaluated. The reaction optimal conditions are as follows: molar ratio of catalyst t...

  20. 1H and 13C resonance designation of antimycin A1 by two-dimensional NMR spectroscopy

    Science.gov (United States)

    Abidi, S.L.; Adams, B.R.

    1987-01-01

    Complete 1H and 13C resonance assignments of antimycin A1 were accomplished by two-dimensional NMR techniques, viz. 1H homonuclear COSY correlation, heteronuclear 13C-1H chemical shift correlation and long-range heteronuclear 13C-1H COLOC correlation. Antimycin A1 was found to consist of two isomeric components in a 2:1 ratio based on NMR spectroscopic evidence. The structure of the major component was newly assigned as the 8-isopentanoic acid ester. The spectra of the minor component were consistent with the known structure of antimycin A1.

  1. Simultaneous 19F-1H medium resolution NMR spectroscopy for online reaction monitoring

    Science.gov (United States)

    Zientek, Nicolai; Laurain, Clément; Meyer, Klas; Kraume, Matthias; Guthausen, Gisela; Maiwald, Michael

    2014-12-01

    Medium resolution nuclear magnetic resonance (MR-NMR) spectroscopy is currently a fast developing field, which has an enormous potential to become an important analytical tool for reaction monitoring, in hyphenated techniques, and for systematic investigations of complex mixtures. The recent developments of innovative MR-NMR spectrometers are therefore remarkable due to their possible applications in quality control, education, and process monitoring. MR-NMR spectroscopy can beneficially be applied for fast, non-invasive, and volume integrating analyses under rough environmental conditions. Within this study, a simple 1/16″ fluorinated ethylene propylene (FEP) tube with an ID of 0.04″ (1.02 mm) was used as a flow cell in combination with a 5 mm glass Dewar tube inserted into a benchtop MR-NMR spectrometer with a 1H Larmor frequency of 43.32 MHz and 40.68 MHz for 19F. For the first time, quasi-simultaneous proton and fluorine NMR spectra were recorded with a series of alternating 19F and 1H single scan spectra along the reaction time coordinate of a homogeneously catalysed esterification model reaction containing fluorinated compounds. The results were compared to quantitative NMR spectra from a hyphenated 500 MHz online NMR instrument for validation. Automation of handling, pre-processing, and analysis of NMR data becomes increasingly important for process monitoring applications of online NMR spectroscopy and for its technical and practical acceptance. Thus, NMR spectra were automatically baseline corrected and phased using the minimum entropy method. Data analysis schemes were designed such that they are based on simple direct integration or first principle line fitting, with the aim that the analysis directly revealed molar concentrations from the spectra. Finally, the performance of 1/16″ FEP tube set-up with an ID of 1.02 mm was characterised regarding the limit of detection (LOQ (1H) = 0.335 mol L-1 and LOQ (19F) = 0.130 mol L-1 for trifluoroethanol in

  2. Personality and neurochemicals in the human brain: A preliminary study using 1H MRS

    Institute of Scientific and Technical Information of China (English)

    XU Shiyong; PENG Danling; JIN Zhen; LIU Hongyan; YANG Jie

    2005-01-01

    To investigate the neuro-biological bases of introversion-extraversion personality traits, the concentra- tion of four neurochemicals (Cho, mI, α-Glx and NAA) in anterior cigulate gyrus between normal extroverts and introverts were examined using non-invasive 1H MRS technique. Our study revealed that introverts have significantly higher level of α-Glx, Cho and mI in the anterior cingulate gyrus than extroverts. This result provides new evidence that the anterior cingulate gyrus is related to personality traits partly in support of Eysenck's supposition that introverts have higher arousal level than extroverts. Moreover, this result offers neurochemical data for psychobiological theories of personality.

  3. (E-2-(2-Furylmethylidene-2,3-dihydro-1H-pyrrolizin-1-one

    Directory of Open Access Journals (Sweden)

    Yousaf Ali

    2010-07-01

    Full Text Available The title compound, C12H9NO2, was prepared by an Aldol reaction of furfuraldehyde with 2,3-dihydro-1H-pyrrolizin-1-one. The molecule is almost planar, with an r.m.s. deviation of 0.045 Å, excluding the methylene H atoms. In the crystal structure, molecules are linked via weak intermolecular C—H...O hydrogen bonding and aromatic π–π stacking [centroid–centroid distance = 3.6151 (9 Å].

  4. 1-Ethyl-2-phenyl-3-[2-(trimethylsilylethynyl]-1H-indole

    Directory of Open Access Journals (Sweden)

    Iaroslav Baglai

    2013-06-01

    Full Text Available The title compound, C21H23NSi, was synthesized by Sonogashira-type reaction of 1-ethyl-3-iodo-2-phenyl-1H-indole with trimethylsilylacetylene. The indole ring system is nearly planar [maximum atomic deviation = 0.0244 (15 Å] and is oriented at a dihedral angle of 51.48 (4° with respect to the phenyl ring. The supramolecular aggregation is completed by weak C—H...π interactions of the methylene and phenyl groups with the benzene and pyrrole rings of the indole ring system. The methyl groups of the trimethylsilyl unit are equally disordered over two sets of sites.

  5. 5-Bromo-1H-thieno[2,3-d]imidazole

    Directory of Open Access Journals (Sweden)

    Fen Wang

    2010-08-01

    Full Text Available The crystal structure of the title compound, C5H3BrN2S, shows that bromination of 1H-thieno[2,3-d]imidazole with N-bromosuccinimide in acetonitrile occurs at position 5 of the bicyclic system. The molecule is almost planar, with a mean deviation of 0.015 Å from the least-squares plane through all the non-H atoms. In the crystal, N—H...N hydrogen bonds link the molecules into infinite C(4 chains running along [101].

  6. 1H NMR Fingerprinting of Soybean Extracts, with Emphasis on Identification and Quantification of Isoflavones

    Directory of Open Access Journals (Sweden)

    Vincenzo Brandolini

    2010-02-01

    Full Text Available 1H NMR spectra were recorded of methanolic extracts of seven soybean varieties (Glycine max., cultivated using traditional and organic farming techniques. It was possible to identify signals belonging to the groups of amino acids, carbohydrates, organic acids and aromatic substances in the spectra. In the aromatic zone, the isoflavone signals were of particular interest: genistein, daidzein, genistin, daidzin, malonylgenistin, acetylgenistin, malonyldaidzin signals were assigned and these compounds were quantified, resulting in accordance with published data, and further demonstrating the potential of the NMR technique in food science.

  7. Synthesis, antimicrobial and antifungal activities of novel 1H-1,4-diazepines containing pyrazolopyrimidinone moiety

    Indian Academy of Sciences (India)

    Rajesh Kumar; Yogesh Chandra Joshi

    2009-07-01

    Acylation of 5-(2-ethoxyphenyl)-1-methyl-3-propyl-1,6-dihydro-7-pyrazolo [4,3-d) pyrimidin-7-one 1 with chloroacetylchloride in the presence of anyhydrous aluminium chloride affords 5-[(5-chloroacetyl-2-ethoxy)phenyl]-1-methyl-3-propyl-1,6-dihydro-7H-pyrazolo [4,3-d] pyrimidin-7-one 2. The compound 2 condensed with various -diketones/-ketoesters compound, to obtain new -diketones/-ketoesters 4a-i treated with ethylenediamine (EDA) gives 1H-1,4-diazepines. The compounds 5a-i has been screened for antimicrobial, antifungal and anthelmintic activities.

  8. Synthesis of substituted 1H-indazoles from arynes and hydrazones.

    Science.gov (United States)

    Li, Pan; Wu, Chunrui; Zhao, Jingjing; Rogness, Donald C; Shi, Feng

    2012-04-06

    The 1H-indazole skeleton can be constructed by a [3 + 2] annulation approach from arynes and hydrazones. Under different reaction conditions, both N-tosylhydrazones and N-aryl/alkylhydrazones can be used to afford a variety of indazoles. The former reaction affords 3-substituted indazoles either via in situ generated diazo compounds or through an annulation/elimination process. The latter reaction leads to 1,3-disubstituted indazoles likely through an annulation/oxidation process. The reactions operate under mild conditions and can accommodate aryl, vinyl, and less satisfactorily, alkyl groups.

  9. Crystal structure of 2-methyl-1H-imidazol-3-ium hydrogen oxalate dihydrate

    Directory of Open Access Journals (Sweden)

    Mouhamadou Birame Diop

    2016-08-01

    Full Text Available Single crystals of the title molecular salt, C4H7N2+·HC2O4−·2H2O, were isolated from the reaction of 2-methyl-1H-imidazole and oxalic acid in a 1:1 molar ratio in water. In the crystal, the cations and anions are positioned alternately along an infinite [010] ribbon and linked together through bifurcated N—H...(O,O hydrogen bonds. The water molecules of crystallization link the chains into (10-1 bilayers, with the methyl groups of the cations organized in an isotactic manner.

  10. 4-Amino-1H-1,2,4-triazol-1-ium nitrate

    Directory of Open Access Journals (Sweden)

    Ivan Němec

    2011-01-01

    Full Text Available The non-centrosymmetric crystal structure of the novel semi-organic title compound, C2H5N4+·NO3−, is based on alternating layers of 4-amino-1H-1,2,4-triazolinium cations (formed by parallel chains of cations mediated by weak C—H...N hydrogen bonds and nitrate anions interconnected via linear and bifurcated N—H...O hydrogen bonds and weak C—H...O hydrogen bonds. N—H...N hydrogen bonds link the anions and cations.

  11. Experimental surface charge density of the Si (100)-2x1H surface

    DEFF Research Database (Denmark)

    Ciston, J.; Marks, L.D.; Feidenhans'l, R.;

    2006-01-01

    We report a three-dimensional charge density refinement from x-ray diffraction intensities of the Si (100) 2x1H surface. By paying careful attention to parameterizing the bulk Si bonding, we are able to locate the hydrogen atoms at the surface, which could not be done previously. In addition, we...... are able to partially refine the local charge density at the surface. We find experimentally an increased, slightly localized bond density of approximately 0.31 electrons between each Si atom pair at the surface. Both the atomic positions and the charge density are in remarkably good agreement with density...

  12. 1H NMR spectra dataset and solid-state NMR data of cowpea (Vigna unguiculata)

    DEFF Research Database (Denmark)

    Alves Filho, Elenilson G.; Silva, Lorena M. A.; Teofilo, Elizita M.

    2017-01-01

    In this article the NMR data from chemical shifts, coupling constants, and structures of all the characterized compounds were provided, beyond a complementary PCA evaluation for the corresponding manuscript (E.G. Alves Filho, L.M.A. Silva, E.M. Teofilo, F.H. Larsen, E.S. de Brito, 2017) [3......]. In addition, a complementary assessment from solid-state NMR data was provided. For further chemometric analysis, numerical matrices from the raw 1H NMR data were made available in Microsoft Excel workbook format (.xls)....

  13. Hip Morphology in MPS-1H Patients: An MRI-based Study.

    Science.gov (United States)

    Breyer, Sandra R; Muschol, Nicole; Schmidt, Mona; Rupprecht, Martin; Babin, Kornelia; Herrmann, Jochen; Stücker, Ralf

    2016-09-15

    Hip dysplasia is common in mucopolysaccharidosis type-1H (MPS-1H) patients, but its morphology is not completely understood. No magnetic resonance imaging (MRI)-based studies have been reported in the literature. The purpose of this study was to improve knowledge of hip dysplasia pathology by describing the hip morphology of these patients in MRI scans, plain radiographs, and arthrograms. We performed a retrospective chart review of 18 MPS-1H patients. Supine anteroposterior pelvic radiographs of 36 hips and MRI scans of 18 hips were analyzed. Six arthrographs were also available. Plain radiographs were available for 18 patients. The mean age was 6.0 (SD=3.8) years. The mean acetabular index (AI) was 36.2 degrees (SD=5.8), and the mean migration percentage was 59.0% (SD=17.2). MRI data were available for 9 patients. The MRI findings were compared with the radiographs of the same patient. The mean AI (39.3 degrees, SD=5.8) was confirmed by the MRI findings (39.1 degrees, SD=5.5). The migration percentage was lower in the MRI scans than in the radiographs. Radiologically, the center-edge angle was negative in all patients, with a mean of -16.8 degrees (SD=7.9), and the MRI images produced a more negative value (-19.6 degrees, SD=7.6). The soft tissue coverage of the femoral head was described with the inclusion of the cartilaginous roof and labrum. The cartilaginous AI was 22.4 degrees (SD=7.5), and the labral AI was 13.5 degrees (SD=6.7). All 6 arthrograms revealed stability during dynamic testing. This study provides the first description of hip morphology in MPS-1H patients through MRI-based data. The cartilaginous coverage of the hip was increased compared with that of healthy children. The use of radiography alone may lead to a misunderstanding of hip morphology. MRI and arthrogram is highly recommended if surgery is considered.

  14. Baryonic violation of R-parity from anomalous $U(1)_H$

    CERN Document Server

    Florez, Andres; Velasquez, Mauricio; Zapata, Oscar

    2013-01-01

    Supersymmetric scenarios with R-parity conservation are becoming very constrained due to the lack of missing energy signals, thus motivating those scenarios with R-parity violation. In view of this, we consider a supersymmetric model with R-parity violation and extended by an anomalous horizontal $U(1)_H$ symmetry, where a self-consistent framework with baryon-number violation is achieved along with a proper supression for lepton number violating dimension-5 operators in order to keep a proton decay safe. With the introduction of right-handed neutrinos both Dirac and Majorana masses can be accommodated within this model. The implications for collider physics are discussed.

  15. 1H NMR fingerprinting of soybean extracts, with emphasis on identification and quantification of isoflavones.

    Science.gov (United States)

    Caligiani, Augusta; Palla, Gerardo; Maietti, Annalisa; Cirlini, Martina; Brandolini, Vincenzo

    2010-03-01

    1H NMR spectra were recorded of methanolic extracts of seven soybean varieties (Glycine max.), cultivated using traditional and organic farming techniques. It was possible to identify signals belonging to the groups of amino acids, carbohydrates, organic acids and aromatic substances in the spectra. In the aromatic zone, the isoflavone signals were of particular interest: genistein, daidzein, genistin, daidzin, malonylgenistin, acetylgenistin, malonyldaidzin signals were assigned and these compounds were quantified, resulting in accordance with published data, and further demonstrating the potential of the NMR technique in food science.

  16. 1H NMR study of fermented cocoa (Theobroma cacao L.) beans.

    Science.gov (United States)

    Caligiani, Augusta; Acquotti, Domenico; Cirlini, Martina; Palla, Gerardo

    2010-12-08

    This study reports for the first time the metabolic profile of cocoa (Theobroma cacao L.) beans using the (1)H NMR technique applied to polar extracts of fermented cocoa beans. The simultaneous detection and quantification of amino acids, polyalcohols, organic acids, sugars, methylxanthines, catechins, and phenols were obtained by assigning the major signals of the spectra for different varieties of cocoa beans (Forastero, Criollo, and Trinitario) from different countries (Ecuador, Ghana, Grenada, and Trinidad). The data set obtained, representative of all classes of soluble compounds of cocoa, was useful to characterize the fermented cocoa beans as a function of the variety and geographic origin.

  17. The 1H NMR Structure of Bovine Pb2+- Osteocalcin and Implications for Lead Toxicity

    OpenAIRE

    Dowd, T. L.; Li, L.; Gundberg, C.M.

    2008-01-01

    Structural information on the effect of Pb2+ on proteins under physiologically relevant conditions is largely unknown. We have previously shown that low levels of lead increased the amount of osteocalcin bound to hydroxyapatite (BBA 1535:153)). This suggested that lead induced a more compact structure in the protein. We have determined the 3D structure of Pb2+-osteocalcin (49 amino acids), a bone protein from a target tissue, using 1H 2D NMR techniques. Lead, at a stoichiometry of only 1:1, i...

  18. {sup 1}H NMR investigation of self-association of vanillin in aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Bogdan, Mircea; Floare, Calin G; PIrnau, Adrian, E-mail: mircea.bogdan@itim-cj.r [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath, 400293 Cluj-Napoca (Romania)

    2009-08-01

    A self-association of vanillin have been studied by {sup 1}H NMR spectroscopy using the analysis of proton chemical shifts changes in aqueous solution as a function of concentration. The experimental results have been analysed using indefinite non-cooperative and cooperative models of molecular self-association, enabling the determination of equilibrium constants, parameters of cooperativity and the limiting values of vanillin proton chemical shifts in the complex. It was found that the dimer formation creates energetically favourable conditions for subsequent molecular association.

  19. 1H NMR investigation of self-association of vanillin in aqueous solution

    Science.gov (United States)

    Bogdan, Mircea; Floare, Calin G.; Pîrnau, Adrian

    2009-08-01

    A self-association of vanillin have been studied by 1H NMR spectroscopy using the analysis of proton chemical shifts changes in aqueous solution as a function of concentration. The experimental results have been analysed using indefinite non-cooperative and cooperative models of molecular self-association, enabling the determination of equilibrium constants, parameters of cooperativity and the limiting values of vanillin proton chemical shifts in the complex. It was found that the dimer formation creates energetically favourable conditions for subsequent molecular association.

  20. 3-Carb-oxy-methyl-1H-indole-4-carb-oxy-lic acid.

    Science.gov (United States)

    Mao, Shulin

    2012-01-01

    In the title compound, C(11)H(9)NO(4), the carboxyl group bonded to the six-membered ring lies close to the plane of the 1H-indole ring system [dihedral angle = 13.13 (9)°], whereas the carb-oxy-lic acid group linked to the five-membered ring by a methyl-ene bridge is close to perpendicular [78.85 (9)°]. In the crystal, O-H⋯O and N-H⋯O hydrogen bonds link the mol-ecules, generating (110) sheets.

  1. (1) H and (13) C NMR characterization of new cycloartane triterpenes from Mangifera indica.

    Science.gov (United States)

    Escobedo-Martínez, Carolina; Concepción Lozada, M; Hernández-Ortega, Simón; Villarreal, María Luisa; Gnecco, Dino; Enríquez, Raúl G; Reynolds, William

    2012-01-01

    From the stem bark of Mangifera indica, seven cycloartane-type secondary metabolites were isolated. Compound 1 has been isolated for the first time from M. indica, whereas compounds 2 (2a and 2b, as an epimeric mixture), 3, and 4 are new triterpenoid-type cycloartanes. Unambiguous (13) C and (1) H NMR assignments for these compounds and the known compounds mangiferonic acid (compound 5), isomangiferolic acid (compound 6), ambolic acid (compound 7), and friedelin (compound 8) are reported; the latter because full NMR data for these compounds are not available in the literature.

  2. Experimental surface charge density of the Si (100)-2x1H surface

    DEFF Research Database (Denmark)

    Ciston, J.; Marks, L.D.; Feidenhans'l, R.

    2006-01-01

    We report a three-dimensional charge density refinement from x-ray diffraction intensities of the Si (100) 2x1H surface. By paying careful attention to parameterizing the bulk Si bonding, we are able to locate the hydrogen atoms at the surface, which could not be done previously. In addition, we...... are able to partially refine the local charge density at the surface. We find experimentally an increased, slightly localized bond density of approximately 0.31 electrons between each Si atom pair at the surface. Both the atomic positions and the charge density are in remarkably good agreement with density...

  3. (1)H NMR Study of the solution structure of sarafotoxin-S6b.

    Science.gov (United States)

    Aumelas, A; Chiche, L; Mahe, E; Le-Nguyen, D; Sizun, P; Berthault, P; Perly, B

    1991-01-01

    Sarafotoxin-S6b has been synthesized and studied by (1)H NMR in 50 50 acetonitrile/water mixture. All spin systems were identified and assigned with the aid of 2D experiments. On the basis of these data, a 3D structure of sarafotoxin is proposed and compared to that of [Nle(7)]endothelin obtained in the same conditions. From this study, it appeared that sarafotoxin-S6b and [Nle(7)]endothelin roughly share the same 3D structure, the main differences being located in the 4-7 loop bearing the sequence variation.

  4. (1)H NMR spectra dataset and solid-state NMR data of cowpea (Vigna unguiculata).

    Science.gov (United States)

    Alves Filho, Elenilson G; Silva, Lorena M A; Teofilo, Elizita M; Larsen, Flemming H; de Brito, Edy S

    2017-04-01

    In this article the NMR data from chemical shifts, coupling constants, and structures of all the characterized compounds were provided, beyond a complementary PCA evaluation for the corresponding manuscript (E.G. Alves Filho, L.M.A. Silva, E.M. Teofilo, F.H. Larsen, E.S. de Brito, 2017) [3]. In addition, a complementary assessment from solid-state NMR data was provided. For further chemometric analysis, numerical matrices from the raw (1)H NMR data were made available in Microsoft Excel workbook format (.xls).

  5. [1H-NMR studies of the ACTH-like immunoregulatory peptides].

    Science.gov (United States)

    Khristoforov, V S; Kutyshenko, V P; Abramov, V M; Zav'ialov, V P

    1997-01-01

    A comparative study of the conformational and dynamics properties of the ACTH-like linear peptides, sequences of which correspond to amino acid residues 11-20 of the heavy chain of human immunoglobulin G1 Eu, residues 78-85 of human pro-interleukin-1 alpha and site 10-18 of human ACTH, was performed in aqueous solution and dimethylsulfoxide by 1H-NMR spectroscopy at 400 MHz. The peptides were shown to possess an unordered unfolded flexible conformation in aqueous solution. The revealed structural and dynamic features of the peptides are discussed together with biological activity of this class of compounds.

  6. 2-(2,4-Dichlorophenoxy-1-(1H-pyrazol-1-ylethanone

    Directory of Open Access Journals (Sweden)

    Abdul Qayyum Ather

    2010-10-01

    Full Text Available In the title compound, C11H8Cl2N2O2, the 2,4-dichlorophenoxy and 1H-pyrazole groups are almost planar [r.m.s. deviations of 0.0157 and 0.0008 Å, respectively] and are oriented at a dihedral angle of 64.17 (5° with respect to one another. In the crystal, the molecules are stabilized in the form of dimers due to inversion-related C—H...O hydrogen bonds, with R22(10 ring motifs.

  7. Magnetic resonance imaging and {sup 1}H-magnetic resonance spectroscopy in amyotrophic lateral sclerosis

    Energy Technology Data Exchange (ETDEWEB)

    Sarchielli, P.; Gallai, V. [Neurological Clinic, Policlinico Monte Luce, Perugia (Italy); Pelliccioli, G.P.; Chiarini, P. [Dept. of Neuroradiology, Azienda Ospedaliera, Perugia (Italy); Tarducci, R.; Presciutti, O.; Gobbi, G. [Dept. of Medical Physics, Azienda Ospedaliera, Perugia (Italy)

    2001-03-01

    We aimed to increase confidence in the combined use of MRI and proton MR spectroscopy ({sup 1}H-MRS) in diagnosis of amyotrophic lateral sclerosis (ALS). We investigated 12 patients with ALS, seven definite and five probable, taking into account clinical measures of motor neuron function. On T2-weighted images we found high signal in the corticospinal tract in six and low signal in the primary motor cortex in seven of the 12 patients. Atrophy of the precentral gyrus was apparent in all the patients apart from one with probable ALS. Absolute quantification of cerebral metabolites using {sup 1}H-MRS demonstrated a significantly lower mean concentration of N-acetylaspartate (NAA) in the precentral gyrus of patients with probable and definite ALS (8.5 {+-} 0.62) than in control subjects (10.4 {+-} 0.71; P < 0.001). NAA concentration in primary motor cortex correlated with Norris scale scores (r = 0.30; P < 0.0001) but not with the ALS Functional Rating Scale score or disease duration. Significantly lower levels of NAA were detected in patients with low signal in the motor cortex than in those without (P < 0.01). Mean choline (Cho) and creatine (Cr) values did not differ between patients with ALS and controls. (orig.)

  8. Antifungal properties of wheat histones (H1-H4) and purified wheat histone H1.

    Science.gov (United States)

    De Lucca, Anthony J; Heden, Lars-Olof; Ingber, Bruce; Bhatnagar, Deepak

    2011-07-13

    Wheat ( Triticum spp.) histones H1, H2, H3, and H4 were extracted, and H1 was further purified. The effect of these histones on specific fungi that may or may not be pathogenic to wheat was determined. These fungi included Aspergillus flavus , Aspergillus fumigatus , Aspergillus niger , Fusarium oxysporum , Fusarium verticillioides , Fusarium solani , Fusarium graminearum , Penicillium digitatum , Penicillium italicum , and Greeneria uvicola . Non-germinated and germinating conidia of these fungi were bioassayed separately. The non-germinated and germinating conidia of all Fusarium species were highly susceptible to the mixture (H1-H4) as well as pure H1, with viability losses of 99-100% found to be significant (p histone mixture and pure H1. F. graminearum was the most sensitive to histone activity. The histones were inactive against all of the non-germinated Penicillium spp. conidia. However, they significantly reduced the viability of the germinating conidia of the Penicillium spp. conidia, with 95% loss at 2.5 μM. Non-germinated and germinating conidia viability of the Aspergillus spp. and G. uvicola were unaffected when exposed to histones up to 10 μM. Results indicate that Fusarium spp. pathogenic to wheat are susceptible to wheat histones, indicating that these proteins may be a resistance mechanism in wheat against fungal infection.

  9. Sterols associated with small unilamellar vesicles (SUVs): intrinsic mobility role for 1H NMR detection.

    Science.gov (United States)

    Mouret, Liza; Da Costa, Grégory; Bondon, Arnaud

    2014-07-01

    Small unilamellar vesicles (SUVs) of phospholipids are often used as a membrane model system for studying the interaction of molecules. When using NMR under the standard liquid-state conditions, SUV phospholipid proton spectra can be recorded, exhibiting sharp signals. This is not only because of the fast vesicular tumbling but also because of the combination of this tumbling with the individual motion of the lipids inside the bilayer. This appears evident because addition of cholesterol is responsible of broader resonances because of the slowing down of the lipid motion. On the other hand, no (1)H signal is detected for cholesterol in the bilayer. This lack of detection of the inserted molecules explains why generally SUVs are not considered as a good model for NMR studies under the standard liquid-state conditions. Here, we use two other sterols in order to demonstrate that an increase of the molecular mobility inside the bilayer could allow the detection of their proton resonances. For desmosterol and lanosterol, which show higher mobility inside the bilayer, with increasing lateral diffusion rates, (1)H sterol signals are detected in contrast to cholesterol. For the fast diffusing lanosterol, no significant improvement in detection is observed using deuterated lipids, demonstrating that homonuclear dipolar coupling is fully averaged out. Furthermore, in the case of low mobility such as for cholesterol, the use of a fast magic angle spinning probe is shown to be efficient to recover the full proton spectrum. Copyright © 2014 John Wiley & Sons, Ltd.

  10. UV-visible and (1)H-(15)N NMR spectroscopic studies of colorimetric thiosemicarbazide anion sensors.

    Science.gov (United States)

    Farrugia, Kristina N; Makuc, Damjan; Podborska, Agnieszka; Szaciłowski, Konrad; Plavec, Janez; Magri, David C

    2015-02-14

    Four model thiosemicarbazide anion chemosensors containing three N-H bonds, substituted with phenyl and/or 4-nitrophenyl units, were synthesised and studied for their anion binding abilities with hydroxide, fluoride, acetate, dihydrogen phosphate and chloride. The anion binding properties were studied in DMSO and 9 : 1 DMSO-H2O by UV-visible absorption and (1)H/(13)C/(15)N NMR spectroscopic techniques and corroborated with DFT studies. Significant changes were observed in the UV-visible absorption spectra with all anions, except for chloride, accompanied by dramatic colour changes visible to the naked eye. These changes were determined to be due to the deprotonation of the central N-H proton and not due to hydrogen bonding based on (1)H/(15)N NMR titration studies with acetate in DMSO-d6-0.5% water. Direct evidence for deprotonation was confirmed by the disappearance of the central thiourea proton and the formation of acetic acid. DFT and charge distribution calculations suggest that for all four compounds the central N-H proton is the most acidic. Hence, the anion chemosensors operate by a deprotonation mechanism of the central N-H proton rather than by hydrogen bonding as is often reported.

  11. 1H-NMR characterization of poly(ethylene glycol) and polydimethylsiloxane copolymer

    Science.gov (United States)

    Zainuddin, Ain Athirah; Othaman, Rizafizah; Noor, Wan Syaidatul Aqma Wan Mohd; Anuar, Farah Hannan

    2016-11-01

    This paper describes the synthesis and characterization of poly(ethylene glycol) (PEG) and polydimethylsiloxane (PDMS) copolymers. The copolymers were synthesized by reacting hydroxyl group (-OH) of poly(ethylene glycol) (PEG) and polydimetylsiloxane (PDMS) with isocyanate group (R-N=C=O) of 1,6-hexamethylene diisocyanate (HMDI). The reaction was carried out at room temperature. The copolymers were synthesized in three different compositions which differ in molar ratios of PEG to PDMS. The ratios (PEG:PDMS) used were 2:6. 3:5 and 4:4. The formation of the copolymers was characterized by 1H Nuclear Magnetic Resonance (1H-NMR) for structural determination. The presence of proton signal at 4.80 ppm which belongs to the proton of urethane group indicates the formation of urethane links. The formation of urethane links showed that two homopolymers were linked together by HMDI to form longer copolymer chains. It is worth to note that the sequence of PEG and PDMS along the copolymer chain is random.

  12. Quantification of organic and amino acids in beer by 1H NMR spectroscopy.

    Science.gov (United States)

    Nord, Lars I; Vaag, Pia; Duus, Jens Ø

    2004-08-15

    The quantification of organic and amino acids in beer using 1H NMR spectroscopy is demonstrated. Quantification was made both by integration of signals in the spectra together with use of calibration references and by use of partial least-squares (PLS) regression. Results from the NMR quantifications were compared with those obtained from determinations by amino acid analysis on HPLC and organic acid analysis by capillary electrophoresis. The described NMR-based methods could satisfactorily be used for quantification of several of the investigated metabolites in beer down to approximately 10 mg/L and for most with a good to high accuracy compared to results obtained by HPLC and capillary electrophoresis (R2 0.90-0.99). This was achieved with a simple sample preparation and one-dimensional 1H NMR spectra obtained in a few minutes. The use of PLS clearly improves the accuracy of the quantifications, based on comparison to results obtained by HPLC and capillary electrophoresis, and furthermore permits the determination of components with partially overlapped signals in the spectrum. NMR spectroscopy in combination with PLS will be a useful tool for the quantification of metabolites, not only in beer but also in other beverages and biofluids.

  13. Evaluation of brain metabolism in autism. A {sup 1}H-MRS study

    Energy Technology Data Exchange (ETDEWEB)

    Otsuka, Hideki; Harada, Masafumi; Mori, Kenji; Taoka, Yoshiaki; Nishitani, Hiromu [Tokushima Univ. (Japan). School of Medicine

    1998-01-01

    We performed a {sup 1}H-MRS study on 13 autistic patients (2-15 y.o., 10 males, 3 females) and 10 normal children (6-14 y.o., 4 males, 6 females). An MR spectra of the bilateral amygdaloid-hippocampal regions, which play a very important role in the limbic system, was obtained for each subject using STEAM sequence (TR=5000 ms, TE=18 ms). In addition to the evaluation of signal intensity ratios, the absolute concentrations of 3 major metabolites, N-acetyl-aspartate (NAA), creatine/phosphocreatine (Cr) and choline-containing substances (Cho), were quantified by means of an internal reference method using unsuppressed tissue water. The concentration of NAA was decreased in autistic patients, and the difference between patients and normal controls was significant (right sided NAA level: autistic group-8.6{+-}2.1 mM, control group-11.0{+-}1.1 mM; left sided NAA level: autistic group-8.9{+-}1.8 mM, control group-10.5{+-}1.4 mM). We speculate that the decrease in NAA levels in the autistic patients reflects neuronal hypofunction or immature neurons. {sup 1}H-MRS may provide useful clinical information which is not readily obtainable with other imaging methods. (author)

  14. 23Na and 1H NMR Relaxometry of Shale at High Magnetic Field

    CERN Document Server

    Yang, Donghan

    2016-01-01

    Formation evaluation of unconventional reservoirs is challenging due to the coexistence of different phases such as kerogen, bitumen, movable and bound light hydrocarbon and water. Current low-frequency (0.05 T) nuclear magnetic resonance (NMR) laboratory and logging methods are incapable of quantitatively separating the different phases. We demonstrate the utility of high-field (9 T) NMR 2D T1-T2 measurements for separating hydrocarbon and the clay-interacting aqueous phases in shale based on the difference in the frequency dependence of the spin-lattice relaxation time. Furthermore, we demonstrate 23Na NMR as a promising complementary technique to conventional 1H NMR for shale fluid typing, taking advantage of the fact that sodium ions are only present in the aqueous phase. We validate high-field (9 T) 23Na-1H NMR relaxometry for assessing brine-filled porosity and brine salinity in various porous materials, including porous glass, conventional rocks, clays, and shale, and apply it for differentiating hydro...

  15. One-pot Synthesis of 2-Nitro-4,5-dicyano-1H-imidazole

    Institute of Scientific and Technical Information of China (English)

    XU Cheng; BIFu-qiang; FAN Xue-zhong; LI Ji-zhen; WANG Bo-zhou; GE Zhong-xue; LIU Qing; ZHANG Guo-fang

    2011-01-01

    In the last few decades,nitroimidazoles have been investigated mostly due to their properties as antibiotics,radiosensitizers and anti-protozoans[1 -3].Recently these nitroimidazoles,such as 2,4-dinitroimidazole,1-methyl-2,4,5-trinitroimidazole and their energetic salts, have attracted renewed attention for their favorable explosive performance as well as improved safety characteristics[4,5].Because of the activity of cyano group,2-nitro-4,5-dicyano-1 H-imidazole (NDCI) could be used as an intermediate in the synthesis of novel energetic materials containing nitroimidazole moiety.NDCI has been synthesized by the procedure given by Yixin Lu and coworkers[6],where the diazotization reaction and the Sandmeyer reaction were separately achieved.NDCI was obtained by adding a solution of sodium nitrite to 2-diazo4,5-dicyanoimidazole which was generated by diazotization of 2-amino-4,5-dicyano-1H-imidazole ( ADCI ) with sodium nitrite in water-hydrochloric acid and collected by filtration.Dry 2-diazo-4,5-dicyanoimidazole was so sensitive to shock that its separation may cause explosion[7].

  16. 1H NMR-based serum metabolic profiling in compensated and decompensated cirrhosis

    Institute of Scientific and Technical Information of China (English)

    Su-Wen Qi; Zhi-Guang Tu; Wu-Jian Peng; Lin-Xian Wang; Xin Ou-Yang; An-Ji Cai; Yong Dai

    2012-01-01

    AIM: To study the metabolic profiling of serum samples from compensated and decompensated cirrhosis patients.METHODS: A pilot metabolic profiling study was conducted using three groups: compensated cirrhosis patients (n = 30), decompensated cirrhosis patients (n = 30) and healthy controls (n = 30). A 1H nuclear magnetic resonance (NMR)-based metabonomics approach was used to obtain the serum metabolic profiles of the samples. The acquired data were processed by multivariate principal component analysis and orthogonal partial least-squares discriminant analysis (OPLS-DA). RESULTS: The OPLS-DA model was capable of distinguishing between decompensated and compensated cirrhosis patients, with an R2Y of 0.784 and a Q2Y of 0.598. Twelve metabolites, such as pyruvate, phenylalanine and succinate, were identified as the most influential factors for the difference between the two groups. The validation of the diagnosis prediction showed that the accuracy of the OPLSDA model was 85% (17/20). CONCLUSION: 1H NMR spectra combined with pattern recognition analysis techniques offer a new way to diagnose compensated and decompensated cirrhosis in the future.

  17. 1H NMR metabolite fingerprinting as a new tool for body fluid identification in forensic science.

    Science.gov (United States)

    Scano, Paola; Locci, Emanuela; Noto, Antonio; Navarra, Gabriele; Murgia, Federica; Lussu, Milena; Barberini, Luigi; Atzori, Luigi; De Giorgio, Fabio; Rosa, Maria Francesca; d'Aloja, Ernesto

    2013-08-01

    In this feasibility study, we propose, for the first time, (1)H NMR spectroscopy coupled with mathematical strategies as a valid tool for body fluid (BF) trace identification in forensic science. In order to assess the ability of this approach to identify traces composed either by a single or by two different BFs, samples of blood, urine, saliva, and semen were collected from different donors, and binary mixtures were prepared. (1)H NMR analyses were carried out for all samples. Spectral data of the whole set were firstly submitted to unsupervised principal component analysis (PCA); it showed that samples of the same BF cluster well on the basis of their characterizing molecular components and that mixtures exhibit intermediate characteristics among BF typologies. Furthermore, samples were divided into a training set and a test set. An average NMR spectral profile for each typology of BF was obtained from the training set and validated as representative of each BF class. Finally, a fitting procedure, based on a system of linear equations with the four obtained average spectral profiles, was applied to the test set and the mixture samples; it showed that BFs can be unambiguously identified, even as components of a mixture. The successful use of this mathematical procedure has the advantage, in forensics, of overcoming bias due to the analyst's personal judgment. We therefore propose this combined approach as a valid, fast, and non-destructive tool for addressing the challenges in the identification of composite traces in forensics.

  18. The cold neutron star in the soft X-ray transient 1H 1905+000

    CERN Document Server

    Jonker, Peter G; Chakrabarty, Deepto; Juett, Adrienne M

    2007-01-01

    We report on our analysis of 300 ks of Chandra observations of the neutron star soft X-ray transient 1H1905+000 in quiescence. We do not detect the source down to a 95% confidence unabsorbed flux upper limit of 2E-16 erg cm-2 s-1 in the 0.5-10 keV energy range for an assumed Gamma=2 power law spectral model. A limit of 1.4E-16 erg cm-2 s-1 is derived if we assume that the spectrum of 1H1905+000 in quiescence is described well with a black body of temperature of 0.2 keV. For the upper limit to the source distance of 10 kpc this yields a 0.5-10 keV luminosity limit of 2.4E30 / 1.7E30 erg/s for the abovementioned power law or black body spectrum, respectively. This luminosity limit is lower than the luminosity of A0620-00, the weakest black hole soft X-ray transient in quiescence reported so far. Together with the uncertainties in relating the mass transfer and mass accretion rates we come to the conclusion that the claim that there is evidence for the presence of a black hole event horizon on the basis of a low...

  19. Low resolution 1H NMR assignment of proton populations in pound cake and its polymeric ingredients.

    Science.gov (United States)

    Luyts, A; Wilderjans, E; Waterschoot, J; Van Haesendonck, I; Brijs, K; Courtin, C M; Hills, B; Delcour, J A

    2013-08-15

    Based on a model system approach, five different proton populations were distinguished in pound cake crumb using one dimensional low resolution (1)H NMR spectroscopy. In free induction decay (FID) measurements, proton populations were assigned to (i) non-exchanging CH protons of crystalline starch, proteins and crystalline fat and (ii) non-exchanging CH protons of amorphous starch and gluten, which are in little contact with water. In Carr-Purcell-Meiboom-Gill (CPMG) measurements, three proton populations were distinguished. The CPMG population with the lowest mobility and the FID population with the highest mobility represent the same proton population. The two CPMG proton populations with the highest mobility were assigned to exchanging protons (i.e., protons of water, starch, gluten, egg proteins and sugar) and protons of lipids (i.e., protons of egg yolk lipids and amorphous lipid fraction of margarine) respectively. Based on their spin-lattice relaxation times (T1), two dimensional (1)H NMR spectroscopy further resolved the two proton populations with the highest mobility into three and two proton populations, respectively.

  20. Novel 1H low field nuclear magnetic resonance applications for the field of biodiesel.

    Science.gov (United States)

    Berman, Paula; Leshem, Adi; Etziony, Oren; Levi, Ofer; Parmet, Yisrael; Saunders, Michael; Wiesman, Zeev

    2013-04-16

    Biodiesel production has increased dramatically over the last decade, raising the need for new rapid and non-destructive analytical tools and technologies. 1H Low Field Nuclear Magnetic Resonance (LF-NMR) applications, which offer great potential to the field of biodiesel, have been developed by the Phyto Lipid Biotechnology Lab research team in the last few years. Supervised and un-supervised chemometric tools are suggested for screening new alternative biodiesel feedstocks according to oil content and viscosity. The tools allowed assignment into viscosity groups of biodiesel-petrodiesel samples whose viscosity is unknown, and uncovered biodiesel samples that have residues of unreacted acylglycerol and/or methanol, and poorly separated and cleaned glycerol and water. In the case of composite materials, relaxation time distribution, and cross-correlation methods were successfully applied to differentiate components. Continuous distributed methods were also applied to calculate the yield of the transesterification reaction, and thus monitor the progress of the common and in-situ transesterification reactions, offering a tool for optimization of reaction parameters. Comprehensive applied tools are detailed for the characterization of new alternative biodiesel resources in their whole conformation, monitoring of the biodiesel transesterification reaction, and quality evaluation of the final product, using a non-invasive and non-destructive technology that is new to the biodiesel research area. A new integrated computational-experimental approach for analysis of 1H LF-NMR relaxometry data is also presented, suggesting improved solution stability and peak resolution.

  1. {sup 1}H MR spectroscopy of skeletal muscle, liver and bone marrow

    Energy Technology Data Exchange (ETDEWEB)

    Machann, Juergen [Section on Experimental Radiology, Department of Diagnostic and Interventional Radiology, Eberhard-Karls University Tuebingen, Hoppe-Seyler-Strasse 3, 72076 Tuebingen (Germany)], E-mail: juergen.machann@med.uni-tuebingen.de; Stefan, Norbert [Department of Endocrinology, Metabolism and Pathobiochemistry, Eberhard-Karls University Tuebingen, 72076 Tuebingen (Germany); Schick, Fritz [Section on Experimental Radiology, Department of Diagnostic and Interventional Radiology, Eberhard-Karls University Tuebingen, Hoppe-Seyler-Strasse 3, 72076 Tuebingen (Germany)

    2008-08-15

    Proton magnetic resonance spectroscopy ({sup 1}H MRS) offers interesting metabolic information even from organs outside the brain. In the first part, applications in skeletal muscle for determination of intramyocellular lipids (IMCL), which are involved in the pathogenesis of insulin resistance, are described. Peculiarities of spectral pattern are discussed and studies for short-term regulation of IMCL, as dietary intervention, exercise and fasting are presented. The second part deals with quantification of small amounts of lipids in the liver (hepatic lipids, HL), which is also of increasing interest in the field of diabetes research. Recommendations for correct assessment of spectra in this 'moving organ' are given and the importance of HL is described by examples of a cohort at increased risk for type 2 diabetes. Regulation of HL is described on the basis of a few studies. The third part concentrates on spectral characterization of bone marrow. Peripheral bone marrow of adults consists mainly of fat, while central marrow regions in the pelvis, spinal column and breast bone (and the peripheral bone marrow of children as well) contribute to blood formation and show a variable composition of adipocytes (fat cells), interstitial fluid and water containing precursor cells for erythrocytes, leucocytes and thrombocytes. Adapted {sup 1}H spectroscopic techniques allow a semi-quantitative analysis of bone marrow composition.

  2. High resolution magic angle spinning 1H NMR of childhood brain and nervous system tumours

    Directory of Open Access Journals (Sweden)

    Davies Nigel P

    2009-02-01

    Full Text Available Abstract Background Brain and nervous system tumours are the most common solid cancers in children. Molecular characterisation of these tumours is important for providing novel biomarkers of disease and identifying molecular pathways which may provide putative targets for new therapies. 1H magic angle spinning NMR spectroscopy (1H HR-MAS is a powerful tool for determining metabolite profiles from small pieces of intact tissue and could potentially provide important molecular information. Methods Forty tissue samples from 29 children with glial and primitive neuro-ectodermal tumours were analysed using HR-MAS (600 MHz Varian gHX nanoprobe. Tumour spectra were fitted to a library of individual metabolite spectra to provide metabolite values. These values were then used in a two tailed t-test and multi-variate analysis employing a principal component analysis and a linear discriminant analysis. Classification accuracy was estimated using a leave-one-out analysis and B632+ bootstrapping. Results Glial tumours had significantly (two tailed t-test p Conclusion HR-MAS identified key differences in the metabolite profiles of childhood brain and nervous system improving the molecular characterisation of these tumours. Further investigation of the underlying molecular pathways is required to assess their potential as targets for new agents.

  3. Environmentally Benign Syntheses and Characterization of 4- Aryldihydropyrimidin-2(1H-ones

    Directory of Open Access Journals (Sweden)

    Shafqat Syed Salman

    2017-01-01

    Full Text Available A general, simple, efficient, cost-effective and environmental benign procedure for the syntheses of 4-aryl-3,4-dihydropyrimidin-2(1H-ones (DHPMs has been developed. The reaction is efficiently catalysed by using various amino acids viz., glycine, L-proline, L-cysteine, leucine and tryptophan. Reactions give excellent yields under reflux conditions. The chemical structures of these compounds were identified by Fourier Transform-Infra Red Spectroscopy (FT-IR, Gas Chromatography-Mass Spectroscopy (GC-MS and Nuclear Magnetic Resonance Spectroscopy (1H NMR. Physical parameters such as m.p., mixed m.p. as well as TLC also helped to characterize the expected products. The progress of the reaction time and purity was checked by TLC and the products were purified by recrystallization using ethyl acetate as a solvent. The synthesized molecule has numerous biological applications as it is anti-microbial, anti-inflammatory and anti-hypertensive in character.

  4. Authentication of beef versus horse meat using 60 MHz 1H NMR spectroscopy.

    Science.gov (United States)

    Jakes, W; Gerdova, A; Defernez, M; Watson, A D; McCallum, C; Limer, E; Colquhoun, I J; Williamson, D C; Kemsley, E K

    2015-05-15

    This work reports a candidate screening protocol to distinguish beef from horse meat based upon comparison of triglyceride signatures obtained by 60 MHz (1)H NMR spectroscopy. Using a simple chloroform-based extraction, we obtained classic low-field triglyceride spectra from typically a 10 min acquisition time. Peak integration was sufficient to differentiate samples of fresh beef (76 extractions) and horse (62 extractions) using Naïve Bayes classification. Principal component analysis gave a two-dimensional "authentic" beef region (p=0.001) against which further spectra could be compared. This model was challenged using a subset of 23 freeze-thawed training samples. The outcomes indicated that storing samples by freezing does not adversely affect the analysis. Of a further collection of extractions from previously unseen samples, 90/91 beef spectra were classified as authentic, and 16/16 horse spectra as non-authentic. We conclude that 60 MHz (1)H NMR represents a feasible high-throughput approach for screening raw meat.

  5. Binding of thiocyanate to lactoperoxidase: 1H and 15N nuclear magnetic resonance studies

    Energy Technology Data Exchange (ETDEWEB)

    Modi, S.; Behere, D.V.; Mitra, S. (Tata Institute of Fundamental Research, Bombay (India))

    1989-05-30

    The binding of thiocyanate to lactoperoxidase (LPO) has been investigated by 1H and 15N NMR spectroscopy. 1H NMR of LPO shows that the major broad heme methyl proton resonance at about 61 ppm is shifted upfield by addition of the thiocyanate, indicating binding of the thiocyanate to the enzyme. The pH dependence of line width of 15N resonance of SC15N- in the presence of the enzyme has revealed that the binding of the thiocyanate to the enzyme is facilitated by protonation of an ionizable group (with pKa of 6.4), which is presumably distal histidine. Dissociation constants (KD) of SC15N-/LPO, SC15N-/LPO/I-, and SC15N-/LPO/CN- equilibria have been determined by 15N T1 measurements and found to be 90 +/- 5, 173 +/- 20, and 83 +/- 6 mM, respectively. On the basis of these values of KD, it is suggested that the iodide ion inhibits the binding of the thiocyanate but cyanide ion does not. The thiocyanate is shown to bind at the same site of LPO as iodide does, but the binding is considerably weaker and is away from the ferric ion. The distance of 15N of the bound thiocyanate ion from the iron is determined to be 7.2 +/- 0.2 A from the 15N T1 measurements.

  6. Stopping power of {sup 1}H and {sup 4}He in lithium niobate

    Energy Technology Data Exchange (ETDEWEB)

    Barradas, N.P., E-mail: nunoni@ctn.ist.utl.pt [Centro de Ciências e Tecnologias Nucleares, Instituto Superior Técnico, Universidade de Lisboa, Estrada Nacional 10, ao km 139.7, 2695-066 Bobadela LRS (Portugal); Laboratório de Engenharia Nuclear, Instituto Superior Técnico, Universidade de Lisboa, Estrada Nacional 10, ao km 139.7, 2695-066 Bobadela LRS (Portugal); Marques, J.G. [Centro de Ciências e Tecnologias Nucleares, Instituto Superior Técnico, Universidade de Lisboa, Estrada Nacional 10, ao km 139.7, 2695-066 Bobadela LRS (Portugal); Laboratório de Engenharia Nuclear, Instituto Superior Técnico, Universidade de Lisboa, Estrada Nacional 10, ao km 139.7, 2695-066 Bobadela LRS (Portugal); Alves, E. [Associação Euratom/IST, Instituto de Plasmas e Fusão Nuclear, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, Lisboa 1049-001 (Portugal)

    2014-08-01

    Highlights: •We measured the stopping power of {sup 1}H in LiNbO{sub 3} between 0.27 and 2.33 MeV. •We measured the stopping power of {sup 4}He in LiNbO{sub 3} between 0.44 and 2.33 MeV. •Good agreement was found with SRIM2012 calculations. -- Abstract: Lithium niobate is an important material for applications in bulk optoelectronics and integrated optics devices. Ion beam analysis methods are often used to study this material. However, to our knowledge a single study has been presented in 1996 on measurement of stopping powers in LiNbO{sub 3} at velocities usual in ion beam analysis, for protons and deuterons near the stopping power maximum. The results were 15% lower than the values calculated from the elemental Li, Nb and O stopping powers then available together with the Bragg rule. In practice, all ion beam analysis studies of LiNbO{sub 3} still use the Bragg rule. We have used a bulk method, previously developed by us and applied successfully to other systems, to determine experimentally the stopping power of lithium niobate for {sup 1}H and {sup 4}He ions in the energy range 0.3–2.3 MeV. The results of our measurements and bulk method analysis are presented and discussed in the context of currently available stopping power calculations.

  7. Spectroscopic and thermal studies on 2- and 4-phenyl-1H-imidazoles

    Science.gov (United States)

    Hachuła, Barbara; Polasz, Anna; Książek, Maria; Kusz, Joachim; Starczewska, Oliwia; Pisarski, Wojciech

    2017-08-01

    The polarized IR spectra of isotopically neat and isotopically substituted monocrystalline samples of 2-phenyl-1H-imidazole (2PI) and 4-phenyl-1H-imidazole (4PI) were recorded at two temperatures of 293 K and 77 K. The room-temperature ATR-FTIR and Raman spectra of 2PI and two polymorphic forms of 4PI were also recorded. Theoretical analysis of the vibrational spectra of selected imidazole derivatives reflected similar characteristics of their hydrogen-bond networks and allowed us to obtain the information about the mechanism of the H/D isotopic ;self-organization; phenomenon. The distribution of protons and deuterons in the lattices of the isotopically diluted crystalline samples of 2PI and 4PI was found to be non-random. In the crystals of the hydrogen- and deuterium-bonded imidazole derivatives the strongest vibrational exciton interactions favored the intrachain (;tail-to-head;)-type exciton coupling widespread at 77 K via the π-electrons. At room temperature a weak interchain (;through-space;)-type exciton coupling was also partially responsible for the IR spectra generation. Differential scanning calorimetry (DSC) measurements showed that the two polymorphic forms of 4PI exhibit an extensive supercooling of crystallization process and cold crystallization on reheating. Additionally, both polymorphic modifications of 4PI are monotropically related. 2PI exhibits only the crystallization and melting processes.

  8. Insight into Metabolic 1H-MRS Changes in Natalizumab Induced Progressive Multifocal Leukoencephalopathy Brain Lesions

    Directory of Open Access Journals (Sweden)

    Ruth Schneider

    2017-09-01

    Full Text Available BackgroundProgressive multifocal leukoencephalopathy (PML is a severe complication of immunosuppressive therapies, especially of natalizumab in relapsing–remitting multiple sclerosis (MS. Metabolic changes within PML lesions have not yet been described in natalizumab-associated PML in MS patients.ObjectiveTo study metabolic profiles in natalizumab-associated PML lesions of MS patients by 1H magnetic resonance spectroscopy (1H-MRS at different stages during the PML course. To assess changes associated with the occurrence of the immune reconstitution inflammatory syndrome (IRIS.Methods20 patients received 1H-MRS and imaging at 3 T either in the pre-IRIS, IRIS, early-post-PML, or late post-PML setting. Five of these patients received individual follow-up examinations, including the pre-IRIS or IRIS phase. Clinical worsening was described by changes in the Karnofsky Performance Scale (KPS and the expanded disability status scale (EDSS 1 year before PML and scoring at the time of 1H-MRS.ResultsIn PML lesions, increased levels of the Lip/Cr ratio, driven by rising of lipid and reduction of Creatine, were found before the occurrence of IRIS (p = 0.014 with a maximum in the PML–IRIS group (p = 0.004. By contrast, marked rises of Cho/Cr in PML lesions were detected exclusively during the IRIS phase (p = 0.003. The Lip/Cr ratio decreased to above-normal levels in early-post-PML (p = 0.007, compared to normal appearing white matter (NAWM and to normal levels in the late-post-PML group. NAA/Cho was reduced compared to NAWM in the pre-IRIS, IRIS, and early-post-PML group. In NAA/Cr, the same effect was seen in the pre-IRIS and early-post-PML group. These cross-sectional results were confirmed by the individual follow-up examinations of four patients. NAA/Cho, Cho/Cr, and the lipid rise relative to NAWM in PML lesions were significantly correlated with the residual clinical worsening (KPS change in post-PML patients (Spearman

  9. Heteronuclear 19F-1H statistical total correlation spectroscopy as a tool in drug metabolism: study of flucloxacillin biotransformation.

    Science.gov (United States)

    Keun, Hector C; Athersuch, Toby J; Beckonert, Olaf; Wang, Yulan; Saric, Jasmina; Shockcor, John P; Lindon, John C; Wilson, Ian D; Holmes, Elaine; Nicholson, Jeremy K

    2008-02-15

    We present a novel application of the heteronuclear statistical total correlation spectroscopy (HET-STOCSY) approach utilizing statistical correlation between one-dimensional 19F/1H NMR spectroscopic data sets collected in parallel to study drug metabolism. Parallel one-dimensional (1D) 800 MHz 1H and 753 MHz 19F{1H} spectra (n = 21) were obtained on urine samples collected from volunteers (n = 6) at various intervals up to 24 h after oral dosing with 500 mg of flucloxacillin. A variety of statistical relationships between and within the spectroscopic datasets were explored without significant loss of the typically high 1D spectral resolution, generating 1H-1H STOCSY plots, and novel 19F-1H HET-STOCSY, 19F-19F STOCSY, and 19F-edited 1H-1H STOCSY (X-STOCSY) spectroscopic maps, with a resolution of approximately 0.8 Hz/pt for both nuclei. The efficient statistical editing provided by these methods readily allowed the collection of drug metabolic data and assisted structure elucidation. This approach is of general applicability for studying the metabolism of other fluorine-containing drugs, including important anticancer agents such as 5-fluorouracil and flutamide, and is extendable to any drug metabolism study where there is a spin-active X-nucleus (e.g., 13C, 15N, 31P) label present.

  10. Response to the Letter to the Editor regarding "Determination of the fatty acid profile by 1H-NMR spectroscopy."

    Science.gov (United States)

    In expansion of previous work (G. Knothe, J.A. Kenar, Determination of the fatty acid profile by 1H-NMR spectroscopy, Eur. J. Lipid Sci. Technol. 2004, 106, 88-96), an additional approach is discussed for quantitating saturated fatty acids in the fatty acid profiles of common vegetable oils by 1H-NM...

  11. Analysis of Cross-Polarization Dynamics between Two Abundant Nuclei, 19F and 1H, Based on Spin Thermodynamics Theory

    Science.gov (United States)

    Ando, Shinji; Harris, Robin K.; Reinsberg, Stefan A.

    1999-11-01

    The phenomenological theory of spin thermodynamics based on the spin temperature hypothesis was employed to describe the cross-polarization (CP) dynamics between two abundant nuclei, 19F and 1H, when the number of fluorine atoms is not substantially less than the number of hydrogens. The influence of T1ρ's of both nuclei and the relative magnitude (heat capacity) of the two spin baths must be incorporated explicitly into the analysis in order to derive values for the parameters involved in the CP dynamics. Numerical calculations were performed to clarify the difference in the evolution of magnetization in variable contact time CP experiments between the 1H → 13C and 1H → 19F cases. A new type of CP-drain experiment was developed for observing the residual 1H magnetization after 1H → 19F CP. 19F direct polarization magic-angle spinning (MAS), 1H → 19F CP, and 1H → 19F CP-drain MAS NMR spectra have been measured for a fluorinated polyimide, 6FDA/ODA. The CP dynamics between 1H and 19F for the polyimide were analyzed on the basis of the spin thermodynamics theory. The constant for polarization transfer (THF) was determined by the analysis using the effective CP parameters, which were directly obtained from the CP and CP-drain experiments, together with independently measured values of TH1ρ and TF1ρ.

  12. 1-Phenylpyrazolo[4',3':5,6]pyrano[3,2-c]pyridine-4(1H-thione

    Directory of Open Access Journals (Sweden)

    Wolfgang Holzer

    2010-04-01

    Full Text Available The title compound is prepared by treatment of 1-phenylpyrazolo[4',3':5,6]pyrano[3,2-c]pyridin-4(1H-one with Lawesson’s reagent in refluxing toluene. Detailed spectroscopic data (1H NMR, 13C NMR, 15N NMR, MS are presented.

  13. 1H NMR of High-Potential Iron-Sulfur Protein from the Purple Non-Sulfur Bacterium Rhodoferax fermentans

    DEFF Research Database (Denmark)

    Ciurli, Stefano; Cremonini, Mauro Andrea; Kofod, Pauli

    1996-01-01

    Oxidized and reduced forms of high-potential iron-sulfur protein (HiPIP) from the purple non-sulfur photosynthetic bacterium Rhodoferux fermentans have been characterized using 1H-NMR spectroscopy. Pairwise and sequence-specific assignments of hyperfine-shifted 1H-NMR signals to protons of cysteine...

  14. Can {sup 1}H MR Spectroscopy be Used to Assess the Success of Uterine Artery Embolisation?

    Energy Technology Data Exchange (ETDEWEB)

    Macnaught, Gillian, E-mail: gillian.macnaught@ed.ac.uk [University of Edinburgh, Clinical Research Imaging Centre, Queen’s Medical Research Institute (United Kingdom); Ananthakrishnan, G., E-mail: a.radiology@gmail.com [Gartnavel General Hospital, Interventional Radiology Unit (United Kingdom); Hinksman, L., E-mail: laurahinksman@nhs.net [Wishaw General Hospital, Radiology Department (United Kingdom); Yadavali, R., E-mail: reddi.yadavali@nhs.net [Gartnavel General Hospital, Interventional Radiology Unit (United Kingdom); Bryden, F., E-mail: Fiona.Bryden@ggc.scot.nhs.uk [Stobhill Hospital, Radiology Department (United Kingdom); Lassman, S., E-mail: Sue.Lassman@ggc.scot.nhs.uk [Gartnavel General Hospital, Radiology Department (United Kingdom); Ritchie, M., E-mail: moirasim9@gmail.com [Gartnavel General Hospital, Interventional Radiology Unit (United Kingdom); Gallacher, K., E-mail: k.gallacher.3@research.gla.ac.uk [University of Glasgow, School of Mathematics and Statistics, University Gardens (United Kingdom); Hay, C., E-mail: c.hay@nhs.net [Royal Infirmary of Edinburgh, Interventional Radiology (United Kingdom); Moss, J. G., E-mail: jon.moss@ggc.scot.nhs.uk [Gartnavel General Hospital, Interventional Radiology Unit (United Kingdom)

    2016-03-15

    PurposeAbsence of contrast on contrast enhanced MRI (CEMRI) and reduction in uterine volume at 6 months post-uterine artery embolisation (UAE) currently indicate the successful disruption of the fibroid blood supply by UAE. This study assesses whether {sup 1}H MR spectroscopy ({sup 1}H MRS) can also indicate the success of UAE.Method20 patients with symptomatic fibroids were randomised 1:1 to undergo UAE with either Gelfoam or Embospheres. CEMRI and spectra (1.5 T) were acquired pre-, 24-h and 6 months post-UAE. LCModel was used to detect significant levels of choline, creatine and lactate in fibroid spectra. Uterine volumes were measured and paired t tests (p < 0.05) assessed volume reduction over time. Qualitative assessments of CEMRI were performed.ResultsCholine was detected in 17/18 spectra pre-UAE, 12/14 at 24-h and 6/16 at 6 months post-UAE. Choline was not detected in the 7/7 spectra available for the Embospheres group at 6 months. These fibroids were non-enhancing on CEMRI and associated with a significant reduction in mean uterine volume at 6 months (mean/min/max 396.5/84.1/997.5 cm{sup 3}, p = 0.003). Choline was detected in 6/9 fibroid spectra available for the Gelfoam group at 6 months. Of these fibroids, four demonstrated persistent enhancement on CEMRI and two were non-enhancing. This group did not demonstrate significant uterine volume reduction (mean/min/max 117.2/−230.6/382.6 cm{sup 3}, p = 0.15). The negative minimum value indicates fibroid growth.ConclusionsThis study has demonstrated the potential of {sup 1}H MRS to provide an additional marker of the success of UAE.

  15. Registration pipeline for pulmonary free-breathing 1H MRI ventilation measurements

    Science.gov (United States)

    Guo, Fumin; Capaldi, Dante P. I.; Di Cesare, Robert; Fenster, Aaron; Parraga, Grace

    2017-03-01

    Objectives: Our aim was to develop a clinically-practical and physiologically-relevant approach for regional structure-function measurements of the lung using Fourier decomposition of free-breathing pulmonary magnetic resonance imaging (FDMRI). Methods: Ten patients with chronic obstructive pulmonary disease provided written informed consent to a study protocol approved by Health Canada and completed pulmonary function tests, 1H/hyperpolarized noble gas and free-breathing pulmonary magnetic resonance imaging (MRI) during a single 2-hour visit. Free-breathing 1H MRI was simultaneously segmented using a multi-region coupled continuous max-flow approach by exploring primal/dual analysis and convex optimization techniques. The segmented free-breathing 1H MRI lung was registered using deformable registration approach that was developed using dual and convex optimization methods to compensate for respiratory/cardiac motion. Fourier decomposition of the co-registered lung was used to generate pulmonary functional information that was quantified as ventilation-defect-percent (VDP). The pipeline was implemented on a GPU for speed-up. Lung segmentation accuracy was measured by comparing algorithm and manual lung masks using Dice-similarity-coefficient (DSC). FD-VDP was compared to 3He-VDP using Pearson correlation coefficient and Bland-Altman analysis. The reproducibility of our algorithm was measured using coefficient of variation (CoV) and intraclass correlation coefficient (ICC) for DSC and FD-VDP. Results: The pipeline yielded a whole lung DSC of 95.7+/-1.7% and FD-VDP that were correlated with 3He-VDP (r = 0.81, p = 0.004). CoV (ICC) were 0.4% (0.98) and 4.1% (0.98) for whole lung DSC and FD-VDP, respectively. The proposed approach requires 45 min for parallel implementation with minimal user interaction. Conclusion: The proposed approach provides a clinically-practical pipeline to generate regional pulmonary structure-function measurements using free

  16. Monoclonal antibody against recombinant Fasciola gigantica cathepsin L1H could detect juvenile and adult cathepsin Ls of Fasciola gigantica.

    Science.gov (United States)

    Wongwairot, Sirima; Kueakhai, Pornanan; Changklungmoa, Narin; Jaikua, Wipaphorn; Sansri, Veerawat; Meemon, Krai; Songkoomkrong, Sineenart; Riengrojpitak, Suda; Sobhon, Prasert

    2015-01-01

    Cathepsin Ls (CatLs), the major cysteine protease secreted by Fasciola spp., are important for parasite digestion and tissue invasion. Fasciola gigantica cathepsin L1H (FgCatL1H) is the isotype expressed in the early stages for migration and invasion. In the present study, a monoclonal antibody (MoAb) against recombinant F. gigantica cathepsin L1H (rFgCatL1H) was produced by hybridoma technique using spleen cells from BALB/c mice immunized with recombinant proFgCatL1H (rproFgCatL1H). This MoAb is an immunoglobulin (Ig)G1 with κ light chain isotype. The MoAb reacted specifically with rproFgCatL1H, the native FgCatL1H at a molecular weight (MW) 38 to 48 kDa in the extract of whole body (WB) of metacercariae and newly excysted juvenile (NEJ) and cross-reacted with rFgCatL1 and native FgCatLs at MW 25 to 28 kDa in WB of 2- and 4-week-old juveniles, adult, and adult excretory-secretory (ES) fractions by immunoblotting and indirect ELISA. It did not cross-react with antigens in WB fractions from other parasites, including Gigantocotyle explanatum, Paramphistomum cervi, Gastrothylax crumenifer, Eurytrema pancreaticum, Setaria labiato-papillosa, and Fischoederius cobboldi. By immunolocalization, MoAb against rFgCatL1H reacted with the native protein in the gut of metacercariae and NEJ and also cross-reacted with CatL1 in 2- and 4-week-old juveniles and adult F. gigantica. Therefore, FgCatL1H and its MoAb may be used for immunodiagnosis of both early and late fasciolosis in ruminants and humans.

  17. Bis[μ-1-(2-pyridylmethyl-1H-benzotriazole]disilver(I bis(perchlorate

    Directory of Open Access Journals (Sweden)

    Chun-Sen Liu

    2009-11-01

    Full Text Available In the title centrosymmetric binuclear AgI complex, [Ag2(C12H10N42](ClO42, each AgI center is two-coordinated by one pyridine and one benzotriazole N-donor atom of two inversion-related 1-(2-pyridylmethyl-1H-benzotriazole (L ligands. This forms a unique box-like cyclic dimer with an intramolecular Ag...Ag separation of 4.479 (2 Å. Intermolecular C—H...O hydrogen-bonding interactions, involving uncoordinated ClO4− ions, link the binuclear units, forming a two-dimensional network parallel to (10overline{2}.

  18. Faster metabolite (1H transverse relaxation in the elder human brain.

    Directory of Open Access Journals (Sweden)

    Małgorzata Marjańska

    Full Text Available (1H magnetic resonance spectroscopy (MRS is unique among imaging modalities because signals from several metabolites are measured during a single examination period. Each metabolite reflects a distinct intracellular process. Furthermore transverse (T2 relaxation times probe the viability of the cell microenvironment, e.g., the viscosity of the cellular fluids, the microscopic susceptibility distribution within the cells, and the iron content. In this study, T2s of brain metabolites were measured in the occipital lobe of eighteen young and fourteen elderly subjects at a field strength of 4 tesla. The T2s of N-acetylaspartate, total creatine, and total choline were 23%, 16% and 10% shorter in elderly than in young subjects. The findings of this study suggest that noninvasive detection of T2 provides useful biological information on changes in the cellular microenvironment that take place during aging.

  19. 5-Methyl-1-[(4-methylphenylsulfonyl]-1H-pyrazol-3-yl 4-methylbenzenesulfonate

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    Shahzad Murtaza

    2012-07-01

    Full Text Available In the title compound, C18H18N2O5S2, the tolyl rings are oriented at a dihedral angle of 16.15 (11° with respect to one another. The 5-methyl-1H-pyrazol-3-ol ring is roughly planar (r.m.s. deviation = 0.0231 Å and subtends angles of 73.82 (8 and 89.85 (8° with the tolyl rings. In the crystal, very weak π–π interactions between tolyl groups, with centroid–centroid distances of 4.1364 (19 and 4.0630 (16 Å, together with a C—H...π contact generate a three-dimensional network.

  20. Characterization of PTCDA nanocrystals on Ge(0 0 1):H-(2 × 1) surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Ahmad Zebari, Amir A.; Kolmer, Marek; Prauzner-Bechcicki, Jakub S., E-mail: jakub.prauzner-bechcicki@uj.edu.pl

    2015-03-30

    Highlights: • We characterize self-assembled PTCDA molecular islands on Ge(0 0 1):H-(2 × 1) surfaces. • Preferred orientation, height, shape and internal structure are identified. • Electronic properties and stability of nanocrystals are discussed. - Abstract: We analyze self-assembled nanocrystals of 3,4,9,10-perylene tetracarboxylic dianhydride (PTCDA) molecules on hydrogen passivated Ge(0 0 1) surfaces with use of scanning tunneling microscopy (STM) and spectroscopy (STS). At 0.7ML coverage, 2.1 nm high, elongated, hexagonal islands inclined at 37° with respect to the substrate row are mostly observed. By measuring the differential tunneling conductance, we observe an effect of electronic decoupling of the nanocrystals due to the introduced passivating layer. Finally, we shortly discuss the stability of the islands and their interaction with the scanning probe in the ultra-high vacuum environment.

  1. Composition of beer by 1H NMR spectroscopy: effects of brewing site and date of production.

    Science.gov (United States)

    Almeida, Cláudia; Duarte, Iola F; Barros, António; Rodrigues, João; Spraul, Manfred; Gil, Ana M

    2006-02-08

    A principal component analysis (PCA) of 1H NMR spectra of beers differing in production site (A, B, C) and date is described, to obtain information about composition variability. First, lactic and pyruvic acids contents were found to vary significantly between production sites, good reproducibility between dates being found for site A but not for sites B and C beers. Second, site B beers were clearly distinguished by the predominance of linear dextrins, while A and C beers were richer in branched dextrins. Carbohydrate reproducibility between dates is poorer for site C with dextrin branching degree varying significantly. Finally, all production sites were successfully distinguished by their contents in adenosine/inosine, uridine, tyrosine/tyrosol, and 2-phenylethanol, reproducibility between dates being again poorer for site C. Interpretation of the above compositional differences is discussed in terms of the biochemistry taking place during brewing, and possible applications of the method in brewing process control are envisaged.

  2. 3-Amino-1-(4-fluorophenyl-8-methoxy-1H-benzo[f]chromene-2-carbonitrile

    Directory of Open Access Journals (Sweden)

    Ahmed M. El-Agrody

    2013-04-01

    Full Text Available The title compound, C21H15FN2O2, features an approximately planar 1H-benzo[f]chromene fused-ring system (r.m.s. deviation for the 14 non-H atoms = 0.052 Å, with the fluorobenzene ring being almost perpendicular to this [dihedral angle = 85.30 (7 °]. The furan ring has a flattened half-chair conformation, with the methine C atom deviating by 0.132 (2 Å from the plane of the remaining atoms (r.m.s. deviation = 0.0107 Å. In the crystal, inversion dimers are formed via pairs of amine–cyano N—H...N hydrogen bonds. The dimers are connected into a three-dimensional architecture by C—H...N(cyano, C—H...π and π–π [intercentroid distance = 3.6671 (10 Å] interactions.

  3. High-resolution /sup 1/H NMR study of the solution structure of delta-hemolysin

    Energy Technology Data Exchange (ETDEWEB)

    Tappin, M.J.; Pastore, A.; Norton, R.S.; Freer, J.H.; Campbell, I.D.

    1988-03-08

    The 26-residue toxin from Staphylococcus aureus delta-hemolysin, is thought to act by traversing the plasma membrane. The structure of this peptide, in methanol solution, has been investigated by using high-resolution NMR in combination with molecular dynamics calculations. The /sup 1/H NMR spectrum has been completely assigned, and it is shown that residues 2-20 form a relatively stable helix while the residues at the C-terminal end appear to be more flexible. The structures were calculated only from nuclear Overhauser effect data and standard bond lengths. It is shown that the results are consistent with /sup 3/J/sub NH-..cap alpha..CH/ coupling constants and amide hydrogen exchange rates.

  4. Inhibition of myeloperoxidase: evaluation of 2H-indazoles and 1H-indazolones.

    Science.gov (United States)

    Roth, Aaron; Ott, Sean; Farber, Kelli M; Palazzo, Teresa A; Conrad, Wayne E; Haddadin, Makhluf J; Tantillo, Dean J; Cross, Carroll E; Eiserich, Jason P; Kurth, Mark J

    2014-11-15

    Myeloperoxidase (MPO) produces hypohalous acids as a key component of the innate immune response; however, release of these acids extracellularly results in inflammatory cell and tissue damage. The two-step, one-pot Davis-Beirut reaction was used to synthesize a library of 2H-indazoles and 1H-indazolones as putative inhibitors of MPO. A structure-activity relationship study was undertaken wherein compounds were evaluated utilizing taurine-chloramine and MPO-mediated H2O2 consumption assays. Docking studies as well as toxicophore and Lipinski analyses were performed. Fourteen compounds were found to be potent inhibitors with IC50 values <1μM, suggesting these compounds could be considered as potential modulators of pro-oxidative tissue injury pertubated by the inflammatory MPO/H2O2/HOCl/HOBr system.

  5. Assessing Heterogeneity of Osteolytic Lesions in Multiple Myeloma by 1H HR-MAS NMR Metabolomics

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    Laurette Tavel

    2016-10-01

    Full Text Available Multiple myeloma (MM is a malignancy of plasma cells characterized by multifocal osteolytic bone lesions. Macroscopic and genetic heterogeneity has been documented within MM lesions. Understanding the bases of such heterogeneity may unveil relevant features of MM pathobiology. To this aim, we deployed unbiased 1H high-resolution magic-angle spinning (HR-MAS nuclear magnetic resonance (NMR metabolomics to analyze multiple biopsy specimens of osteolytic lesions from one case of pathological fracture caused by MM. Multivariate analyses on normalized metabolite peak integrals allowed clusterization of samples in accordance with a posteriori histological findings. We investigated the relationship between morphological and NMR features by merging morphological data and metabolite profiling into a single correlation matrix. Data-merging addressed tissue heterogeneity, and greatly facilitated the mapping of lesions and nearby healthy tissues. Our proof-of-principle study reveals integrated metabolomics and histomorphology as a promising approach for the targeted study of osteolytic lesions.

  6. Ethyl 4-[3-(1H-imidazol-1-ylpropylamino]-3-nitrobenzoate

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    Hoong-Kun Fun

    2011-10-01

    Full Text Available In the title compound, C15H18N4O4, the 1H-imidazole ring forms a dihedral angle of 67.12 (8° with the benzene ring. An S(6 ring motif is formed via an intramolecular N—H...O hydrogen bond. In the crystal, neighbouring molecules are linked by a pair of intermolecular N—H...N hydrogen bonds, forming an inversion dimer. The dimers are further linked by a pair of C—H...O hydrogen bonds, leading to the formation of chain along [021]. A C—H...π interaction involving the centroid of the benzene ring is also observed between the chains.

  7. Low-field (1)H NMR spectroscopy for distinguishing between arabica and robusta ground roast coffees.

    Science.gov (United States)

    Defernez, Marianne; Wren, Ella; Watson, Andrew D; Gunning, Yvonne; Colquhoun, Ian J; Le Gall, Gwénaëlle; Williamson, David; Kemsley, E Kate

    2017-02-01

    This work reports a new screening protocol for addressing issues of coffee authenticity using low-field (60MHz) bench-top (1)H NMR spectroscopy. Using a simple chloroform-based extraction, useful spectra were obtained from the lipophilic fraction of ground roast coffees. It was found that 16-O-methylcafestol (16-OMC, a recognized marker compound for robusta beans) gives rise to an isolated peak in the 60MHz spectrum, which can be used as an indicator of the presence of robusta beans in the sample. A total of 81 extracts from authenticated coffees and mixtures were analysed, from which the detection limit of robusta in arabica was estimated to be between 10% and 20% w/w. Using the established protocol, a surveillance exercise was conducted of 27 retail samples of ground roast coffees which were labelled as "100% arabica". None were found to contain undeclared robusta content above the estimated detection limit.

  8. 5-Amino-1H-1,2,4-triazol-4-ium-3-carboxylate hemihydrate

    Directory of Open Access Journals (Sweden)

    José A. Fernandes

    2011-08-01

    Full Text Available The asymmetric unit of the title compound, C3H4N4O2·0.5H2O, comprises two whole molecules of 5-amino-1H-1,2,4-triazole-3-carboxylic acid in its zwitterionic form (proton transfer occurs from the carboxylic acid group to the N heteroatom at position 1, plus one water molecule of crystallization. The organic moieties are disposed into supramolecular layers linked by N—H...O and N—H...N hydrogen bonds parallel to the bc plane. Additional O—H...O and N—H...O hydrogen bonds involving the water molecules and the organic molecules lead to the formation of double-deck supramolecular arrangements which are interconnected along the a axis via π–π stacking [centroid–centroid distance = 3.507 (3 Å].

  9. Complete 1H NMR assignments of pyrrolizidine alkaloids and a new eudesmanoid from Senecio polypodioides.

    Science.gov (United States)

    Villanueva-Cañongo, Claudia; Pérez-Hernández, Nury; Hernández-Carlos, Beatriz; Cedillo-Portugal, Ernestina; Joseph-Nathan, Pedro; Burgueño-Tapia, Eleuterio

    2014-05-01

    Chemical investigation of the aerial parts of Senecio polypodioides lead to the isolation of the new eudesmanoid 1β-angeloyloxyeudesm-7-ene-4β,9α-diol (1) and the known dirhamnosyl flavonoid lespidin (3), while from roots, the known 7β-angeloyloxy-1-methylene-8α-pyrrolizidine (5) and sarracine N-oxide (6), as well as the new neosarracine N-oxide (8), were obtained. The structure of 1 and 8 was elucidated by spectral means. Complete assignments of the (1)H NMR data for 5, 6, sarracine (7), and 8 were made using one-dimensional and two-dimensional NMR experiments and by application of the iterative full spin analysis of the PERCH NMR software.

  10. Diaqua(5-methyl-1H-pyrazole-3-carboxylato(4-nitrobenzoatocopper(II

    Directory of Open Access Journals (Sweden)

    Shan-shan Zhang

    2009-02-01

    Full Text Available In the title complex, [Cu(C7H4NO4(C5H5N2O2(H2O2], the CuII ion is coordinated in a slightly distorted square-pyramidal enviroment. The basal plane is formed by an N atom and an O atom from a 5-methyl-1H-pyrazole-3-carboxylate ligand and by two O atoms from two water ligands. The apical position is occupied by a carboxylate O atom from a 4-nitrobenzoate ligand. In the crystal structure, intermolecular O—H...O and N—H...O hydrogen bonds link complex moleclues, forming extended chains parallel to the a axis.

  11. Total assignment of 1H and 13C NMR data for the sesquiterpene lactone 15-deoxygoyazensolide.

    Science.gov (United States)

    Heleno, Vladimir Constantino Gomes; Crotti, Antônio Eduardo Miller; Constantino, Mauricio Gomes; Lopes, Norberto Peporine; Lopes, João Luis Callegari

    2004-03-01

    We describe a complete analysis of the 1H and 13C spectra of the anti-inflamatory, schistossomicidal and trypanosomicidal sesquiterpene lactone 15-deoxygoyazensolide. This lactone, with a structure similar to other important ones, was studied by NMR techniques such as COSY, HMQC, HMBC, Jres and NOE experiments. The comparison of the data with some computational results led to an unequivocal assignment of all hydrogen and carbon chemical shifts, even eliminating some previous ambiguities. We were able to determine all hydrogen coupling constants (J) and signal multiplicities and to confirm the stereochemistry. A new method for the determination of the relative position of the lactonization and the position of the ester group on a medium-sized ring by NMR was developed.

  12. Tetra-μ-oxido-tetrakis{dioxido[3-(2-pyridyl-1H-pyrazole]molybdenum(VI}

    Directory of Open Access Journals (Sweden)

    Dacheng Li

    2009-09-01

    Full Text Available In the title compound, [Mo4O12(C8H7N34], the MoVI ion has a distorted octahedral coordination completed by two terminal O atoms, two μ-oxide atoms and two N atoms from one 3-(2-pyridyl-1H-pyrazole ligand. It is noteworthy that in the tetranuclear unit (overline4 symmetry, any three MoVI atoms define a plane, and the fourth lies 1.8 (1 Å out of that plane. The degree of linearity of the oxide bridges between two Mo atoms is 175.38 (13°. Moreover, the N—H group forms an intramolecular hydrogen bond (four per molecule.

  13. A subzero 1H NMR relaxation investigation of water dynamics in tomato pericarp.

    Science.gov (United States)

    Foucat, Loïc; Lahaye, Marc

    2014-09-01

    (1)H NMR relaxation times (T1 and T2) were measured at low field (0.47 T) in pericarp tissues of three tomato genotypes (Ferum, LA0147 and Levovil) at subzero temperature (-20 °C) and two ripening stages (mature green and red). The unfrozen water dynamics was characterised by two T1 and three T2 components. The relaxation time values and their associated relative populations allowed differentiating the ripening stage of only LA0147 and Levovil lines. But the three genotypes were unequivocally discriminated at the red ripe stage. The unfrozen water distribution was discussed in terms of specific interactions, especially with sugars, in relation with their osmoprotectant effects.

  14. 1H NMR Study of Polyvinylalcohol Irradiated by Ultra-violet

    Institute of Scientific and Technical Information of China (English)

    Xiu Ling YAN; Wan Fu SUN; Jun TANG; Xin ZHAO

    2005-01-01

    The effect of Ultra-violet light on the structure and motion of the polyvinyl alcohol(PVA) chains was studied by 1H NMR, spin-lattice relaxation and IR spectroscopy. The results indicated that with the increase of irradiation time, the intensity of the polymer hydroxyl proton peaks decreased and finally vanished, which suggested the self-condensation between the hydroxyl groups proceeded. No methyl proton peaks appeared in the spectra after irradiation shows that there is no cleavage of polymer chain. The longer the irradiation time is, the wider the proton peak of the residual water of the solvent is and it shifted toward low field. This result implies that the hydrogen bonds formed between the polymer and the residual water. The absorption peak of hydroxyl group of the polymer moves toward the lower wave number in the IR spectrum that showed the existence of the hydrogen bonds between the PVA macromolecules.

  15. Design, synthesis and evaluation of 5-substituted 1-H-tetrazoles as potent anticonvulsant agents.

    Science.gov (United States)

    Liao, Ai-Mei; Wang, Tiantian; Cai, Bangrong; Jin, Yi; Cheon, Seunghoon; Chun, ChangJu; Wang, Zengtao

    2017-04-01

    A series of 5-substituted 1-H-tetrazoles were designed and synthesized as potent anticonvulsant agents. Their preliminary anticonvulsant activities were evaluated using maximal electroshock and subcutaneous pentylenetetrazole (scPTZ) seizure tests. Neurotoxicity was determined using rotarod test. The results indicated that the compound 2j in scPTZ model exhibited the ED50 values of 83.3 mg/kg, superior to the standard drug ethosuximide with the maximum activity. In addition, compound 2k showed the most potent activity in MES model with ED50 value of 9.6 mg/kg and TD50 value of 189.5 mg/kg after intraperitoneal injection in mice, and displayed a high protective index (TD50/ED50) of 19.7 compared to reference antiepileptic drugs.

  16. Theoretical and experimental investigation of the 1H NMR spectrum of putrescine

    Science.gov (United States)

    Allouche, A. R.; Graveron-Demilly, D.; Fauvelle, F.; Aubert-Frécon, M.

    2008-12-01

    Chemical shifts δ and spin-spin coupling constants J have been calculated for the putrescine molecule, a polyamine present in prostate tissue, through a DFT/B3LYP/6-311++G(d,p)/PCM/(GIAO) approach, which has been shown to be accurate in previous work. From δ and J values, calculated for the first time for the isolated and the solvated putrescine, the 1H NMR spectra have been simulated. Comparisons between the calculated and the experimental NMR spectra at 400 MHz show a good agreement and allow to propose reliable values for the NMR spin Hamiltonian parameters of putrescine to be used as good starting values for further quantitation methods of metabolites in prostate tissue.

  17. Synthesis of new 1H-1,2,3-triazole-1,4-naphthoquinones

    Directory of Open Access Journals (Sweden)

    Wagner O. Valença

    2012-06-01

    Full Text Available In this work, were synthesized new 1H-1,2,3-triazole-1,4-naphthoquinones via 1,3-dipolar cycloaddition reaction using CuI/acetonitrile without addition of base or ligand. The compounds (3a-i were obtained in moderate-to-good yields 45-92%. To prepare (3d, we obtain a mixture of (3d and (4 in a ratio 3:1, that it was difficult to separate. The low yield for the compound (3f can be also justified based in the formation of aminonaphthoquinone (4. The acetylation of (3h and (3i afforded the compounds (5 and (6 in 77% and 35% of yields, respectively. The low yield of (6 was due to formation of 35 % of the elimination product (7.

  18. Synthesis of aryl-1H-1,2,3-triazoles via 1,3-dipolar cycloaddition

    Directory of Open Access Journals (Sweden)

    Wagner O. Valença

    2012-06-01

    Full Text Available A series of Aryl-1H-1,2,3-triazoles were prepared from the reaction between aril-azide (1 with 1.5 equiv. of terminal alkynes (2a-o. The reactions carried out at room temperature and in the presence of CuI (10 mol% in acetonitrile. The compounds (3a-o were obtained in moderate-to-good yields (50-94%. In general, not was observed significant inductive effect on the reactivity of the alkynes (2a-f. The alcohol alkynes (2i-k showed moderate yields 50-72%. On the other hand, the reaction with alkyl alkynes (2m,n furnished the compounds (3m and (3n in excellent yields of 89% and 90%, respectively.

  19. (1) H-NMR with Multivariate Analysis for Automobile Lubricant Comparison.

    Science.gov (United States)

    Kim, Siwon; Yoon, Dahye; Lee, Dong-Kye; Yoon, Changshin; Kim, Suhkmann

    2017-02-23

    Identification of suspected automobile-related lubricants could provide valuable information in forensic cases. We examined that automobile lubricants might exhibit the chemometric characteristics to their individual usages. To compare the degree of clustering in the plots, we co-plotted general industrial oils that were highly dissimilar with automobile lubricants in additive compositions. (1) H-NMR spectroscopy was used with multivariate statistics as a tool for grouping, clustering, and identification of automobile lubricants in laboratory conditions. We analyzed automobile lubricants including automobile engine oils, automobile transmission oils, automobile gear oils, and motorcycle oils. In contrast to the general industrial oils, automobile lubricants showed relatively high tendencies of clustering to their usages. Our pilot study demonstrated that the comparison of known and questioned samples to their usages might be possible in forensic fields.

  20. Classification of Wines Based on Combination of 1H NMR Spectroscopy and Principal Component Analysis

    Institute of Scientific and Technical Information of China (English)

    DU, Yuan-Yuan; BAI, Guo-Yun; ZHANG, Xu; LIU, Mai-Li

    2007-01-01

    A combination of 1H nuclear magnetic resonance (NMR) spectroscopy and principal component analysis (PCA)has shown the potential for being a useful method for classification of type, production origin or geographic origin of wines. In this preliminary study, twenty-one bottled wines were classified/separated for their location of production in Shacheng, Changli and Yantai, and the types of the blended, medium dry, dry white and dry red wines, using the NMR-PCA method. The wines were produced by three subsidiary companies of an enterprise according to the same national standard. The separation was believed to be mainly due to the fermentation process for different wines and environmental variations, such as local climate, soil, underground water, sunlight and rainfall. The major chemicals associated with the separation were identified.

  1. Human Equilibrative Nucleoside Transporter 1 (hENT1 in Pancreatic Adenocarcinoma: Towards Individualized Treatment Decisions

    Directory of Open Access Journals (Sweden)

    Jennifer L. Spratlin

    2010-12-01

    Full Text Available Pancreatic cancer is one of the most lethal cancers, where curative surgical resections are rare and less than 5% of patients experience long-term survival. Despite numerous clinical trials, improvements in the systemic treatment of this disease have been limited. Gemcitabine, a nucleoside analogue, is still considered the standard of care chemotherapy for most patients in the advanced disease setting. To exert its cytotoxic effects, gemcitabine must enter cells via nucleoside transporters, most notably human equilibrative nucleoside transporter 1 (hENT1. Increasingly strong evidence suggests hENT1 is a prognostic biomarker in gemcitabine-treated pancreatic cancer, and may well be a predictive biomarker of gemcitabine efficacy. In this review, we synthesize the literature surrounding hENT1 in pancreatic cancer, identify the key outstanding questions, and suggest strategies to prospectively evaluate the clinical utility of hENT1 in future clinical studies.

  2. Quantitative analysis of sesquiterpene lactones in extract of Arnica montana L. by 1H NMR spectroscopy.

    Science.gov (United States)

    Staneva, Jordanka; Denkova, Pavletta; Todorova, Milka; Evstatieva, Ljuba

    2011-01-01

    (1)H NMR spectroscopy was used as a method for quantitative analysis of sesquiterpene lactones present in a crude lactone fraction isolated from Arnica montana. Eight main components - tigloyl-, methacryloyl-, isobutyryl- and 2-methylbutyryl-esters of helenalin (H) and 11α,13-dihydrohelenalin (DH) were identified in the studied sample. The method allows the determination of the total amount of sesquiterpene lactones and the quantity of both type helenalin and 11α,13-dihydrohelenalin esters separately. Furthermore, 6-O-tigloylhelenalin (HT, 1), 6-O-methacryloylhelenalin (HM, 2), 6-O-tigloyl-11α,13-dihydrohelenalin (DHT, 5), and 6-O-methacryloyl-11α,13-dihydrohelenalin (DHM, 6) were quantified as individual components.

  3. Structural analysis of complex saponins of Balanites aegyptiaca by 800 MHz 1H NMR spectroscopy.

    Science.gov (United States)

    Staerk, Dan; Chapagain, Bishnu P; Lindin, Therese; Wiesman, Zeev; Jaroszewski, Jerzy W

    2006-10-01

    The main saponin (1) present in the mesocarp of Balanites aegyptiaca fruit is a mixture of 22R and 22S epimers of 26-(O-beta-D-glucopyranosyl)-3-beta-[4-O-(beta-D-glucopyranosyl)-2-O-(alpha-L-rhamnopyranosyl)-beta-D-glucopyranosyloxy]-22,26-dihydroxyfurost-5-ene. This structure differs from a previously reported saponin isolated from this source by the site of attachment of the rhamnosyl residue, and presumably represents a structural revision of the latter. The main saponin (2) present in the kernel is a xylopyranosyl derivative of 1. The use of high-field NMR enabled the practically complete assignment of 1H and 13C chemical shifts of these complex saponins, existing as a mixture of C-22 epimers. Moreover, the work represents a new approach to structural elucidation of saponins: direct preparative-scale HPLC-RID of crude extracts followed by high-field NMR investigations supported by ESI-MSn.

  4. 1H and 15N Dynamic Nuclear Polarization Studies of Carbazole

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Jian Zhi; Solum, Mark S.; Wind, Robert A.; Nilsson, Brad L.; Peterson, Matt A.; Pugmire, Ronald J.; Grant, David M.

    2000-01-01

    15N NMR experiments, combined with dynamic nuclear polarization (DNP), are reported on carbazole doped with the stable free radical 1,3 bisdiphenylene-2 phenylally1 (BDPA). Doping shortens the nuclear relaxation times and provides paramagnetic centers that can be used to enhance the nuclear signal by means of DNP so that 15 N NMR experiments can be done in minutes. The factors were measured in a 1.4 T external field, using both unlabeled and 98% 15N labeled carbazole with doping levels varying between 0.65 and 5.0 wt % BDPA. A doping level of approximately 1 wt % produced optimal results. DNP enhancement factors of 35 and 930 were obtained for 1H and 15N, respectively making it possible to perform 15N DNP NMR experiments at the natural abundance level.

  5. Novel ethyl-5-amino-3-methylthio-1H-pyrazole-4-carboxylates: Synthesis and pharmacological activity

    Directory of Open Access Journals (Sweden)

    S.N. Thore

    2016-05-01

    Full Text Available A series of novel ethyl-5-amino-3-methylthio-1H-pyrazole-4-carboxylates 3a–j were synthesized from condensation of various hydrazides 2a–j with ketene dithioacetal. The synthesized compounds were screened for in vivo analgesic and anti-inflammatory activities using acetic acid writhing test in mice and carrageenan-induced paw edema test in rat, respectively. Diclofenac sodium was used as a standard drug for comparison. Compounds 3a, 3c and 3d exhibited significant analgesic and anti-inflammatory activities at a dose of 25 mg/kg and showed quite less ulcerogenic index in the range of 0.9–1.12 whereas diclofenac sodium showed 3.10.

  6. Aquachloridobis[5-(2-pyridyl-1H-tetrazolato-κN1]iron(III

    Directory of Open Access Journals (Sweden)

    Bo Wang

    2009-08-01

    Full Text Available The title compound, [Fe(C6H4N52Cl(H2O], was synthesized by hydrothermal reaction of FeCl3 with 2-(1H-tetrazol-5-ylpyridine. The iron(III metal centre exhibits a distorted octahedral coordination geometry provided by four N atoms from two bidentate organic ligands, one water O atom and one chloride anion. The pyridine and tetrazole rings are nearly coplanar [dihedral angles = 4.32 (15 and 5.04 (14°]. In the crystal structure, intermolecular O—H...N hydrogen bonds link the complex molecules into a two-dimensional network parallel to (100.

  7. Experimental and theoretical investigation of optical nonlinearities in (nitrovinyl)-1H-pyrazole derivative

    Science.gov (United States)

    Dwivedi, Y.; de Boni, L.; Gonçalves, P. J.; Mairink, L. M.; Menegatti, R.; Fonseca, T. L.; Zilio, S. C.

    2013-03-01

    This work reports on the optical nonlinearities of a newly synthesized pyrazole derivative, namely (E)-1-(4-chlorophenyl)-4-(2-nitrovinyl)-1H-pyrazole. The Z-scan technique with femtosecond laser pulses was used to determine the two-photon absorption (2PA) cross-section spectrum, which presents a maximum of 67 GM at 690 nm. We have combined hyper-Rayleigh scattering (HRS) experiments and second-order Møller-Plesset perturbation theory (MP2) calculations to study the first hyperpolarizability (βHRS). It was found that the MP2/6-311+G(d) model, taking into account solvent and dispersion effects, provides the βHRS value of 40 × 10-30 cm5/esu for the compound, in good agreement with the experimental result of 45 ± 2 × 10-30 cm5/esu.

  8. 5-Fluoro-3-phenyl-N′-(4-propylcyclohexylidene-1H-indole-2-carbohydrazide

    Directory of Open Access Journals (Sweden)

    Orhan Büyükgüngör

    2013-08-01

    Full Text Available In the title compound, C24H26FN3O, the cyclohexane ring adopts a chair conformation; the propyl substituent is in an equatorial orientation and the bond-angle sum at the C atom bonded to the carbohydrazide N atom is 360.0°. The dihedral angle between the 1H-indole ring system and the phenyl ring is 82.77 (13°. A weak intramolecular C—H...π contact occurs. In the crystal, pairs of molecules related by a crystallographic twofold axis are linked by bifurcated N—H...(O,N hydrogen bonds; a C—H...O interaction occurs between the same pair. The dimers are linked by C—H...F and C—H...π interactions, generating a three-dimensional network.

  9. {sup 1}H magnetic resonance spectroscopy in the diagnosis of paediatric low grade brain tumours

    Energy Technology Data Exchange (ETDEWEB)

    Orphanidou-Vlachou, E., E-mail: eleni.orphanidou@googlemail.com [School of Cancer Sciences, College of Medical and Dental Sciences, University of Birmingham, Edgbaston, Birmingham, B15 2TT (United Kingdom); Birmingham Children' s Hospital NHS Foundation Trust, Whittall Street, Birmingham, B4 6NH (United Kingdom); Auer, D., E-mail: dorothee.auer@nottingham.ac.uk [Division of Academic Radiology, School of Medical and Surgical Sciences, The University of Nottingham, University Park, Nottingham, NG7 2RD (United Kingdom); Children' s Brain Tumour Research Centre, Queens Medical Centre, University of Nottingham (United Kingdom); Brundler, M.A., E-mail: marie-anne.brundler@bch.nhs.uk [Birmingham Children' s Hospital NHS Foundation Trust, Whittall Street, Birmingham, B4 6NH (United Kingdom); Davies, N.P., E-mail: nigel.davies@nhs.net [School of Cancer Sciences, College of Medical and Dental Sciences, University of Birmingham, Edgbaston, Birmingham, B15 2TT (United Kingdom); Birmingham Children' s Hospital NHS Foundation Trust, Whittall Street, Birmingham, B4 6NH (United Kingdom); Department of Medical Physics, University Hospitals Birmingham NHS Foundation Trust, Mindelsohn Way, Edgbaston, Birmingham, B15 2WB (United Kingdom); Jaspan, T., E-mail: tim.jaspan@nuh.nhs.uk [Children' s Brain Tumour Research Centre, Queens Medical Centre, University of Nottingham (United Kingdom); MacPherson, L., E-mail: Lesley.MacPherson@bch.nhs.uk [Birmingham Children' s Hospital NHS Foundation Trust, Whittall Street, Birmingham, B4 6NH (United Kingdom); Natarajan, K., E-mail: Kal.Natarajan@uhb.nhs.uk [Birmingham Children' s Hospital NHS Foundation Trust, Whittall Street, Birmingham, B4 6NH (United Kingdom); Department of Medical Physics, University Hospitals Birmingham NHS Foundation Trust, Mindelsohn Way, Edgbaston, Birmingham, B15 2WB (United Kingdom); and others

    2013-06-15

    Introduction: Low grade gliomas are the commonest brain tumours in children but present in a myriad of ways, each with its own treatment challenges. Conventional MRI scans play an important role in their management but have limited ability to identify likely clinical behaviour. The aim of this study is to investigate {sup 1}H magnetic resonance spectroscopy (MRS) as a method for detecting differences between the various low grade gliomas and related tumours in children. Patients and methods: Short echo time single voxel {sup 1}H MRS at 1.5 or 3.0 T was performed prior to treatment on children with low grade brain tumours at two centres and five MR scanners, 69 cases had data which passed quality control. MRS data was processed using LCModel to give mean spectra and metabolite concentrations which were compared using T-tests, ANOVA, Receiver Operator Characteristic curves and logistic regression in SPSS. Results: Significant differences were found in concentrations of key metabolites between glioneuronal and glial tumours (T-test p < 0.05) and between most of the individual histological subtypes of low grade gliomas. The discriminatory metabolites identified, such as choline and myoinositol, are known tumour biomarkers. In the set of pilocytic astrocytomas and unbiopsied optic pathway gliomas, significant differences (p < 0.05, ANOVA) were found in metabolite profiles of tumours depending on location and patient neurofibromatosis type 1 status. Logistic regression analyses yielded equations which could be used to assess the probability of a tumour being of a specific type. Conclusions: MRS can detect subtle differences between low grade brain tumours in children and should form part of the clinical assessment of these tumours.

  10. 1H-NMR metabolomic biomarkers of poor outcome after hemorrhagic shock are absent in hibernators.

    Directory of Open Access Journals (Sweden)

    Lori K Bogren

    Full Text Available Hemorrhagic shock (HS following trauma is a leading cause of death among persons under the age of 40. During HS the body undergoes systemic warm ischemia followed by reperfusion during medical intervention. Ischemia/reperfusion (I/R results in a disruption of cellular metabolic processes that ultimately lead to tissue and organ dysfunction or failure. Resistance to I/R injury is a characteristic of hibernating mammals. The present study sought to identify circulating metabolites in the rat as biomarkers for metabolic alterations associated with poor outcome after HS. Arctic ground squirrels (AGS, a hibernating species that resists I/R injury independent of decreased body temperature (warm I/R, was used as a negative control.Male Sprague-Dawley rats and AGS were subject to HS by withdrawing blood to a mean arterial pressure (MAP of 35 mmHg and maintaining the low MAP for 20 min before reperfusing with Ringers. The animals' temperature was maintained at 37 ± 0.5 °C for the duration of the experiment. Plasma samples were taken immediately before hemorrhage and three hours after reperfusion. Hydrophilic and lipid metabolites from plasma were then analyzed via 1H-NMR from unprocessed plasma and lipid extracts, respectively. Rats, susceptible to I/R injury, had a qualitative shift in their hydrophilic metabolic fingerprint including differential activation of glucose and anaerobic metabolism and had alterations in several metabolites during I/R indicative of metabolic adjustments and organ damage. In contrast, I/R injury resistant AGS, regardless of season or body temperature, maintained a stable metabolic homeostasis revealed by a qualitative 1H-NMR metabolic profile with few changes in quantified metabolites during HS-induced global I/R.An increase in circulating metabolites indicative of anaerobic metabolism and activation of glycolytic pathways is associated with poor prognosis after HS in rats. These same biomarkers are absent in AGS after HS

  11. Thermal degradation in a trimodal PDMS network by 1H Multiple Quantum NMR

    Energy Technology Data Exchange (ETDEWEB)

    Giuliani, J R; Gjersing, E L; Chinn, S C; Jones, T V; Wilson, T S; Alviso, C T; Herberg, J L; Pearson, M A; Maxwell, R S

    2007-06-06

    Thermal degradation of a filled, crosslinked siloxane material synthesized from PDMS chains of three different average molecular weights and with two different crosslinking species has been studied by {sup 1}H Multiple Quantum (MQ) NMR methods. Multiple domains of polymer chains were detected by MQ NMR exhibiting Residual Dipolar Coupling (<{Omega}{sub d}>) values of 200 Hz and 600 Hz, corresponding to chains with high average molecular weight between crosslinks and chains with low average molecular weight between crosslinks or near the multifunctional crosslinking sites. Characterization of the <{Omega}{sub d}> values and changes in <{Omega}{sub d}> distributions present in the material were studied as a function of time at 250 C and indicates significant time dependent degradation. For the domains with low <{Omega}{sub d}>, a broadening in the distribution was observed with aging time. For the domain with high <{Omega}{sub d}>, increases in both the mean <{Omega}{sub d}> and the width in <{Omega}{sub d}> were observed with increasing aging time. Isothermal Thermal Gravimetric Analysis (TGA) reveals a 3% decrease in weight over 20 hours of aging at 250 C. Degraded samples also were analyzed by traditional solid state {sup 1}H NMR techniques and offgassing products were identified by Solid Phase MicroExtraction followed by Gas Chromatography-Mass Spectrometry (SPME GC-MS). The results, which will be discussed here, suggest that thermal degradation proceeds by complex competition between oxidative chain scissioning and post-curing crosslinking that both contribute to embrittlement.

  12. A {sup 1}H nuclear magnetic resonance study of structural and organisational changes in the cell

    Energy Technology Data Exchange (ETDEWEB)

    Tunnah, Susan K

    2000-07-01

    Increasing importance is being placed on understanding the role of membrane lipids in many different areas of biochemistry. It is of interest to determine what interactions may occur between membrane lipids and drug species. Furthermore, an increasing body of evidence suggests that membrane lipids are involved in the pathology of numerous diseases such as rheumatoid arthritis, cancer and HIV. Clearly, the more information available on the mechanisms involved in diseases, the greater the potential for identifying a cure or even a prevention. {sup 1}H nuclear magnetic resonance (NMR) spectroscopy was used to study the alterations in membrane lipid organisation and structure in intact, viable cultured cells. Changes in the {sup 1}H NMR spectra and the spin-lattice relaxation measurements of the human K562 and the rat FRTL-5 cell lines were observed on the addition of the fatty acid species: triolein, evening primrose oil, arachidonic acid and ITF 1779. Results indicate that the membrane lipids are reorganised to accommodate the interpolation of these molecules. The spatial arrangement adopted by each of these species appeared to dictate its effect on the lipids. Doxorubicin and menadione, both known to cause oxidative stress, were added to K562 cells. Although both agents are known to act by different mechanisms, the NMR data and scanning electron microscopy suggested that both caused similar alterations in the membrane organisation and lipid fluidity. Protrusions were formed indicating areas of weakness in the membrane. Spin-echo NMR was employed to investigate the action of the thiol-containing compounds, penicillamine, captopril and N-acetylcysteine in erythrocytes under conditions of oxidative stress. Results indicate that while captopril acts as a free radical scavenger, penicillamine may act as either oxidant or reductant. N-acetylcysteine was observed to act as a reducing agent. (author)

  13. Multivariate modelling with 1H NMR of pleural effusion in murine cerebral malaria

    Directory of Open Access Journals (Sweden)

    Ghosh Soumita

    2011-11-01

    Full Text Available Abstract Background Cerebral malaria is a clinical manifestation of Plasmodium falciparum infection. Although brain damage is the predominant pathophysiological complication of cerebral malaria (CM, respiratory distress, acute lung injury, hydrothorax/pleural effusion are also observed in several cases. Immunological parameters have been assessed in pleural fluid in murine models; however there are no reports of characterization of metabolites present in pleural effusion. Methods 1H NMR of the sera and the pleural effusion of cerebral malaria infected mice were analyzed using principal component analysis, orthogonal partial least square analysis, multiway principal component analysis, and multivariate curve resolution. Results It has been observed that there was 100% occurrence of pleural effusion (PE in the mice affected with CM, as opposed to those are non-cerebral and succumbing to hyperparasitaemia (NCM/HP. An analysis of 1H NMR and SDS-PAGE profile of PE and serum samples of each of the CM mice exhibited a similar profile in terms of constituents. Multivariate analysis on these two classes of biofluids was performed and significant differences were detected in concentrations of metabolites. Glucose, creatine and glutamine contents were high in the PE and lipids being high in the sera. Multivariate curve resolution between sera and pleural effusion showed that changes in PE co-varied with that of serum in CM mice. The increase of glucose in PE is negatively correlated to the glucose in serum in CM as obtained from the result of multiway principal component analysis. Conclusions This study reports for the first time, the characterization of metabolites in pleural effusion formed during murine cerebral malaria. The study indicates that the origin of PE metabolites in murine CM may be the serum. The loss of the components like glucose, glutamine and creatine into the PE may worsen the situation of patients, in conjunction with the enhanced

  14. Predicting Fuel Ignition Quality Using 1H NMR Spectroscopy and Multiple Linear Regression

    KAUST Repository

    Abdul Jameel, Abdul Gani

    2016-09-14

    An improved model for the prediction of ignition quality of hydrocarbon fuels has been developed using 1H nuclear magnetic resonance (NMR) spectroscopy and multiple linear regression (MLR) modeling. Cetane number (CN) and derived cetane number (DCN) of 71 pure hydrocarbons and 54 hydrocarbon blends were utilized as a data set to study the relationship between ignition quality and molecular structure. CN and DCN are functional equivalents and collectively referred to as D/CN, herein. The effect of molecular weight and weight percent of structural parameters such as paraffinic CH3 groups, paraffinic CH2 groups, paraffinic CH groups, olefinic CH–CH2 groups, naphthenic CH–CH2 groups, and aromatic C–CH groups on D/CN was studied. A particular emphasis on the effect of branching (i.e., methyl substitution) on the D/CN was studied, and a new parameter denoted as the branching index (BI) was introduced to quantify this effect. A new formula was developed to calculate the BI of hydrocarbon fuels using 1H NMR spectroscopy. Multiple linear regression (MLR) modeling was used to develop an empirical relationship between D/CN and the eight structural parameters. This was then used to predict the DCN of many hydrocarbon fuels. The developed model has a high correlation coefficient (R2 = 0.97) and was validated with experimentally measured DCN of twenty-two real fuel mixtures (e.g., gasolines and diesels) and fifty-nine blends of known composition, and the predicted values matched well with the experimental data.

  15. BEBEtr and BUBI: J-compensated concurrent shaped pulses for 1H-13C experiments

    Science.gov (United States)

    Ehni, Sebastian; Luy, Burkhard

    2013-07-01

    Shaped pulses designed for broadband excitation, inversion and refocusing are important tools in modern NMR spectroscopy to achieve robust pulse sequences especially in heteronuclear correlation experiments. A large variety of mostly computer-optimized pulse shapes exist for different desired bandwidths, available rf-field strengths, and tolerance to B1-inhomogeneity. They are usually derived for a single spin 1/2, neglecting evolution due to J-couplings. While pulses with constant resulting phase are selfcompensated for heteronuclear coupling evolution as long as they are applied exclusively on a single nucleus, the situation changes for concurrently applied pulse shapes. Using the example of a 1H,13C two spin system, two J-compensated pulse pairs for the application in INEPT-type transfer elements were optimized: a point-to-point pulse sandwich called BEBEtr, consisting of a broadband excitation and time-reversed excitation pulse, and a combined universal rotation and point-to-point pulse pair called BUBI, which acts as a refocusing pulse on 1H and a corresponding inversion pulse on 13C. After a derivation of quality factors and optimization protocols, a theoretical and experimental comparison with conventionally derived BEBOP, BIBOP, and BURBOP-180° pulses is given. While the overall transfer efficiency of a single pulse pair is only reduced by approximately 0.1%, resulting transfer to undesired coherences is reduced by several percent. In experiments this can lead to undesired phase distortions for pairs of uncompensated pulse shapes and even differences in signal intensities of 5-10% in HSQC and up to 68% in more complex COB-HSQC experiments.

  16. The peculiar radio-loud narrow line Seyfert 1 galaxy 1H 0323+342

    Energy Technology Data Exchange (ETDEWEB)

    Paliya, Vaidehi S.; Stalin, C. S. [Indian Institute of Astrophysics, Block-II, Koramangala, Bangalore-560034 (India); Sahayanathan, S. [Astrophysical Science Division, Bhabha Atomic Research Center, Mumbai-400085 (India); Parker, M. L.; Fabian, A. C. [Institute of Astronomy, Madingley Road, Cambridge CB3 0HA (United Kingdom); Anjum, Ayesha [Department of Physics, Christ University, Bangalore-560029 (India); Pandey, S. B., E-mail: vaidehi@iiap.res.in [Aryabhatta Research Institute of Observational Sciences, Manora peak, Nainital-263129 (India)

    2014-07-10

    We present a multiwavelength study of the radio-loud narrow-line Seyfert 1 galaxy (NLSy1) 1H 0323+342, detected by the Fermi Gamma-Ray Space Telescope. Multiband light curves show many orphan X-ray and optical flares having no corresponding γ-ray counterparts. Such anomalous variability behavior can be due to different locations of the emission region from the central source. During a large flare, a γ-ray flux doubling timescale as small as ∼3 hr is noticed. We built spectral energy distributions (SEDs) during different activity states and modeled them using a one-zone leptonic model. The shape of the optical/UV component of the SEDs is dominated by accretion disk emission in all the activity states. In the X-ray band, significant thermal emission from the hot corona is inferred during quiescent and first flaring states; however, during subsequent flares, the nonthermal jet component dominates. The γ-ray emission in all the states can be well explained by inverse-Compton scattering of accretion disk photons reprocessed by the broad-line region. The source showed violent intra-night optical variability, coinciding with one of the high γ-ray activity states. An analysis of the overall X-ray spectrum fitted with an absorbed power-law plus relativistic reflection component hints at the presence of an Fe Kα line and returns a high black hole spin value of a = 0.96 ± 0.14. We argue that 1H 0323+342 possesses dual characteristics, akin to both flat-spectrum radio quasars (FSRQs) and radio-quiet NLSy1 galaxies, though at a low jet power regime compared to powerful FSRQs.

  17. The alveolin IMC1h is required for normal ookinete and sporozoite motility behaviour and host colonisation in Plasmodium berghei.

    Directory of Open Access Journals (Sweden)

    Katrin Volkmann

    Full Text Available Alveolins, or inner membrane complex (IMC proteins, are components of the subpellicular network that forms a structural part of the pellicle of malaria parasites. In Plasmodium berghei, deletions of three alveolins, IMC1a, b, and h, each resulted in reduced mechanical strength and gliding velocity of ookinetes or sporozoites. Using time lapse imaging, we show here that deletion of IMC1h (PBANKA_143660 also has an impact on the directionality and motility behaviour of both ookinetes and sporozoites. Despite their marked motility defects, sporozoites lacking IMC1h were able to invade mosquito salivary glands, allowing us to investigate the role of IMC1h in colonisation of the mammalian host. We show that IMC1h is essential for sporozoites to progress through the dermis in vivo but does not play a significant role in hepatoma cell transmigration and invasion in vitro. Colocalisation of IMC1h with the residual IMC in liver stages was detected up to 30 hours after infection and parasites lacking IMC1h showed developmental defects in vitro and a delayed onset of blood stage infection in vivo. Together, these results suggest that IMC1h is involved in maintaining the cellular architecture which supports normal motility behaviour, access of the sporozoites to the blood stream, and further colonisation of the mammalian host.

  18. The alveolin IMC1h is required for normal ookinete and sporozoite motility behaviour and host colonisation in Plasmodium berghei.

    Science.gov (United States)

    Volkmann, Katrin; Pfander, Claudia; Burstroem, Charlotte; Ahras, Malika; Goulding, David; Rayner, Julian C; Frischknecht, Friedrich; Billker, Oliver; Brochet, Mathieu

    2012-01-01

    Alveolins, or inner membrane complex (IMC) proteins, are components of the subpellicular network that forms a structural part of the pellicle of malaria parasites. In Plasmodium berghei, deletions of three alveolins, IMC1a, b, and h, each resulted in reduced mechanical strength and gliding velocity of ookinetes or sporozoites. Using time lapse imaging, we show here that deletion of IMC1h (PBANKA_143660) also has an impact on the directionality and motility behaviour of both ookinetes and sporozoites. Despite their marked motility defects, sporozoites lacking IMC1h were able to invade mosquito salivary glands, allowing us to investigate the role of IMC1h in colonisation of the mammalian host. We show that IMC1h is essential for sporozoites to progress through the dermis in vivo but does not play a significant role in hepatoma cell transmigration and invasion in vitro. Colocalisation of IMC1h with the residual IMC in liver stages was detected up to 30 hours after infection and parasites lacking IMC1h showed developmental defects in vitro and a delayed onset of blood stage infection in vivo. Together, these results suggest that IMC1h is involved in maintaining the cellular architecture which supports normal motility behaviour, access of the sporozoites to the blood stream, and further colonisation of the mammalian host.

  19. Synthesis of 4-hydroxy-2(1H)-quinolone derived chalcones, pyrazolines and their antimicrobial, in silico antimalarial evaluations.

    Science.gov (United States)

    Sarveswari, S; Vijayakumar, V; Siva, R; Priya, R

    2015-01-01

    A few derivatives of 3-(4,5-dihydro-5-aryl-1-phenyl-1H-pyrazol-3-yl)-4-hydroxyquinolin-2(1H)-ones (5a-j) that are synthesized from 4-hydroxy-3-(3-arylacryloyl)quinolin-2(1H)-ones (4a-j) by microwave-assisted synthesis are screened for their antimicrobial, in silico antimalarial activities. Among the tested compounds 4h and 5d were found to have a potent antimalarial activity than the standards, and the others are found to show considerable antimalarial activity and moderate antimicrobial activity.

  20. Styrylpyrylium Salts: 1H and 13C NMR High-Resolution Spectroscopy (1D and 2D

    Directory of Open Access Journals (Sweden)

    Jean Claude W. Ouédraogo

    2010-01-01

    Full Text Available 1H and 13C NMR high-resolution spectroscopy (1D and 2D (1H, 1H-COSY, HSQC, HMBC for four styrylpyrylium perchlorates were carried out and signal attributions are reported. Chemical shifts observed on 13C NMR spectra for the styrylpyrylium salts were compared with net atomic charge for carbon obtained by AM1 semiempirical calculations. The position of the styryl group present low effect on chemical shifts for carbon atoms, while the presence of methyl group led to the unshielding of the substituted carbon.

  1. 1H, 1H, 2H, 2H-Perfluoroalkyl-Functionalization of Ni(II), Pd(II) and Pt(II) Mono- and Diphosphine Complexes : minimizing the Electronic Consequences for the Metal Center

    NARCIS (Netherlands)

    Koten, G. van; Wolf, E. de; Mens, A.J.M.; Gijzeman, O.L.J.; Lenthe, J.H. van; Jenneskens, L.W.; Deelman, B.J.

    2003-01-01

    A series of fluorous derivatives of group 10 complexes MCl2(dppe) and [M(dppe)2](BF4)2 (M = Ni, Pd or Pt; dppe = 1,2-bis(diphenylphosphino)ethane) and cis-PtCl2(PPh3)2 was synthesized. The influence of para-(1H,1H,2H,2H-perfluoroalkyl)dimethylsilyl-functionalization of the phosphine phenyl groups of

  2. DFT calculations of 1H and 13C NMR chemical shifts in transition metal hydrides.

    Science.gov (United States)

    del Rosal, I; Maron, L; Poteau, R; Jolibois, F

    2008-08-14

    Transition metal hydrides are of great interest in chemistry because of their reactivity and their potential use as catalysts for hydrogenation. Among other available techniques, structural properties in transition metal (TM) complexes are often probed by NMR spectroscopy. In this paper we will show that it is possible to establish a viable methodological strategy in the context of density functional theory, that allows the determination of 1H NMR chemical shifts of hydride ligands attached to transition metal atoms in mononuclear systems and clusters with good accuracy with respect to experiment. 13C chemical shifts have also been considered in some cases. We have studied mononuclear ruthenium complexes such as Ru(L)(H)(dppm)2 with L = H or Cl, cationic complex [Ru(H)(H2O)(dppm)2]+ and Ru(H)2(dppm)(PPh3)2, in which hydride ligands are characterized by a negative 1H NMR chemical shift. For these complexes all calculations are in relatively good agreement compared to experimental data with errors not exceeding 20% except for the hydrogen atom in Ru(H)2(dppm)(PPh3)2. For this last complex, the relative error increases to 30%, probably owing to the necessity to take into account dynamical effects of phenyl groups. Carbonyl ligands are often encountered in coordination chemistry. Specific issues arise when calculating 1H or 13C NMR chemical shifts in TM carbonyl complexes. Indeed, while errors of 10 to 20% with respect to experiment are often considered good in the framework of density functional theory, this difference in the case of mononuclear carbonyl complexes culminates to 80%: results obtained with all-electron calculations are overall in very satisfactory agreement with experiment, the error in this case does not exceed 11% contrary to effective core potentials (ECPs) calculations which yield errors always larger than 20%. We conclude that for carbonyl groups the use of ECPs is not recommended, although their use could save time for very large systems, for

  3. 1H to 13C Energy Transfer in Solid State NMR Spectroscopy of Natural Organic Systems

    Science.gov (United States)

    Berns, Anne E.; Conte, Pellegrino

    2010-05-01

    Cross polarization (CP) magic angle spinning (MAS) 13C-NMR spectroscopy is a solid state NMR technique widely used to study chemical composition of organic materials with low or no solubility in the common deuterated solvents used to run liquid state NMR experiments. Based on the magnetization transfer from abundant nuclei (with spin of 1 -2) having a high gyromagnetic ratio (γ), such as protons, to the less abundant 13C nuclei with low γ values, 13C-CPMAS NMR spectroscopy is often applied in environmental chemistry to obtain quantitative information on the chemical composition of natural organic matter (NOM) (Conte et al., 2004), although its quantitative assessment is still matter of heavy debates. Many authors (Baldock et al., 1997; Conte et al., 1997, 2002; Dria et al., 2002; Kiem et al., 2000; Kögel-Knabner, 2000; Preston, 2001), reported that the application of appropriate instrument setup as well as the use of special pulse sequences and correct spectra elaboration may provide signal intensities that are directly proportional to the amount of nuclei creating a NMR signal. However, many other papers dealt with the quantitative unsuitability of 13C-CPMAS NMR spectroscopy. Among those, Mao et al. (2000), Smernik and Oades (2000 a,b), and Preston (2001) reported that cross-polarized NMR techniques may fail in a complete excitation of the 13C nuclei. In fact, the amount of observable carbons via 13C-CPMAS NMR spectroscopy appeared, in many cases, lower than that measured by a direct observation of the 13C nuclei. As a consequence, cross-polarized NMR techniques may provide spectra where signal distribution may not be representative of the quantitative distribution of the different natural organic matter components. Cross-polarization is obtained after application of an initial 90° x pulse on protons and a further spin lock pulse (along the y axis) having a fixed length (contact time) for both nuclei (1H and 13C) once the Hartmann-Hahn condition is matched

  4. Synthesis of 3-(1-Methyl-1H-imidazol-2-ylthio)propanoic Acid and (E)-3-(1-Methyl-1H-imidazol-2-ylthio)acrylic Acid.

    Science.gov (United States)

    Hattan, Christopher M; Shojaie, Jalil; Lau, Serrine S; Anders, M W

    2013-01-01

    The syntheses of 3-(1-methyl-1H-imidazol-2-ylthio)acrylic acid and 3-(1-methyl-1H-imidazol-2-ylthio)propanoic acid, mitochondria-targeted prodrugs of the antioxidant methimazole, are described. The method of Fan et al. (Fan et al., Synthesis2006, 2286) for the reaction of phenols with propiolic acid and propiolate esters was modified to synthesize (E)-3-(1-methyl-1H-imidazol-2-ylthio)acrylic acid. The intermediate tert-butyl (E)-3-(1-methyl-1H-imidazol-2-ylthio)acrylate was prepared by the reaction of tert-butyl propiolate with methimazole; the use of tert-butyl propiolate rather than methyl propiolate gave tert-butyl (E)-3-(1-methyl-1H-imidazol-2-ylthio)acrylate as the predominant isomer. Acid hydrolysis of the intermediate ester afforded the target compound. 3-(1-Methyl-1H-imidazol-2-ylthio)propanoic acid was synthesized from 3-bromopropanoic acid and methimazole under conditions that gave preferential substitution on sulfur and minimized substitution on nitrogen.

  5. Hydrochemistry and 18O/16O and 2H/1H Ratios of Ugandan Waters

    Science.gov (United States)

    Gebremichael, M. G.; Jasechko, S.

    2013-12-01

    Today, 70% of the 35 million people living in Uganda have access to an improved water source, ranking Uganda 148 out of 179 nations reporting in 2010 (Millennium Development Goals Indicators). 80% of Ugandans rely on groundwater as their primary drinking water source, collecting at springs or from shallow wells. Similarly, 80% of Ugandans rely upon agriculture - usually rain fed - as their primary income source. Despite lack of access to protected water sources faced by 10 million Ugandans, and the importance of the blue economy to Uganda's continued development, a country-wide investigation of the chemistry and the stable oxygen and hydrogen isotope compositions of waters has yet to be completed. Here we present 250 analyses of 18O/16O, 2H/1H and dissolved ion concentrations of Ugandan lakes, rivers, groundwaters and springs collected during July, 2013. We use the new data to characterize regional scale groundwater recharge sources, advection pathways and interactions with surface waters. Large lakes - Albert, Edward and Victoria - show increases in 18O/16O and 2H/1H ratios consistent with open water evaporation, and are shown to be distinct from nearby groundwaters, suggesting minimal recharge from large lakes to the subsurface. Salinities of eastern Ugandan groundwaters are elevated relative to samples collected from the central and western regions, suggesting that longer groundwater residence times and enhanced water-rock interactions characterize these waters. Springs from western Uganda show a shift in 18O/16O to higher values as a result of hydrothermal water-rock exchanges. Dissolved ion and noble gas concentrations show potential for use in assessing geothermal energy resources, perhaps aiding the Ugandan Ministry for Energy, Minerals and Development to meet their goal of increasing renewable energy from 4% (current) to 61% of total use by 2017 (Nyakabwa-Atwoki, 2013). Millennium Development Goals Indicators. mdgs.un.org/unsd/mdg/data.aspx Nyakabwa

  6. The evolving role of alemtuzumab (Campath-1H in renal transplantation

    Directory of Open Access Journals (Sweden)

    Phuong-Thu T Pham

    2008-12-01

    Full Text Available Phuong-Thu T Pham1, Gerald S Lipshutz2, Phuong-Truc T Pham3, Joseph Kawahji1, Jennifer S Singer4, Phuong-Chi T Pham51Division of Nephrology, Department of Medicine, Kidney and Pancreas Transplant Program, University of California at Los Angeles, David Geffen School of Medicine, Los Angeles, California; 2Kidney and Pancreas Transplant Program, Department of Surgery and Urology, University of California at Los Angeles, David Geffen School of Medicine, Los Angeles, California; 3Department of Science, Penn State University, Worthington-Scranton, Dunmore, Pennsylvania; 4Renal Transplantation and Pediatric Urology, Department of Urology, University of California at Los Angeles, David Geffen School of Medicine, Los Angeles, California; 5Division of Nephrology, Department of Medicine, University of California at Los Angeles, David Geffen School of Medicine, Los Angeles, and Olive-View-UCLA Medical Center, Sylmar, California, USAAbstract: The introduction of new immunosuppressive agents into clinical transplantation in the 1990s has resulted in excellent short-term graft survival. Nonetheless, extended long-term graft outcomes have not been achieved due in part to the nephrotoxic effects of calcineurin inhibitors (CNIs and the adverse effects of steroid on cardiovascular disease risk factors. Induction therapy with lymphocyte depleting antibodies has originally been introduced into renal transplantation to provide intense immunosuppression in the early post-transplant period to prevent allograft rejection. Over the past half decade, induction therapy with both non-lymphocyte depleting (basiliximab and daclizumab and lymphocyte-depleting antibodies (antithymocyte antibodies, OKT3, alemtuzumab has increasingly been utilized in steroid or CNI sparing protocols in the early postoperative period. Alemtuzumab is a humanized monoclonal antibody targeted against CD52 on the surface of circulatory mononuclear cells. The ability of alemtuzumab (Campath-1H to

  7. Primary somatosensory cortex in chronic low back pain – a 1H-MRS study

    Directory of Open Access Journals (Sweden)

    Sharma KN

    2011-05-01

    Full Text Available Neena K Sharma1, Kenneth McCarson2, Linda Van Dillen5, Angela Lentz1, Talal Khan3, Carmen M Cirstea1,41Department of Physical Therapy and Rehabilitation Science, 2Department of Pharmacology, Toxicology and Therapeutics, 3Department of Anesthesiology, 4Hoglund Brain Imaging Center, University of Kansas Medical Center, Kansas City, KS, USA; 5Program in Physical Therapy and Department of Orthopedic Surgery, Washington University School of Medicine, St Louis, MO, USAAbstract: The goal of this study was to investigate whether certain metabolites, specific to neurons, glial cells, and the neuronal-glial neurotransmission system, in the primary somatosensory cortex (SSC, are altered and correlated with clinical characteristics of pain in patients with chronic low back pain (LBP. Eleven LBP patients and eleven age-matched healthy controls were included. N-acetylaspartate (NAA, choline (Cho, myo-inositol (mI, and glutamine/glutamate (Glx were measured with proton magnetic resonance spectroscopy (1H-MRS in left and right SSC. Differences in metabolite concentrations relative to those of controls were evaluated as well as analyses of metabolite correlations within and between SSCs. Relationships between metabolite concentrations and pain characteristics were also evaluated. We found decreased NAA in the left SSC (P = 0.001 and decreased Cho (P = 0.04 along with lower correlations between all metabolites in right SSC (P = 0.007 in LBP compared to controls. In addition, we found higher and significant correlations between left and right mI (P < 0.001 in LBP vs P = 0.1 in controls and between left mI and right Cho (P = 0.048 vs P = 0.6. Left and right NAA levels were negatively correlated with pain duration (P = 0.04 and P = 0.02 respectively while right Glx was positively correlated with pain severity (P = 0.04. Our preliminary results demonstrated significant altered neuronal-glial interactions in SSC, with left neural alterations related to pain duration

  8. 1H MAS NMR characterization of hydrogen over silica-supported rhodium catalyst

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Hydrogen species in both SiO2 and Rh/SiO2 catalysts pretreated indifferent atmospheres (H2, O2, helium or air) at different temperatures (773 or 973 K) were investigated by means of 1H MAS NMR. In SiO2 and O2-pretreated catalysts, a series of downfield signals at ~7.0, 3.8-4.0, 2.0 and 1.5-1.0 were detected. The first two signals can be attributed to strongly adsorbed and physisorbed water and the others to terminal silanol (SiOH) and SiOH under the screening of oxygen vacancies in SiO2 lattice, respectively. Besides the above signals, both upfield signal at ~-110 and downfield signals at 3.0 and 0.0 were also detected in H2-pretreated catalyst, respectively. The upfield signal at ~-110 originated from the dissociative adsorption of H2 over rhodium and was found to consist of both the contributions of reversible and irreversible hydrogen. There also probably existed another dissociatively adsorbed hydrogen over rhodium, which was known to be b hydrogen and in a unique form of "delocalized hydrogen". It was presumed that the b hydrogen had an upfield shift of ca. -20- -50, though its 1H NMR signals, which, having been masked by the spinning sidebands of Si-OH, failed to be directly detected out. The downfield signal at 3.0 was assigned to spillover hydrogen weakly bound by the bridge oxygen of SiO2. Another downfield signal at 0.0 was assigned to hydrogen held in the oxygen vacancies of SiO2 (Si-H species), suffering from the screening of trapped electrons. Both the spillover hydrogen and the Si-H resulted from the migration of the reversible hydrogen and the b hydrogen from rhodium to SiO2 in the close vicinity. It was proved that the above migration of hydrogen was preferred to occur at higher temperature than at lower temperature.

  9. Atribuição dos deslocamentos químicos dos átomos de ¹H e 13C do acetato de acantoaustralida 1H and 13C NMR assignments of acanthoaustralide-1-O-Acetate

    Directory of Open Access Journals (Sweden)

    Lúcia R. Rocha Martins

    2006-12-01

    Full Text Available Do extrato hidroetanólico das partes aéreas de Acanthospermum australe (Asteraceae foram identificados uma lactona diterpênica, o acetato de acantoaustralida (1 e dois flavonoides: quercetina (2 e crisosplenol D (3. As estruturas foram identificadas através de técnicas espectroscópicas de RMN de ¹H e 13C, gHSQC, gHMBC, TOCSY, gNOESY, EM e pela comparação com dados da literatura.From the hydroethanolic extract of the aerial parts of Acanthospermum australe (Asteraceae a diterpene lactone, acanthoaustralide-1-O-Acetate (1 and two flavonoids: quercetin (2 and chrysosplenol D (3 were identified. The structures were determined though the use of spectroscopic techniques such as NMR (¹H, 13C{¹H}, gHSQC, gHMBC, TOCSY, gNOESY, MS and compared with the literature data.

  10. DABCO-promoted facile and convenient synthesis of novel isoxazolyl-1H-2,3-pyrrole dicarboxylates

    Institute of Scientific and Technical Information of China (English)

    Rajanarendar Eligeti; Kishore Baireddy; Ramakrishna Saini

    2013-01-01

    Synthesis of isoxazolyl-1H-2,3-pyrrole dicarboxylate (4) was simply achieved by one-pot three component reaction of isoxazole amine (1) with diethyl acetylenedicarboxylate (DEAD) (2),and glyoxal (3),in acetonitrile catalyzed by diazabicyclo octane (DABCO).

  11. /sup 14/C isotope effects in /sup 1/H and /sup 13/C N. M. R. spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Funke, C.W.; Kaspersen, F.M.; Sperling, E.M.G.; Wagenaars, G.N.

    1986-03-15

    Replacement of /sup 12/C by /sup 14/C induces small upfield shifts of the directly bonded /sup 1/H and /sup 13/C nuclei; these shift differences can be used to measure the extent of /sup 14/C labelling.

  12. Rapid determination of coenzyme Q10 in food supplements using 1H NMR spectroscopy.

    Science.gov (United States)

    Monakhova, Yulia B; Ruge, Ingrid; Kuballa, Thomas; Lerch, Christiane; Lachenmeier, Dirk W

    2013-01-01

    A methodology utilizing 1H NMR spectroscopy has been developed to measure the concentration of coenzyme Q10 (CoQ10) in dietary supplements. For sample preparation, a very simple dilution with deuterated chloroform and addition of internal standard is sufficient. CoQ10 produces a distinct peak of the CH groups in the isoprene side chain of the molecule in the δ 5.15 - 5.05 ppm range, where it can be distinguished from other matrix compounds. The method was shown to be of adequate sensitivity with a limit of detection (LOD) of 7.8 mg/L, to control the CoQ10 content in the majority of the products. The precision expressed as relative standard deviation was around 5 %; linearity was observed from 14 to 2000 mg/L (R = 0.99). The developed methodology was applied for the analysis of 21 food supplements (capsules, tablets, and liquid products). On the basis of the labeled amounts, only two products contained substantially lower concentrations of CoQ10 (57 % and 51 %). All other concentrations varied between 83 % and 190 % with respect to labeling. The developed NMR method may be used by quality assurance laboratories for routine control of CoQ10 products.

  13. 1H NMR Metabolic Profiling of Biofluids from Rats with Gastric Mucosal Lesion and Electroacupuncture Treatment

    Directory of Open Access Journals (Sweden)

    Jingjing Xu

    2015-01-01

    Full Text Available Gastric mucosal lesion (GML is a common gastrointestinal disorder with multiple pathogenic mechanisms in clinical practice. In traditional Chinese medicine (TCM, electroacupuncture (EA treatment has been proven as an effective therapy for GML, although the underlying healing mechanism is not yet clear. Here, we used proton nuclear magnetic resonance- (1H NMR- based metabolomic method to investigate the metabolic perturbation induced by GML and the therapeutic effect of EA treatment on stomach meridian (SM acupoints. Clear metabolic differences were observed between GML and control groups, and related metabolic pathways were discussed by means of online metabolic network analysis toolbox. By comparing the endogenous metabolites from GML and GML-SM groups, the disturbed pathways were partly recovered towards healthy state via EA treated on SM acupoints. Further comparison of the metabolic variations induced by EA stimulated on SM and the control gallbladder meridian (GM acupoints showed a quite similar metabolite composition except for increased phenylacetylglycine, 3,4-dihydroxymandelate, and meta-hydroxyphenylacetate and decreased N-methylnicotinamide in urine from rats with EA treated on SM acupoints. The current study showed the potential application of metabolomics in providing further insight into the molecular mechanism of acupuncture.

  14. 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.

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

    Science.gov (United States)

    Castejón, David; Fricke, Pascal; Cambero, María Isabel; Herrera, Antonio

    2016-01-01

    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. PMID:26891323

  16. Visual stimulation, {sup 1}H MR spectroscopy and fMRI of the human visual pathways

    Energy Technology Data Exchange (ETDEWEB)

    Boucard, Christine C.; Cornelissen, Frans W. [University of Groningen, Laboratory for Experimental Ophthalmology, Postbus 30001, Groningen (Netherlands); University of Groningen, BCN Neuro-imaging Center, Postbus 196, Groningen (Netherlands); Mostert, Jop P.; Keyser, Jacques De [University Hospital Groningen, Department of Neurology, Groningen (Netherlands); Oudkerk, Matthijs; Sijens, Paul E. [University Hospital Groningen, Department of Radiology, Groningen (Netherlands)

    2005-01-01

    The purpose was to assess changes in lactate content and other brain metabolites under visual stimulation in optical chiasm, optic radiations and occipital cortex using multiple voxel MR spectroscopy (MRS). {sup 1}H chemical shift imaging (CSI) examinations of transverse planes centered to include the above structures were performed in four subjects at an echo time of 135 ms. Functional MRI (fMRI) was used to confirm the presence of activity in the visual cortex during the visual stimulation. Spectral maps of optical chiasm were of poor quality due to field disturbances caused by nearby large blood vessels and/or eye movements. The optic radiations and the occipital lobe did not show any significant MR spectral change upon visual stimulation, i.e., the peak areas of inositol, choline, creatine, glutamate and N-acetylaspartate were not affected. Reproducible lactate signals were not observed. fMRI confirmed the presence of strong activations in stimulated visual cortex. Prolonged visual stimulation did not cause significant changes in MR spectra. Any signal observed near the 1.33 ppm resonance frequency of the lactate methyl-group was artifactual, originating from lipid signals from outside the volume of interest (VOI). Previous claims about changes in lactate levels in the visual cortex upon visual stimulation may have been based on such erroneous observations. (orig.)

  17. 1H0419-577 A "two-state" soft X-ray Seyfert galaxy

    CERN Document Server

    Guainazzi, M; Stripe, G M; Brandt, W N; Fiore, F; Leighly, K M; Matt, G; Molendi, S; Puchnarewicz, E M; Piro, L; Siemiginowska, A L

    1998-01-01

    In this paper we report on the first simultaneous optical and X-ray (Beppo-SAX) observations of the radio-quiet AGN 1H0419-577. The optical spectrum clearly leads us to classify this source as a Seyfert 1. The X-ray spectrum is, however, somewhat at odds with this classification: a simple flat (Gamma ~ 1.55) and featureless power--law is a good description of the whole 1.8-40 keV spectrum, even if the upper limit to a broad iron line is not very tight. An analysis of a still unpublished ROSAT observation of the same target reveals that the soft X-ray spectrum has undergone a transition from a steep (Gamma ~ 2.5) to a flat (Gamma ~ 1.55) state, at least in the 0.7-2 keV band. If this difference is due to a remarkably variable soft excess, it is unlikely that a single component is responsible for the optical/UV/soft X-ray spectral distribution. The hypothesis that the difference is due to a change in the primary X-ray continuum and its implications for current Comptonization models are discussed.

  18. (1)H NMR-based metabolomic approach for understanding the fermentation behaviors of wine yeast strains.

    Science.gov (United States)

    Son, Hong-Seok; Hwang, Geum-Sook; Kim, Ki Myong; Kim, Eun-Young; van den Berg, Frans; Park, Won-Mok; Lee, Cherl-Ho; Hong, Young-Shick

    2009-02-01

    (1)H NMR spectroscopy coupled with multivariate statistical analysis was used for the first time to investigate metabolic changes in musts during alcoholic fermentation and wines during aging. Three Saccharomyces cerevisiae yeast strains (RC-212, KIV-1116, and KUBY-501) were also evaluated for their impacts on the metabolic changes in must and wine. Pattern recognition (PR) methods, including PCA, PLS-DA, and OPLS-DA scores plots, showed clear differences for metabolites among musts or wines for each fermentation stage up to 6 months. Metabolites responsible for the differentiation were identified as valine, 2,3-butanediol (2,3-BD), pyruvate, succinate, proline, citrate, glycerol, malate, tartarate, glucose, N-methylnicotinic acid (NMNA), and polyphenol compounds. PCA scores plots showed continuous movements away from days 1 to 8 in all musts for all yeast strains, indicating continuous and active fermentation. During alcoholic fermentation, the highest levels of 2,3-BD, succinate, and glycerol were found in musts with the KIV-1116 strain, which showed the fastest fermentation or highest fermentative activity of the three strains, whereas the KUBY-501 strain showed the slowest fermentative activity. This study highlights the applicability of NMR-based metabolomics for monitoring wine fermentation and evaluating the fermentative characteristics of yeast strains.

  19. Pore size distribution calculation from 1H NMR signal and N2 adsorption-desorption techniques

    Science.gov (United States)

    Hassan, Jamal

    2012-09-01

    The pore size distribution (PSD) of nano-material MCM-41 is determined using two different approaches: N2 adsorption-desorption and 1H NMR signal of water confined in silica nano-pores of MCM-41. The first approach is based on the recently modified Kelvin equation [J.V. Rocha, D. Barrera, K. Sapag, Top. Catal. 54(2011) 121-134] which deals with the known underestimation in pore size distribution for the mesoporous materials such as MCM-41 by introducing a correction factor to the classical Kelvin equation. The second method employs the Gibbs-Thompson equation, using NMR, for melting point depression of liquid in confined geometries. The result shows that both approaches give similar pore size distribution to some extent, and also the NMR technique can be considered as an alternative direct method to obtain quantitative results especially for mesoporous materials. The pore diameter estimated for the nano-material used in this study was about 35 and 38 Å for the modified Kelvin and NMR methods respectively. A comparison between these methods and the classical Kelvin equation is also presented.

  20. 1H NMR spectra of humic and fulvic acids and their peracetic oxidation products

    Science.gov (United States)

    Ruggiero, P.; Interesse, F. S.; Cassidei, L.; Sciacovelli, O.

    1980-04-01

    1H NMR spectra of humic (HA) and fulvic (FA) acids and their oxidative degradation products are reported. The HA shows the presence of -( CH2) n - CH3 ( n > 6) chemical fragments belonging to n-alkanes and/or n-fatty acids physically adsorbed onto the macromolecule structure. These fragments are absent in the FA fraction. Both humic fractions reveal the presence of similar amounts of aromatic protons which partly undergo exchange phenomena. The importance of this experimental observation is discussed. Oxidative degradation seems to cause partial cleavage of aromatic rings, more pronounced in the FA than in the HA. The degraded FA shows a higher total acidity and a higher phenolic OH content than the degraded HA. Both degraded fractions display some sharp singlet signals at 1.9 and 3.9 ppm arising from protons belonging to repetitive chemical fragments probably formed during the oxidation reaction. Tentative assignments of these signals are given. A general analysis of the HA and FA degraded spectra seems to indicate that the chemical fragments which undergo peracetic oxidation are substantially similar. The extent of oxidation of the two humic fractions is different. The HA degradation products reveal the presence of oligomeric structures, whereas the degraded FA appears less resistant to the oxidizing agent.

  1. Polypharmacotherapy in rheumatology: 1H NMR analysis of binding of phenylbutazone and methotrexate to serum albumin

    Science.gov (United States)

    Maciążek-Jurczyk, M.; Sułkowska, A.; Równicka-Zubik, J.; Bojko, B.; Szkudlarek-Haśnik, A.; Knopik, M.; Sułkowski, W. W.

    2011-05-01

    The influence of phenylbutazone (Phe) and methotrexate (MTX) on binding of MTX and Phe to human (HSA) and bovine (BSA) serum albumin in the low-affinity binding sites is investigated. The strength and kind of interactions between serum albumin (SA) and drugs used in combination therapy were found using 1H NMR spectroscopy. A stoichiometric molar ratios for Phe-SA and MTX-SA complexes are 36:1 and 31:1, respectively. It appeared these molar ratios are higher for the ternary systems than it were in the binary ones. The presence of the additional drug (MTX or Phe) causes the increase of an affinity of albumin towards Phe and MTX. It was found that the aliphatic groups of MTX are more resistant to the influence of Phe on the MTX-SA complex than the aromatic rings. The results showed the important impact of another drug (MTX or Phe) on the affinity of SA towards Phe and MTX in the low-affinity binding sites. This work is a subsequent part of the spectroscopic study on Phe-MTX-SA interactions (Maciążek-Jurczyk, 2009 [1]).

  2. 1H HR-MAS NMR of carotenoids in aqueous samples and raw vegetables.

    Science.gov (United States)

    Miglietta, M L; Lamanna, R

    2006-07-01

    Carotenoids are linear C40 tetraterpenoid hydrocarbons and represent a wide category of natural pigments. They are components of the pigment system of chloroplasts and are involved in the primary light absorption and the photon canalization of photosynthesis. Moreover, they also behave as quenchers of singlet oxygen, protecting cells and organisms against lipid peroxidation. Carotenoids have a strong lipophilic character and are usually analyzed in organic solvents. However, because of their biological activity, the characterization of these compounds in an aqueous environment or in the natural matrix is very important. One of the most important dietary carotenoids is beta-carotene, which has been extensively studied both in vivo and in model systems, but because of the low concentration and strong interaction with the biological matrix, beta-carotene has never been observed by NMR in solid aqueous samples.In the present work, a model system has been developed for the detection and identification of beta-carotene in solid aqueous samples by 1H HR-MAS NMR. The efficiency of the model has led to the identification of beta-carotene in a raw vegetable matrix.

  3. 1D and 2D ~1H NMR studies on bisantrene complexes with short DNA oligomers

    Institute of Scientific and Technical Information of China (English)

    姚世杰; WILSON.W.David

    1995-01-01

    The binding of bisantrene to four DNA tetramers,d(CGCG)2,d(GCGC)2,d(CATG)2,and d(GTAC)2,was investigated by 1D and 2D NMR spectroscopy.Bisantrene is.a well knownanticancer drug and has been used clinically for years.DNA is believed to be one of its cellular targets.Re-suits from both ID and 2D 1H NMR are in agreement with an intercalation binding mode of bisantrene withthe four DNA tetramers in this study.The results further indicate that a threading intercalation birdingmode,in which one bisantrene side chain is in the minor groove and the other in the major groove of DNA,is preferred.The NMR results also suggest that bisantrene prefers binding at pyrimidine-(3’,5’)-purineintercalation sequences rather than at purine-(3’,5’)-pyrimidine sequences.The intramolecular andintermolecular NOE contacts of bisantrene-DNA tetramer complexes indicate that a C2’-endo uniform sugarpucker,rather than a mixed sugar conformation,is preferred by the intercalation site of both the 5’-(TA)-3’and the 5’-(CG)-3’ binding steps.

  4. Broad iron L-line and X-ray reverberation in 1H0707-495

    CERN Document Server

    Zoghbi, A; Uttley, P; Miniutti, G; Gallo, L; Reynolds, C; Miller, J; Ponti, G

    2009-01-01

    A detailed analysis of a long XMM-Newton observation of the Narrow Line Seyfert 1 galaxy 1H0707-495 is presented, including spectral fitting, spectral variability and timing studies. The two main features in the spectrum are the drop at ~ 7 keV and a complex excess below 1 keV. These are well described by two broad, K and L, iron lines. Alternative models based on absorption, although they may fit the high energy drop, cannot account for the 1 keV complexity and the spectrum as a whole. Spectral variability shows that the spectrum is composed of at least two components, which are interpreted as a power-law dominating between 1-4 keV, and a reflection component outside this range. The high count rate at the iron L energies has enabled us to measure a significant soft lag of ~ 30 s between 0.3-1 and 1-4 keV, meaning that the direct hard emission leads the reflected emissions. We interpret the lag as a reverberation signal originating within a few gravitational radii of the black hole.

  5. Continuous Flow 1H and 13C NMR Spectroscopy in Microfluidic Stripline NMR Chips

    Science.gov (United States)

    2017-01-01

    Microfluidic stripline NMR technology not only allows for NMR experiments to be performed on small sample volumes in the submicroliter range, but also experiments can easily be performed in continuous flow because of the stripline’s favorable geometry. In this study we demonstrate the possibility of dual-channel operation of a microfluidic stripline NMR setup showing one- and two-dimensional 1H, 13C and heteronuclear NMR experiments under continuous flow. We performed experiments on ethyl crotonate and menthol, using three different types of NMR chips aiming for straightforward microfluidic connectivity. The detection volumes are approximately 150 and 250 nL, while flow rates ranging from 0.5 μL/min to 15 μL/min have been employed. We show that in continuous flow the pulse delay is determined by the replenishment time of the detector volume, if the sample trajectory in the magnet toward NMR detector is long enough to polarize the spin systems. This can considerably speed up quantitative measurement of samples needing signal averaging. So it can be beneficial to perform continuous flow measurements in this setup for analysis of, e.g., reactive, unstable, or mass-limited compounds. PMID:28194934

  6. Study of Conformation and Dynamics of Molecules Adsorbed in Zeolites by 1H NMR

    Science.gov (United States)

    Michel, Dieter; Bohlmann, Winfried; Roland, Jorg; Mulla-Osman, Samir

    The chapter Study of Conformation and Dynamics of Molecules Adsorbed in Zeolites by 1H NMR is concerned with the application of high-resolution (HR) solid-state NMR techniques to study the behavior of molecules adsorbed on surfaces of nanoporous solids, such as zeolitic molecular sieves. This includes a combined or alternative application of conventional high-resolution NMR methods and of high-resolution solid-state NMR techniques, including magic-angle sample spinning (MAS), cross-polarization (CP), high-power decoupling and appropriate multiple-pulse sequences for two- or higher dimensional NMR and multiple-quantum spectroscopy. The interaction of adsorbed molecules with adsorption centers in the internal surfaces of porous solids does not only lead to changes in the reorientational and translational mobility of the molecular species but influences also the molecular conformation. Examples will be given for simple olefins in interaction with inner zeolite surfaces. Conclusions about the correlation times of the internal reorientational and translational dynamics are derived in complete agreement with the conclusion obtained from diffusion coefficients by means of PFG NMR (second chapter). Since the methodical approach of HR MAS NMR in heterogeneous systems presented here is also valuable for the investigation of lyotropic crystalline phases using HR MAS NMR (in Chap. 12) And for the NMR studies of cartilage (in Chap. 13) it was also the aim of this chapter to elucidate also the methodical background of these measurements in some more detail.

  7. Self-assembled 1-octadecyl-1H-benzimidazole film on copper surface for corrosion protection

    Indian Academy of Sciences (India)

    B V Appa Rao; M Marsihma Reddy

    2013-11-01

    Films of 1-octadecyl-1H-benzimidazole (OBI) have been formed on copper surface by selfassembly method. Optimum conditions viz. the solvent, concentration of OBI, immersion period and temperature for the formation of a protective film on copper have been established using impedance studies. The OBI film has been characterized by X-ray photoelectron spectroscopy, reflection absorption Fourier transform infrared (FTIR) spectroscopy, contact angle measurements and atomic force microscopy. Efficiency of the OBI film to protect copper from corrosion has been investigated in aq. HCl solution using electrochemical impedance spectroscopy, potentiodynamic polarization method, cyclic voltammetry, scanning electron microscopy and gravimetry. Results of these studies inferred that the OBI film has an inhibition efficiency in the range of 97-99% under different conditions. Polarization studies inferred that the OBI film functions as a cathodic inhibitor. Cyclic voltammetric studies showed that the film is stable even after 15 cycles, when the copper electrode is polarized to an anodic potential of 0.35V vs. Ag/AgCl electrode.

  8. Relativistic force field: parametric computations of proton-proton coupling constants in (1)H NMR spectra.

    Science.gov (United States)

    Kutateladze, Andrei G; Mukhina, Olga A

    2014-09-05

    Spin-spin coupling constants in (1)H NMR carry a wealth of structural information and offer a powerful tool for deciphering molecular structures. However, accurate ab initio or DFT calculations of spin-spin coupling constants have been very challenging and expensive. Scaling of (easy) Fermi contacts, fc, especially in the context of recent findings by Bally and Rablen (Bally, T.; Rablen, P. R. J. Org. Chem. 2011, 76, 4818), offers a framework for achieving practical evaluation of spin-spin coupling constants. We report a faster and more precise parametrization approach utilizing a new basis set for hydrogen atoms optimized in conjunction with (i) inexpensive B3LYP/6-31G(d) molecular geometries, (ii) inexpensive 4-31G basis set for carbon atoms in fc calculations, and (iii) individual parametrization for different atom types/hybridizations, not unlike a force field in molecular mechanics, but designed for the fc's. With the training set of 608 experimental constants we achieved rmsd <0.19 Hz. The methodology performs very well as we illustrate with a set of complex organic natural products, including strychnine (rmsd 0.19 Hz), morphine (rmsd 0.24 Hz), etc. This precision is achieved with much shorter computational times: accurate spin-spin coupling constants for the two conformers of strychnine were computed in parallel on two 16-core nodes of a Linux cluster within 10 min.

  9. Biochemical effects of gadolinium chloride in rats liver and kidney studied by 1H NMR metabolomics

    Institute of Scientific and Technical Information of China (English)

    LIAO Peiqiu; WEI Lai; Wu Huifeng; LI Weisheng; WU Yijie; LI Xiaojing; NI Jiazuan; PEI Fengkui

    2009-01-01

    The biochemical effects of gadolinium chloride were studied using high-resolution IH nuclear magnetic resonance (NMR) spec-troscopy to investigate the biochemical composition of tissue (liver and kidney) aqueous extracts obtained from control and gadolinium chlo-ride (GdCl3) (10 and 50 mg/kg body weight, intraperitoneal injection, i.p.) treated rats. Tissue samples were collected at 48, 96 and 168 h p.d. after exposure to GdCl3, and extracted using methanol/chloroform solvent system. 1H NMR spectra of tissue extracts were analyzed by pat-tern recognition using principal components analysis. The liver damages caused by GdCl3 were characterized by increased succinate and de-creased glycogen level and elevated lactate, alanine and betaine concentration in liver. Furthermore, the increase of creatine and lactate, and decrease of glutamate, alanine, phosphocholine, glycophosphocholine (GPC), betaine, myo-inositoi and trimethylamine N-oxide (TMAO)levels in kidney illustrated kidney disturbance induced by GdCl3.

  10. Metabolite signature of developmental foregut cyst on in vivo and in vitro (1)H MR spectroscopy.

    Science.gov (United States)

    Santhosh, Kannath; Thomas, Bejoy; Varma, Luxmi; Sandhyamany, S; Kesavadas, Chandrasekharan; Appukuttan, P S; Srinivas, G; Gupta, Arun Kumar; Kapilamoorthy, T R; Unnikrishnan, M

    2008-08-01

    Foregut duplication cysts are developmental anomalies of the bronchopulmonary foregut and are common cystic lesions of the mediastinum. We describe a case of mediastinal foregut duplication cyst with in vivo (1)H MR spectroscopy on a 1.5T magnet showing a large metabolite peak at 2.02 ppm, attributable to N-acetylated compounds, in addition to a smaller peak at 1.33 ppm, considered to represent lipids. In vitro NMR spectroscopy (7.05T) of cyst fluid confirmed the presence of these peaks. In addition, a broad multiplet centered at 3.7 ppm, possibly from various protons of the hexose ring system, was also noted. Chemical analysis of the cyst fluid demonstrated the presence of N-acetylhexosamines, proteins, and lipids. Again, in vitro spectra of pure samples of N-acetylglucosamine and N-acetylgalactosamine were obtained for comparison, which better resolved the N-acetyl peak and the peaks at 3.7 ppm. The mucus secreted by respiratory epithelium and the mucous glands of the foregut cysts contains glycoproteins that have N-acetylhexosamines as components and lipid breakdown products that are thought to contribute to the observed spectrum. This information might be useful in predicting the cyst content and, in turn, the lining of the epithelium and the glandular elements.

  11. 1H NMR Spectroscopy and MVA Analysis of Diplodus sargus Eating the Exotic Pest Caulerpa cylindracea

    Directory of Open Access Journals (Sweden)

    Sandra A. De Pascali

    2015-06-01

    Full Text Available The green alga Caulerpa cylindracea is a non-autochthonous and invasive species that is severely affecting the native communities in the Mediterranean Sea. Recent researches show that the native edible fish Diplodus sargus actively feeds on this alga and cellular and physiological alterations have been related to the novel alimentary habits. The complex effects of such a trophic exposure to the invasive pest are still poorly understood. Here we report on the metabolic profiles of plasma from D. sargus individuals exposed to C. cylindracea along the southern Italian coast, using 1H NMR spectroscopy and multivariate analysis (Principal Component Analysis, PCA, Orthogonal Partial Least Square, PLS, and Orthogonal Partial Least Square Discriminant Analysis, OPLS-DA. Fish were sampled in two seasonal periods from three different locations, each characterized by a different degree of algal abundance. The levels of the algal bisindole alkaloid caulerpin, which is accumulated in the fish tissues, was used as an indicator of the trophic exposure to the seaweed and related to the plasma metabolic profiles. The profiles appeared clearly influenced by the sampling period beside the content of caulerpin, while the analyses also supported a moderate alteration of lipid and choline metabolism related to the Caulerpa-based diet.

  12. 1H NMR Spectroscopy and MVA Analysis of Diplodus sargus Eating the Exotic Pest Caulerpa cylindracea

    Science.gov (United States)

    De Pascali, Sandra A.; Del Coco, Laura; Felline, Serena; Mollo, Ernesto; Terlizzi, Antonio; Fanizzi, Francesco P.

    2015-01-01

    The green alga Caulerpa cylindracea is a non-autochthonous and invasive species that is severely affecting the native communities in the Mediterranean Sea. Recent researches show that the native edible fish Diplodus sargus actively feeds on this alga and cellular and physiological alterations have been related to the novel alimentary habits. The complex effects of such a trophic exposure to the invasive pest are still poorly understood. Here we report on the metabolic profiles of plasma from D. sargus individuals exposed to C. cylindracea along the southern Italian coast, using 1H NMR spectroscopy and multivariate analysis (Principal Component Analysis, PCA, Orthogonal Partial Least Square, PLS, and Orthogonal Partial Least Square Discriminant Analysis, OPLS-DA). Fish were sampled in two seasonal periods from three different locations, each characterized by a different degree of algal abundance. The levels of the algal bisindole alkaloid caulerpin, which is accumulated in the fish tissues, was used as an indicator of the trophic exposure to the seaweed and related to the plasma metabolic profiles. The profiles appeared clearly influenced by the sampling period beside the content of caulerpin, while the analyses also supported a moderate alteration of lipid and choline metabolism related to the Caulerpa-based diet. PMID:26058009

  13. 1H NMR based metabolic profiling in Crohn's disease by random forest methodology.

    Science.gov (United States)

    Fathi, Fariba; Majari-Kasmaee, Laleh; Mani-Varnosfaderani, Ahmad; Kyani, Anahita; Rostami-Nejad, Mohammad; Sohrabzadeh, Kaveh; Naderi, Nosratollah; Zali, Mohammad Reza; Rezaei-Tavirani, Mostafa; Tafazzoli, Mohsen; Arefi-Oskouie, Afsaneh

    2014-07-01

    The present study was designed to search for metabolic biomarkers and their correlation with serum zinc in Crohn's disease patients. Crohn's disease (CD) is a form of inflammatory bowel disease that may affect any part of the gastrointestinal tract and can be difficult to diagnose using the clinical tests. Thus, introduction of a novel diagnostic method would be a major step towards CD treatment. Proton nuclear magnetic resonance spectroscopy ((1)H NMR) was employed for metabolic profiling to find out which metabolites in the serum have meaningful significance in the diagnosis of CD. CD and healthy subjects were correctly classified using random forest methodology. The classification model for the external test set showed a 94% correct classification of CD and healthy subjects. The present study suggests Valine and Isoleucine as differentiating metabolites for CD diagnosis. These metabolites can be used for screening of risky samples at the early stages of CD diagnoses. Moreover, a robust random forest regression model with good prediction outcomes was developed for correlating serum zinc level and metabolite concentrations. The regression model showed the correlation (R(2)) and root mean square error values of 0.83 and 6.44, respectively. This model suggests valuable clues for understanding the mechanism of zinc deficiency in CD patients.

  14. Regional age-related effects in the monkey brain measured with 1H magnetic resonance spectroscopy.

    Science.gov (United States)

    Ronen, Itamar; Fan, Xiaoying; Schettler, Steve; Jain, Sahil; Murray, Donna; Kim, Dae-Shik; Killiany, Ronald; Rosene, Douglas

    2011-06-01

    The rhesus monkey is a useful model for examining age-related effects on the brain, because of the extensive neuroanatomical homology between the monkey and the human brain, the tight control for neurological diseases as well as the possibility of obtaining relevant behavioral data and post-mortem tissue for histological analyses. Here, proton magnetic resonance spectroscopy ((1)H-MRS) was used together with high-resolution anatomical MRI images to carefully assess regional concentrations of brain metabolites in a group of 20 rhesus monkeys. In an anterior volume of interest (VOI) that covered frontal and prefrontal areas, significant positive correlations of myo-inositol and of total creatine concentrations with age were detected, whereas N-acetyl aspartate (NAA) and choline compounds (Cho) were not significantly correlated with age. In an occipito-parietal VOI, all metabolites showed no statistically significant age-dependent trend. Strong correlations were found between NAA concentration and gray matter fraction in the VOIs as well as between choline compounds and white matter fraction.

  15. Quantification of acesulfame potassium in processed foods by quantitative 1H NMR.

    Science.gov (United States)

    Ohtsuki, Takashi; Sato, Kyoko; Abe, Yutaka; Sugimoto, Naoki; Akiyama, Hiroshi

    2015-01-01

    Acesulfame potassium (AceK), a high-intensity and non-caloric artificial sweetener, is used in various processed foods as a food additive. In this study, we established and validated a method for determining the AceK content in various processed foods by solvent extraction and quantitative (1)H NMR, using a certified reference material as the internal standard. In the recovery test, the proposed method gave satisfactory recoveries (88.4-99.6%) and repeatabilities (0.6-5.6%) for various processed foods. The limit of quantification was confirmed as 0.13 g kg(-1), which was sufficiently low for the purposes of monitoring AceK levels. In the analysis of commercially processed foods containing AceK, all AceK contents determined by the proposed method were in good agreement with those obtained by a conventional method based on dialysis and HPLC. Moreover, this method can achieve rapid quantification and yields analytical data with traceability to the International System of Units (SI) without the need for an authentic analyte standard. Therefore, the proposed method is a useful and practical tool for the determination of AceK in processed foods.

  16. Psychophysical determination of load carrying capacity for a 1-h work period by Chinese males.

    Science.gov (United States)

    Wu, S P; Chen, C C

    2001-09-15

    This study used the psychophysical approach to examine the effects of container width, the presence or absence of container handles, and different load-carrying frequencies and distances on the maximum acceptable weight carried and the resulting response (heart rate and rating of perceived exertion) by well-conditioned males for a 1-h work period. After training, 12 male subjects performed a load-carrying task at knuckle height. Each subject performed 30 different carrying combinations. The conditions examined were container width, from 15.2 to 55.9 cm; carrying frequency, from 1 carry to 5 carries/min; and carrying distance from 1 to 6 m. The results were compared with prior studies and led to the following conclusions: (1) the use of container handles leads to the subjects carrying a significantly higher maximum acceptable weight than when containers do not have handles, which differs from the results of a previous study by Morrissey and Liou; (2) there were significant reductions in the maximum acceptable carrying weight with increases in container width, frequency and distance; (3) the presence or absence of container handles, different frequencies and load-carrying distances had significant effects on heart rate, although the effect of container width was not significant. In addition, the various frequencies and distances for load carrying had significant interaction effects on heart rate; (4) the effects of various frequencies and load-carrying distances on the rating of perceived exertion were statistically significant. The most stressed body parts were the wrists and arms.

  17. Evidence of vintage effects on grape wines using 1H NMR-based metabolomic study.

    Science.gov (United States)

    Lee, Jang-Eun; Hwang, Geum-Sook; Van Den Berg, Frans; Lee, Cherl-Ho; Hong, Young-Shick

    2009-08-19

    The chemical composition of grape wines varies with grape variety, environmental factors of climate and soil, and bacterial strains, which can each affect the wine quality. Using (1)H NMR analysis coupled with multivariate statistical data sets, we investigated the effects of grape vintage on metabolic profiles of wine and the relationship between wine metabolites and meteorological data. Principal component analysis (PCA) showed a clear differentiation between Meoru wines that were vinified with the same yeast strain and Meoru grapes harvested from the same vineyard but with a different vintage. The metabolites contributing to the differentiation were identified as 2,3-butandiol, lactic acid, alanine, proline, gamma-aminobutyric acid (GABA), choline, and polyphenols, by complementary PCA loading plot. Markedly higher levels of proline, lactic acid and polyphenols were observed in the 2006 vintage wines compared to those of 2007 vintage, showing excellent agreement with the meteorological data that the sun-exposed time and rainfall in 2006 were approximately two times more and four times less, respectively, than those in 2007. These results revealed the important role of climate during ripening period in the chemical compositions of the grape. This study highlights the reliability of NMR-based metabolomic data by integration with meteorological data in characterizing wine or grape.

  18. 1H NMR Spectroscopy and MVA Analysis of Diplodus sargus Eating the Exotic Pest Caulerpa cylindracea.

    Science.gov (United States)

    De Pascali, Sandra A; Del Coco, Laura; Felline, Serena; Mollo, Ernesto; Terlizzi, Antonio; Fanizzi, Francesco P

    2015-06-05

    The green alga Caulerpa cylindracea is a non-autochthonous and invasive species that is severely affecting the native communities in the Mediterranean Sea. Recent researches show that the native edible fish Diplodus sargus actively feeds on this alga and cellular and physiological alterations have been related to the novel alimentary habits. The complex effects of such a trophic exposure to the invasive pest are still poorly understood. Here we report on the metabolic profiles of plasma from D. sargus individuals exposed to C. cylindracea along the southern Italian coast, using 1H NMR spectroscopy and multivariate analysis (Principal Component Analysis, PCA, Orthogonal Partial Least Square, PLS, and Orthogonal Partial Least Square Discriminant Analysis, OPLS-DA). Fish were sampled in two seasonal periods from three different locations, each characterized by a different degree of algal abundance. The levels of the algal bisindole alkaloid caulerpin, which is accumulated in the fish tissues, was used as an indicator of the trophic exposure to the seaweed and related to the plasma metabolic profiles. The profiles appeared clearly influenced by the sampling period beside the content of caulerpin, while the analyses also supported a moderate alteration of lipid and choline metabolism related to the Caulerpa-based diet.

  19. Phase response curve to 1 h light pulses for the European rabbit (Oryctolagus cuniculus).

    Science.gov (United States)

    Kennedy, Gerard A; Hudson, Robyn

    2016-01-01

    While much is known about the circadian systems of rodents, chronobiological studies of other mammalian groups have been limited. One of the most extensively studied nonrodent species, both in the laboratory and in the wild, is the European rabbit. The aim of this study was to extend knowledge of the rabbit circadian system by examining its phasic response to light. Twelve Dutch-Himalayan cross rabbits of both sexes were allowed to free-run in constant darkness and then administered 1 h light pulses (1000 lux) at multiple predetermined circadian times. Changes in the phase of the rabbits' circadian wheel-running rhythms were measured after each light pulse and used to construct a phase-response curve (PRC). The rabbits' PRC and free-running period (τ) conformed to the empirical regularities reported for other predominantly nocturnal animals, including rodents and predatory marsupials. The results of the study are thus consistent with reports that the rabbit is essentially a nocturnal animal and show that it can entrain to light/dark (LD) cycles via discrete phase shifts. Knowledge about the rabbit's circadian range of entrainment to LD cycles gained in this study will be useful for examining the putative circadian processes believed to underlie the unusual rhythm of very brief, once-daily nest visits by nursing rabbit mothers and other nursing lagomorphs.

  20. MUSIC in triple-resonance experiments: amino acid type-selective (1)H-(15)N correlations

    Science.gov (United States)

    Schubert; Smalla; Schmieder; Oschkinat

    1999-11-01

    Amino acid type-selective triple-resonance experiments can be of great help for the assignment of protein spectra, since they help to remove ambiguities in either manual or automated assignment procedures. Here, modified triple-resonance experiments that yield amino acid type-selective (1)H-(15)N correlations are presented. They are based on novel coherence transfer schemes, the MUSIC pulse sequence elements, that replace the initial INEPT transfer and are selective for XH(2) or XH(3) (X can be (15)N or (13)C). The desired amino acid type is thereby selected based on the topology of the side chain. Experiments for Gly (G-HSQC); Ala (A-HSQC); Thr, Val, Ile, and Ala (TAVI-HSQC); Thr and Ala (TA-HSQC), as well as Asn and Gln (N-HSQC and QN-HSQC), are described. The new experiments are recorded as two-dimensional experiments and therefore need only small amounts of spectrometer time. The performance of the experiments is demonstrated with the application to two protein domains. Copyright 1999 Academic Press.

  1. Resolution Improvements in in Vivo1H NMR Spectra with Increased Magnetic Field Strength

    Science.gov (United States)

    Gruetter, Rolf; Weisdorf, Sally A.; Rajanayagan, Vasantham; Terpstra, Melissa; Merkle, Hellmut; Truwit, Charles L.; Garwood, Michael; Nyberg, Scott L.; Ugurbil, Kâmil

    1998-11-01

    The measurement of cerebral metabolites using highly homologous localization techniques and similar shimming methods was performed in the human brain at 1.5 and 4 T as well as in the dog and rat brain at 9.4 T. In rat brain, improved resolution was achieved by shimming all first- and second-order shim coils using a fully adiabatic FASTMAP sequence. The spectra showed a clear improvement in spectral resolution for all metabolite resonances with increased field strength. Changes in cerebral glutamine content were clearly observed at 4 T compared to 1.5 T in patients with hepatic encephalopathy. At 9.4 T, glutamine H4 at 2.46 ppm was fully resolved from glutamate H4 at 2.37 ppm, as was the potential resonance from γ-amino-butyric acid at 2.30 ppm and N-acetyl-aspartyl-glutamate at 2.05 ppm. Singlet linewidths were found to be as low as 6 Hz (0.015 ppm) at 9.4 T, indicating a substantial decrease in ppm linewidth with field strength. Furthermore, the methylene peak of creatine was partially resolved from phosphocreatine, indicating a close to 1:1 relationship in gray matter. We conclude that increasing the magnetic field strength increases spectral resolution also for1H NMR, which can lead to more than linear sensitivity gains.

  2. Homonuclear 1H NMR and circular dichroism study of the HIV-1 Tat Eli variant

    Science.gov (United States)

    Watkins, Jennifer D; Campbell, Grant R; Halimi, Hubert; Loret, Erwann P

    2008-01-01

    Background The HIV-1 Tat protein is a promising target to develop AIDS therapies, particularly vaccines, due to its extracellular role that protects HIV-1-infected cells from the immune system. Tat exists in two different lengths, 86 or 87 residues and 99 or 101 residues, with the long form being predominant in clinical isolates. We report here a structural study of the 99 residue Tat Eli variant using 2D liquid-state NMR, molecular modeling and circular dichroism. Results Tat Eli was obtained from solid-phase peptide synthesis and the purified protein was proven biologically active in a trans-activation assay. Circular dichroism spectra at different temperatures up to 70°C showed that Tat Eli is not a random coil at 20°C. Homonuclear 1H NMR spectra allowed us to identify 1639 NMR distance constraints out of which 264 were interresidual. Molecular modeling satisfying at least 1474 NMR constraints revealed the same folding for different model structures. The Tat Eli model has a core region composed of a part of the N-terminus including the highly conserved Trp 11. The extra residues in the Tat Eli C-terminus protrude from a groove between the basic region and the cysteine-rich region and are well exposed to the solvent. Conclusion We show that active Tat variants share a similar folding pattern whatever their size, but mutations induce local structural changes. PMID:18808674

  3. A 610 MHz Survey of the 1H XMM-Newton/Chandra Survey Field

    CERN Document Server

    Moss, D; McHardy, I M; Dwelly, T; Page, M J; Loaring, N S

    2007-01-01

    We present the results of a deep 610 MHz survey of the 1^H XMM/Chandra survey area with the GMRT. The resulting maps have a resolution of ~7 arcsec and an rms noise limit of 60 microJy. To a 5 sigma detection limit of 300 microJy we detect 223 sources within a survey area of diameter 64 arcmin. We compute the 610 MHz source counts and compare them to those measured at other radio wavelengths. The well know flattening of the Euclidean-normalised 1.4 GHz source counts below ~2 mJy, usually explained by a population of starburst galaxies undergoing luminosity evolution, is seen at 610 MHz. The 610 MHz source counts can be modelled by the same populations that explain the 1.4 GHz source counts, assuming a spectral index of -0.7 for the starburst galaxies and the steep spectrum AGN population. We find a similar dependence of luminosity evolution on redshift for the starburst galaxies at 610 MHz as is found at 1.4 GHz (i.e. 'Q'= 2.45 (+0.3,-0.4)).

  4. Molecular mobility in dense protein systems: an investigation through 1H NMR relaxometry and diffusometry.

    Science.gov (United States)

    Bouchoux, Antoine; Schorr, Diane; Daffé, Awa; Cambert, Mireille; Gésan-Guiziou, Geneviève; Mariette, François

    2012-09-27

    Understanding how proteins behave in highly concentrated systems is a major issue in many fields of research, including biology, biophysics, and chemical engineering. In this paper, we provide a comprehensive (1)H NMR study of molecular mobility in dilute to highly concentrated dispersions of the exact same protein (casein) but organized in two distinct supramolecular forms: spongelike casein micelles or soft casein aggregates. Both relaxometry and diffusometry experiments were performed, so that three different parameters are reported: spin-spin relaxation rates of non-water protons (1/T(2,ne)), spin-spin relaxation rates of water protons (1/T(2,e+w)), and water self-diffusion coefficients (D(w)). The results are discussed in an effort to understand the respective effects of protein crowding and protein supramolecular organization on each mobility indicator. We also examine if connections exist between the observed changes in molecular mobility and the already documented changes in rheological and osmotic properties of casein dispersions as concentration is increased.

  5. Serum Metabolomic Profiling of Sulphur Mustard-Exposed Individuals Using (1)H Nuclear Magnetic Resonance Spectroscopy.

    Science.gov (United States)

    Zamani, Zahra; Ghanei, Mostafa; Panahi, Yunus; Arjmand, Mohammad; Sadeghi, Sedigheh; Mirkhani, Fatemeh; Parvin, Shahram; Salehi, Maryam; Sahebkar, Amirhossein; Vahabi, Farideh

    2016-01-01

    Sulphur mustard is an alkylating agent that reacts with different cellular components, causing acute and delayed complications that may remain for decades after exposure. This study aimed to identify differentially expressed metabolites between mustard-exposed individuals suffering from chronic complications compared with unexposed individuals as the control group. Serum samples were obtained from 15 mustard-exposed individuals and 15 apparently healthy unexposed individuals. Metabolomic profiling was performed using (1)H nuclear magnetic resonance spectroscopy, and analyses were carried out using Chenomex and MATLAB softwares. Metabolites were identified using Human Metabolome Database, and the main metabolic pathways were identified using MetaboAnalyst software. Chemometric analysis of serum samples identified 11 differentially expressed metabolites between mustard-exposed and unexposed groups. The main pathways that were influenced by sulphur mustard exposure were related to vitamin B6 (down-regulation), bile acid (up-regulation) and tryptophan (down-regulation) metabolism. Metabolism of vitamin B6, bile acids and tryptophan are the most severely impaired pathways in individuals suffering from chronic mustard-induced complications. These findings may find implications in the monitoring of exposed patients and identification of new therapeutic approaches.

  6. /sup 1/H NMR studied of cardiostimulant polypeptides from sea anemones

    Energy Technology Data Exchange (ETDEWEB)

    Gooley, P.R.

    1985-01-01

    Sea anemones contain a series of homologous polypeptides which are potent cardiac stimulants. They exert their effect by binding to the Na/sup +/ channel of excitable membranes and delaying its closure. Although their physiological and pharmacological properties have been extensively studied, little is known about their conformations. The aim of the work described in this thesis is to characterize the solution conformation of several of these polypeptides, viz. ATXI and II from Anemonia sulcata and AP-A from Anthopleura xanthogrammica, by using high resolution /sup 1/H Nuclear Magnetic Resonance spectroscopy at 300 MHz. Resonances are assigned to amino acid types by a variety of techniques, including pH dependence and two-dimensional homonuclear correlated spectroscopy (COSY). The assignments reveal extensive conformational heterogeneity in AP-A and ATXII, but not in ATXI. The heterogeneity, manifested in the splitting of a number of resonances, is explained in terms of cis-trans isomerism of the peptide bond preceding Pro-41. Information on the secondary and tertiary structures of these polypeptides has been obtained from NOE data. The polypeptides undergo a conformational change at low pH reflecting pK/sub a/ values of 1.7/2.5, 3.0 and 1.9/2.3 for AP-A, ATXI and ATXII, respectively.

  7. Differential Effects of Dry Eye Disorders on Metabolomic Profile by 1H Nuclear Magnetic Resonance Spectroscopy

    Directory of Open Access Journals (Sweden)

    Carmen Galbis-Estrada

    2014-01-01

    Full Text Available We used 1H NMR spectroscopy to analyze the metabolomic profile of reflex tears from patients with dry eye disorders (DEDs. 90 subjects were divided into 2 groups: (1 patients with DEDs (DEDG; n = 55 and (2 healthy subjects (CG; n = 35. Additionally, the DEDG was subdivided into 2 subgroups based on DED severity: mild-to-moderate and moderate (n = 22 and n = 33, resp.. Personal interviews and systematized ophthalmologic examinations were carried out. Reflex tears (20–30 μL were collected by gently rubbing in the inferior meniscus of both eyelids with a microglass pipette and stored at −80°C until analysis. NMR spectra were acquired using a standard one-dimensional pulse sequence with water suppression. Data were processed and transferred to MATLAB for further chemometric analysis. Main differences in tear composition between DEDG and CG were found in cholesterol, N-acetylglucosamine, glutamate, creatine, amino-n-butyrate, choline, acetylcholine, arginine, phosphoethanolamine, glucose, and phenylalanine levels. This metabolic fingerprint helped also to discriminate between the three additional subgroups of DEDG. Our results suggest that tear metabolic differences between DEDG and CG identified by NMR could be useful in understanding ocular surface pathogenesis and improving biotherapy.

  8. 1H and 13C NMR spectral assignments of chalcones bearing pyrazoline-carbothioamide groups.

    Science.gov (United States)

    Yoon, Hyuk; Ahn, Seunghyun; Park, Mijoo; Kim, Dong-Wook; Kim, Sang Ho; Koh, Dongsoo; Lim, Yoongho

    2013-08-01

    Chalcones are known to act on various physiological targets. As a result, structural modifications of chalcones have been studied extensively. Benzochalcones, in which the A-ring of chalcone is substituted with a naphthalene unit, inhibits breast cancer resistance protein. Chalcones in which the α,β-unsaturated carbonyl group is switched with a pyrazoline moiety are potent cytotoxic agents against various cancer cell lines, and chalcones with a pyrazoline-1-carbothioamide group instead of an α,β-unsaturated carbonyl group exhibit antimicrobial activities. The present report describes hybrid molecules designed from benzochalcone and pyrazoline-carbothioamide. Methoxylation of plant-derived polyphenols alters their hydrophobicity, resulting in changes in biological function and intracellular compartmentation. In the current study, 22 novel methoxylated 3-(naphthalen-2-yl)-N,5-diphenyl-pyrazoline-1-carbothioamide derivatives were prepared. This report provides complete assignments of their (1)H and (13)C NMR data, which can be used to subsequently identify chalcones bearing pyrazoline-carbothioamide groups.

  9. Computerized MRS voxel registration and partial volume effects in single voxel 1H-MRS.

    Science.gov (United States)

    Lee, Hedok; Caparelli, Elisabeth; Li, Haifang; Mandal, Amit; Smith, S David; Zhang, Shaonan; Bilfinger, Thomas V; Benveniste, Helene

    2013-09-01

    Partial volume effects in proton magnetic resonance spectroscopy in the brain have been studied previously in terms of proper water concentration calculations, but there is a lack of disclosure in terms of voxel placement techniques that would affect the calculations. The purpose of this study is to facilitate a fully automated MRS voxel registration method which is time efficient, accurate, and can be extended to all imaging modalities. A total of thirteen healthy adults underwent single voxel 1H-MRS scans in 3.0T MRI scanners. Transposition of a MRS voxel onto an anatomical scan is derived along with a full calculation of water concentration with a correction term to account for the partial volume effects. Five metabolites (tNAA, Glx, tCr, mI, and tCho) known to yield high reliability are studied. Pearson's correlation analyses between tissue volume fractions and metabolite concentrations were statistically significant in parietal (tCr, Glx, and tNAA) lobe and occipital lobe (tNAA). MRS voxel overlaps quantified by dice metric over repeated visits yielded 60%~70% and coefficients of variance in metabolites concentration were 4%~10%. These findings reiterate an importance of considering the partial volume effects when tissue water is used as an internal concentration reference so as to avoid misinterpreting a morphometric difference as a metabolic difference.

  10. 1H NMR study of robustoxin, the lethal neurotoxin from the funnel web spider Atrax robustus.

    Science.gov (United States)

    Temple, M D; Hinds, M G; Sheumack, D D; Howden, M E; Norton, R S

    1999-03-01

    Robustoxin, the lethal neurotoxin from the Sydney funnel web spider Atrax robustus, is a polypeptide of 42 residues cross-linked by four disulfide bonds. This paper describes the sequence-specific assignment of resonances in the 1H nuclear magnetic resonance spectrum of robustoxin in aqueous solution. Several broad backbone amide resonances were encountered in spectra recorded at 27 degrees C, making the assignments at that temperature incomplete. In spectra recorded at lower temperatures these amide resonances became sharper, but others that were sharp at 27 degrees C became broad, indicative of conformational averaging on the millisecond timescale for certain regions of the structure. Nevertheless, it was possible to establish that robustoxin contains a small, triple-stranded, antiparallel beta-sheet and several reverse turns, but no alpha-helix. These observations indicate that this toxin may adopt the inhibitor cystine knot structure found in polypeptides from a diverse range of species, including a number of spiders. Analysis of the pH dependence of the spectrum yielded pKa values for Tyr22 and Tyr25, one of the three carboxyl groups, and the Lys residues.

  11. Interplay of Nitrogen-Atom Inversion and Conformational Inversion in Enantiomerization of 1H-1-Benzazepines.

    Science.gov (United States)

    Ramig, Keith; Subramaniam, Gopal; Karimi, Sasan; Szalda, David J; Ko, Allen; Lam, Aaron; Li, Jeffrey; Coaderaj, Ani; Cavdar, Leyla; Bogdan, Lukasz; Kwon, Kitae; Greer, Edyta M

    2016-04-15

    A series of 2,4-disubstituted 1H-1-benzazepines, 2a-d, 4, and 6, were studied, varying both the substituents at C2 and C4 and at the nitrogen atom. The conformational inversion (ring-flip) and nitrogen-atom inversion (N-inversion) energetics were studied by variable-temperature NMR spectroscopy and computations. The steric bulk of the nitrogen-atom substituent was found to affect both the conformation of the azepine ring and the geometry around the nitrogen atom. Also affected were the Gibbs free energy barriers for the ring-flip and the N-inversion. When the nitrogen-atom substituent was alkyl, as in 2a-c, the geometry of the nitrogen atom was nearly planar and the azepine ring was highly puckered; the result was a relatively high-energy barrier to ring-flip and a low barrier to N-inversion. Conversely, when the nitrogen-atom substituent was a hydrogen atom, as in 2d, 4, and 6, the nitrogen atom was significantly pyramidalized and the azepine ring was less puckered; the result here was a relatively high energy barrier to N-inversion and a low barrier to ring-flip. In these N-unsubstituted compounds, it was found computationally that the lowest-energy stereodynamic process was ring-flip coupled with N-inversion, as N-inversion alone had a much higher energy barrier.

  12. Experimental and DFT studies on the vibrational spectra of 1H-indene-2-boronic acid

    Science.gov (United States)

    Alver, Özgur; Kaya, Mehmet Fatih

    2014-11-01

    Stable conformers and geometrical molecular structures of 1H-indene-2-boronic acid (I-2B(OH)2) were studied experimentally and theoretically using FT-IR and FT-Raman spectroscopic methods. FT-IR and FT-Raman spectra were recorded in the region of 4000-400 cm-1, and 3700-400 cm-1, respectively. The optimized geometric structures were searched by Becke-3-Lee-Yang-Parr (B3LYP) hybrid density functional theory method with 6-31++G(d,p) basis set. Vibrational wavenumbers of I-2B(OH)2 were calculated using B3LYP density functional methods including 6-31++G(d,p) basis set. Experimental and theoretical results show that density functional B3LYP method gives satisfactory results for predicting vibrational wavenumbers except OH stretching modes which is probably due to increasing unharmonicity in the high wave number region and possible intra and inter molecular interaction at OH edges. To support the assigned vibrational wavenumbers, the potential energy distribution (PED) values were also calculated using VEDA 4 (Vibrational Energy Distribution Analysis) program.

  13. Combined Analysis of Stable Isotope, (1)H NMR, and Fatty Acid To Verify Sesame Oil Authenticity.

    Science.gov (United States)

    Kim, Jeongeun; Jin, Gyungsu; Lee, Yunhee; Chun, Hyang Sook; Ahn, Sangdoo; Kim, Byung Hee

    2015-10-14

    The aim of this study was to verify the authenticity of sesame oils using combined analysis of stable isotope ratio, (1)H NMR spectroscopy, and fatty acid profiles of the oils. Analytical data were obtained from 35 samples of authentic sesame oils and 29 samples of adulterated sesame oils currently distributed in Korea. The orthogonal projection to latent structure discriminant analysis technique was used to select variables that most effectively verify the sesame oil authenticity. The variables include δ(13)C value, integration values of NMR peaks that signify the CH3 of n-3 fatty acids, CH2 between two C═C, protons from sesamin/sesamolin, and 18:1n-9, 18:3n-3, 18:2t, and 18:3t content values. The authenticity of 65 of 70 blind samples was correctly verified by applying the range of the eight variables found in the authentic sesame oil samples, suggesting that triple analysis is a useful approach to verify sesame oil authenticity.

  14. Brain biochemistry in Duchenne muscular dystrophy: a 1H magnetic resonance and neuropsychological study.

    Science.gov (United States)

    Rae, C; Scott, R B; Thompson, C H; Dixon, R M; Dumughn, I; Kemp, G J; Male, A; Pike, M; Styles, P; Radda, G K

    1998-10-08

    Duchenne muscular dystrophy (DMD) is a progressive muscle disorder associated with an intellectual deficit which is non-progressive. We obtained localised 1H magnetic resonance spectra from the left frontal lobe and left cerebellum of 15 boys with DMD (mean age 106 months+/-32) and 15 similarly aged control boys (mean age 115 months+/-31); all boys underwent a battery of neuropsychological tests. We found a significant (PAnalogies Test (MAT). The MAT is a test of visuo-spatial ability and non-verbal reasoning which requires neither manual dexterity nor a verbal response for an adequate performance. A comparison of DMD boys whose cerebellar Cho/NA fell within 2 standard deviations of the control norm (0.56+/-0.24) with DMD boys whose cerebellar Cho/NA was outside this range (i.e. >0.80) revealed a significant difference in ability on the MAT (P<0.05). DMD boys whose Cho/NA ratio is more than two standard deviations higher than controls perform significantly better on the MAT than DMD boys whose Cho/NA ratio is within the normal range. This finding suggests that the observed elevation in Cho/NA and Cho/creatine is not associated with intellectual deficit (as sampled by the MAT), and may represent a compensatory mechanism. The possible interpretations of these metabolic changes are discussed.

  15. Three-dimensional solution structure of ω-conotoxin SO3 determined by 1H NMR

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    Cone snails (Conus) elaborate a series of conotoxin (CTX) peptides in their venoms to paralyze their prey. Among these toxins, ω-CTX's specifically target to presynaptic voltage-gated calcium channel subsets, causing inhibition of neurotransmitter release. Ω-CTX SO3 was isolated from the venom of Conus striatus, which is the only available fish-hunting snail near the coast of the South China Sea. The three-dimensional solution structure of ω-CTX SO3, a peptide which is the only ω-conotoxin reported to show high homology with another ω-CTX (MVIIA from C. Magus), has been determined by 1H NMR techniques. The molecular structure of ω-CTX SO3 is stabilized by three disulfide bridges and a short triple-stranded antiparallel ω-sheet with four turns. A comprehensive comparison suggested that the backbone conformation of ω-CTX's was quite conserved, while the length of ω-sheet and the type of some turns might have minor differences.

  16. 1H NMR-based metabolic profiling for evaluating poppy seed rancidity and brewing.

    Science.gov (United States)

    Jawień, Ewa; Ząbek, Adam; Deja, Stanisław; Łukaszewicz, Marcin; Młynarz, Piotr

    2015-12-01

    Poppy seeds are widely used in household and commercial confectionery. The aim of this study was to demonstrate the application of metabolic profiling for industrial monitoring of the molecular changes which occur during minced poppy seed rancidity and brewing processes performed on raw seeds. Both forms of poppy seeds were obtained from a confectionery company. Proton nuclear magnetic resonance (1H NMR) was applied as the analytical method of choice together with multivariate statistical data analysis. Metabolic fingerprinting was applied as a bioprocess control tool to monitor rancidity with the trajectory of change and brewing progressions. Low molecular weight compounds were found to be statistically significant biomarkers of these bioprocesses. Changes in concentrations of chemical compounds were explained relative to the biochemical processes and external conditions. The obtained results provide valuable and comprehensive information to gain a better understanding of the biology of rancidity and brewing processes, while demonstrating the potential for applying NMR spectroscopy combined with multivariate data analysis tools for quality control in food industries involved in the processing of oilseeds. This precious and versatile information gives a better understanding of the biology of these processes.

  17. Strong impact of the solvent on the photokinetics of a 2(1H)-pyrimidinone.

    Science.gov (United States)

    Ryseck, G; Villnow, T; Hugenbruch, S; Schaper, K; Gilch, P

    2013-08-01

    Pyrimidinones are part of the (6-4) photolesions which may be formed from two pyrimidine bases adjacent on a DNA strand. In relation to the secondary photochemistry of the (6-4) lesion, i.e. its transformation into a Dewar valence isomer, photophysical and photochemical properties of 1-methyl-2(1H)-pyrimidinone (1MP) in water, acetonitrile, methanol, and 1,4-dioxane are reported here. As deduced from steady state fluorescence and femtosecond transient absorption spectroscopy the S1 lifetime of 1MP is strongly affected by the solvent. The lifetimes range from 400 ps for water to 40 ps for 1,4-dioxane. Internal conversion (IC) and intersystem crossing (ISC) contribute to the S1 decay. The solvent effect on the IC rate constant is more pronounced than on the ISC constant. The quantum yields for the consumption of 1MP (values for nitrogen purged solvents) are large for methanol (0.35) and 1,4-dioxane (0.24) and small for acetonitrile (0.02) and water (0.003). Hydrogen abstraction from the solvent by the triplet state of 1MP may rationalize this.

  18. Lipid composition of integral purple membrane by 1H and 31P NMR.

    Science.gov (United States)

    Renner, Christian; Kessler, Brigitte; Oesterhelt, Dieter

    2005-08-01

    In the purple membrane (PM) of halobacteria, lipids stabilize the trimeric arrangement of bacteriorhodopsin (BR) molecules and mediate the packing of the trimers in a regular crystalline arrangement. To date, the identification and quantification of these lipids has been based either on lipid extraction procedures or structural models. By directly solubilizing PMs from Halobacterium salinarum in aqueous detergent solutions (SDS or Triton X-100), we avoided any separation or modification steps that might modify the lipid composition or even the lipid molecules themselves. Our analysis of integral PM preparations should resolve partially conflicting literature data on the lipid composition of the PM. Using 31P and 1H NMR of detergent-solubilized but otherwise untreated samples, we found two glycolipids and 6.4 +/- 0.1 phospholipids per BR molecule, 4.4 +/- 0.1 of the latter being the phosphatidylglycerophosphate methyl ester. The only glycolipid detected was S-TGD-1. For an additional glycolipid, glycocardiolipin, that was recently identified in lipid extracts, we show that it was produced mainly during the lipid extraction procedure but also was partially dependent on the preparation of the PM suspensions.

  19. [Shortening of the measurement time by 1H-MR turbo spectroscopic imaging of the brain].

    Science.gov (United States)

    Träber, F; Block, W; Lamerichs, R; Keller, E; Schild, H H

    1997-03-01

    Development of a new technique for reduction of measurement time in 1H-MR spectroscopic imaging of the brain. Optimisation of the sequence parameters in volunteer and in patient examinations and comparison to the results obtained with conventional 2 D-SI. Examination of 20 healthy volunteers and 5 patients in a 1.5 T whole-body MR system. In "turbo-spectroscopic imaging" (TSI) sequences, a train of spin-echo signals with different phase encoding is acquired after each 90 degrees excitation. 32 x 32 matrix elements covered a field of view of 20 cm, and additional volume selection was performed by double spin echo excitation. Measurement duration 9 min with acquisition of four phase encoding steps per TR interval, whereas the corresponding 2 D-SI sequence (TR/TE 2000/272 ms) took 30 min. The TSI data sets yielded maps of the regional distribution of metabolite concentrations with a quality comparable to the 2 D-SI results. Signal homogeneity and delineation of brain lesions, however, were superior in conventional spectroscopic imaging. The T2 relaxation of the metabolites required a reduced sampling interval for each phase-encoded echo, and hence the frequency resolution of the corresponding TSI spectra was not always sufficient for separating choline and creatine signals. With measurement durations TSI technique allows in clinical studies a combination with single-voxel MRS for accurate quantification and with a diagnostic MRI within a total examination time of less than one hour.

  20. Identification of a de novo DYNC1H1 mutation via WES according to published guidelines

    Science.gov (United States)

    Ding, Dongxue; Chen, Zhao; Li, Kai; Long, Zhe; Ye, Wei; Tang, Zhaoli; Xia, Kun; Qiu, Rong; Tang, Beisha; Jiang, Hong

    2016-01-01

    De novo mutations that contribute to rare Mendelian diseases, including neurological disorders, have been recently identified. Whole-exome sequencing (WES) has become a powerful tool for the identification of inherited and de novo mutations in Mendelian diseases. Two important guidelines were recently published regarding the investigation of causality of sequence variant in human disease and the interpretation of novel variants identified in human genome sequences. In this study, a family with supposed movement disorders was sequenced via WES (including the proband and her unaffected parents), and a standard investigation and interpretation of the identified variants was performed according to the published guidelines. We identified a novel de novo mutation (c.2327C > T, p.P776L) in DYNC1H1 gene and confirmed that it was the causal variant. The phenotype of the affected twins included delayed motor milestones, pes cavus, lower limb weakness and atrophy, and a waddling gait. Electromyographic (EMG) recordings revealed typical signs of chronic denervation. Our study demonstrates the power of WES to discover the de novo mutations associated with a neurological disease on the whole exome scale, and guidelines to conduct WES studies and interpret of identified variants are a preferable option for the exploration of the pathogenesis of rare neurological disorders. PMID:26846447

  1. Nuclear localization of human DNA mismatch repair protein exonuclease 1 (hEXO1)

    DEFF Research Database (Denmark)

    Knudsen, Nina Østergaard; Nielsen, Finn Cilius; Vinther, Lena

    2007-01-01

    localization signals (NLSs) in hEXO1. Using fluorescent fusion proteins, we show that the sequence 418KRPR421, which exhibit strong homology to other monopartite NLS sequences, is responsible for correct nuclear localization of hEXO1. This NLS sequence is located in a region that is also required for hEXO1......Human exonuclease 1 (hEXO1) is implicated in DNA mismatch repair (MMR) and mutations in hEXO1 may be associated with hereditary nonpolyposis colorectal cancer (HNPCC). Since the subcellular localization of MMR proteins is essential for proper MMR function, we characterized possible nuclear...... interaction with hMLH1 and we show that defective nuclear localization of hEXO1 mutant proteins could be rescued by hMLH1 or hMSH2. Both hEXO1 and hMLH1 form complexes with the nuclear import factors importin beta/alpha1,3,7 whereas hMSH2 specifically recognizes importin beta/alpha3. Taken together, we infer...

  2. Potassium 3-oxo-2,3-dihydro-1H-inden-4-olate: Formation, molecular and electronic structure

    Science.gov (United States)

    Sigalov, Mark; Shainyan, Bagrat; Sterkhova, Irina

    2016-11-01

    Unlike 1-indanone, 7-hydroxy-1-indanone does not enter the base-catalyzed condensation reaction with 1H-pyrrole-2-carbaldehyde but, instead, gives the salt, potassium 3-oxo-2,3-dihydro-1H-inden-4-olate dihydrate. X-ray analysis, NMR, IR, UV spectroscopy, DFT and MP2 calculations allowed to prove the chelate structure of the salt and to estimate the effect of chelation on the spectral properties as well as to explain the specific reactivity.

  3. Complete {sup 1}H and {sup 13}C NMR structural assignments for a group of four goyazensolide-type furanoheliangolides

    Energy Technology Data Exchange (ETDEWEB)

    Soares, Ana Carolina Ferreira; Silva, Aline Nazare; Matos, Priscilla Mendonca; Silva, Eder Henrique da; Heleno, Vladimir Constantino Gomes [Universidade de Franca, Franca, SP (Brazil). Nucleo de Pesquisas em Ciencias Exatas e Tecnologicas; Lopes, Norberto Peporine; Lopes, Joao Luis Callegari [Universidade de Sao Paulo (FCFRP/USP), Ribeirao Preto, SP (Brazil). Fac. de Ciencias Farmaceuticas de Ribeirao Preto. Dept. de Quimica e Fisica; Sass, Daiane Cristina, E-mail: vheleno_05@yahoo.com.br [Universidade de Sao Paulo (FFCLRP/USP), Ribeirao Preto, SP (Brazil). Fac. de Filosofia, Ciencias e Letras de Ribeirao Preto. Dept. de Quimica

    2012-07-01

    Four goyazensolide-type sesquiterpene lactones - lychnofolide, centratherin, goyazensolide and goyazensolide acetate - were thoroughly studied by NMR experimental techniques. {sup 1}H NMR, {sup 13}C NMR {l_brace}{sup 1}H{r_brace}, COSY, HMQC, HMBC, J-res. and NOE experiments were performed to provide the needed structural information. Complete and unequivocal assignment, including the determination of all multiplicities, was obtained for each structure and the data collections are presented in tables (author)

  4. Solid-phase synthesis of the 2(1H)-pyrazinone scaffold: a new approach toward diversely substituted heterocycles.

    Science.gov (United States)

    Kaval, Nadya; Dehaen, Wim; Van der Eycken, Erik

    2005-01-01

    The first solid-phase synthesis of the 2(1H)-pyrazinone scaffold is described. The diversity at position C6 of the pyrazinone ring is determined by the choice of the starting aldehyde. Microwave-enhanced transition metal-catalyzed reactions allow easy introduction of a variety of substituents at the C3 position. This opens a way for the generation of libraries of diversely substituted 2(1H)-pyrazinones that will be screened for biological activities.

  5. A Synthesis of 1H-Indazoles via a Cu(OAc)2-Catalyzed N-N Bond Formation.

    Science.gov (United States)

    Chen, Cheng-yi; Tang, Guangrong; He, Fengxian; Wang, Zhaobin; Jing, Hailin; Faessler, Roger

    2016-04-01

    A facile synthesis of 1H-indazoles featuring a Cu(OAc)2-catalyzed N-N bond formation using oxygen as the terminal oxidant is described. The reaction of readily available 2-aminobenzonitriles with various organometallic reagents led to o-aminoaryl N-H ketimine species. The subsequent Cu(OAc)2-catalyzed N-N bond formation in DMSO under oxygen afforded a wide variety of 1H-indazoles in good to excellent yields.

  6. Synthesis of new 2-aryl-6-styryl-2,3-dihydropyridin-4(1H)-one derivatives from curcuminoids

    Institute of Scientific and Technical Information of China (English)

    Ying Peng Huo; Xu Qiu; Wei Yan Shao; Lin Kun An; Xian Zhang Bu; Lian Quan Gu

    2009-01-01

    Series of new 2-aryl-6-styryl-2,3-dihydropyridin-4(1H)-one derivatives were synthesized in acceptable to good yields by treatment of the curcuminoids with aqueous ammonia, the mechanism was proposed. By modification of the primary products, total 13 new compounds were obtained. The structures of all products were elucidated by spectroscopy analysis including HR-MS, ~1H NMR and ~(13)C NMR.

  7. Bioactive 2(1H-Pyrazinones and Diketopiperazine Alkaloids from a Tunicate-Derived Actinomycete Streptomyces sp.

    Directory of Open Access Journals (Sweden)

    Lamiaa A. Shaala

    2016-08-01

    Full Text Available As a part of our ongoing effort to allocate marine microbial bioactive leads, a tunicate-derived actinomycete, Streptomyces sp. Did-27, was investigated. Three new 2(1H-pyrazinones derivatives, (S-6-(sec-butyl-3-isopropylpyrazin-2(1H-one (1, (S-3-(sec-butyl-6-isopropylpyrazin-2(1H-one (2 and (S-6-(sec-butyl-3-isobutylpyrazin-2(1H-one (3, together with the known (1H-pyrazinones analogues deoxymutaaspergillic acid (4, 3,6-diisobutyl-2(1H-pyrazinone (5 and 3,6-di-sec-butyl-2(1H-pyrazinone (6, and the diketopiperazine alkaloids cyclo(6-OH-d-Pro-l-Phe (7, bacillusamide B (8, cyclo(l-Pro-l-Leu and cyclo(l-Pro-l-Ile (10 were isolated from this strain. The structures of the compounds were determined by study of their one- and two-dimensional NMR spectra as well as high-resolution mass spectral determinations. Compound 4 was reported previously as a synthetic product, while compound 6 was reported as 2-hydroxy-3,6-di-sec-butylpyrazine. Herein, we report the complete NMR data for compounds 4 and 6. The compounds were evaluated for their cytotoxic activities against three cell lines. Compound 5 showed potent and selective activity against HCT-116 cell line with IC50 of 1.5 μg/mL, while 1–10 showed variable cytotoxic activities against these cancer cell lines. These results provide further understanding about the chemistry and bioactivities of the alkylated 2(1H-pyrazinone derivatives.

  8. Syntheses of Some 3-[1'( 1' H )-Substituent-pyrazol-5'-yl ] benzo [5,6] coumarins

    Institute of Scientific and Technical Information of China (English)

    EL-DEEN, Ibrahim Mohey; AL-WAKEEL, El-Sayed Ismail; El-MAWLA, Ahmed Gad

    2002-01-01

    3-[1' (1' H)-Substitueut-pyrazol-5'-yl] benzo [ 5, 6] coumarins and 3-(1' , 2 '-oxazol- 5 '- yl ) benzo [ 5 , 6 ] coumarin were prepared via condensation of 3-(2'-formyl-1'-chlorovinyl) benzo [ 5, 6]coumarin with hydrazine derivatives or hydroxylamine. Reaction of 3-[1' (1'H)-pyrazol-5'-yl] benzo[5, 6] coumarin with alkyl halides, olefinic compounds or acid chlorides are described.

  9. ATP6V1H Deficiency Impairs Bone Development through Activation of MMP9 and MMP13

    Science.gov (United States)

    Zhao, Gexin; Yokoyama, Tadafumi; Huang, Yan; Bishop, Kevin; Maduro, Valerie; Accardi, John; Toro, Camilo; Boerkoel, Cornelius F.; Gahl, William A.; Duan, Xiaohong; Malicdan, May Christine V.; Lin, Shuo

    2017-01-01

    ATP6V1H is a component of a large protein complex with vacuolar ATPase (V-ATPase) activity. We identified two generations of individuals in which short stature and osteoporosis co-segregated with a mutation in ATP6V1H. Since V-ATPases are highly conserved between human and zebrafish, we generated loss-of-function mutants in atp6v1h in zebrafish through CRISPR/Cas9-mediated gene knockout. Homozygous mutant atp6v1h zebrafish exhibited a severe reduction in the number of mature calcified bone cells and a dramatic increase in the expression of mmp9 and mmp13. Heterozygous adults showed curved vertebra that lack calcified centrum structure and reduced bone mass and density. Treatment of mutant embryos with small molecule inhibitors of MMP9 and MMP13 significantly restored bone mass in the atp6v1h mutants. These studies have uncovered a new, ATP6V1H-mediated pathway that regulates bone formation, and defines a new mechanism of disease that leads to bone loss. We propose that MMP9/MMP13 could be therapeutic targets for patients with this rare genetic disease. PMID:28158191

  10. Differential protonation and dynamic structure of doxylamine succinate in solution using 1H and 13C NMR.

    Science.gov (United States)

    Somashekar, B S; Nagana Gowda, G A; Ramesha, A R; Khetrapal, C L

    2004-07-01

    A protonation and dynamic structural study of doxylamine succinate, a 1:1 salt of succinic acid with dimethyl-[2-(1-phenyl-1-pyridin-2-yl-ethoxy)ethyl]amine, in solution using one- and two-dimensional 1H and 13C NMR experiments at variable temperature and concentration is presented. The two acidic protons of the salt doxylamine succinate are in 'intermediate' exchange at room temperature, as evidenced by the appearance of a broad signal. This signal evolves into two distinct signals below about -30 degrees C. A two-dimensional 1H-1H double quantum filtered correlation experiment carried out at -55 degrees C shows protonation of one of the acidic protons to the dimethylamine nitrogen. A two-dimensional rotating frame 1H-1H NOE experiment at the same temperature reveals that the other proton remains with the succinate moiety. Comparison of the 1H and 13C chemical shifts and the 13C T1 relaxation times of the salt with those of the free base further substantiate the findings.

  11. Dark Matter and Dark Force in the Type-I Inert 2HDM with Local U(1)_H Gauge Symmetry

    CERN Document Server

    Ko, P; Yu, Chaehyun

    2014-01-01

    We discuss dark matter (DM) physics in the Type-I inert two-Higgs-doublet model (2HDM) with local U(1)_H Higgs gauge symmetry. The local U(1)_H gauge symmetry is assigned to the extra Higgs doublet in order to avoid the Higgs-mediated flavor problems, and it spontaneously breaks down to its discrete subgroup. The lightest neutral scalar component H of the U(1)_H-charged Higgs doublet, which does not have Yukawa couplings with the Standard-Model (SM) fermions, is stable because of the remnant discrete symmetry, and it interacts with the SM particles through the U(1)_H gauge boson (Z_H) exchange as well as the SM boson exchange. We first investigate the constraint on the U(1)_H gauge interaction, especially through the kinetic and mass mixing between the SM gauge bosons and the extra gauge boson. Then we discuss dark matter physics in our 2HDM: thermal relic density, and direct/indirect detections of dark matter. The additional U(1)_H gauge interaction plays a crucial role in reducing the DM thermal relic densi...

  12. Efficient colonization and therapy of human hepatocellular carcinoma (HCC using the oncolytic vaccinia virus strain GLV-1h68.

    Directory of Open Access Journals (Sweden)

    Ivaylo Gentschev

    Full Text Available Virotherapy using oncolytic vaccinia virus strains is one of the most promising new strategies for cancer therapy. In this study, we analyzed for the first time the therapeutic efficacy of the oncolytic vaccinia virus GLV-1h68 in two human hepatocellular carcinoma cell lines HuH7 and PLC/PRF/5 (PLC in cell culture and in tumor xenograft models. By viral proliferation assays and cell survival tests, we demonstrated that GLV-1h68 efficiently colonized, replicated in, and did lyse these cancer cells in culture. Experiments with HuH7 and PLC xenografts have revealed that a single intravenous injection (i.v. of mice with GLV-1h68 resulted in a significant reduction of primary tumor sizes compared to uninjected controls. In addition, replication of GLV-1h68 in tumor cells led to strong inflammatory and oncolytic effects resulting in intense infiltration of MHC class II-positive cells like neutrophils, macrophages, B cells and dendritic cells and in up-regulation of 13 pro-inflammatory cytokines. Furthermore, GLV-1h68 infection of PLC tumors inhibited the formation of hemorrhagic structures which occur naturally in PLC tumors. Interestingly, we found a strongly reduced vascular density in infected PLC tumors only, but not in the non-hemorrhagic HuH7 tumor model. These data demonstrate that the GLV-1h68 vaccinia virus may have an enormous potential for treatment of human hepatocellular carcinoma in man.

  13. Single voxel 1 H magnetic resonance spectroscopy in the diagnosis of musculoskeletal mass lesions

    Directory of Open Access Journals (Sweden)

    Shalini Agarwal

    2014-01-01

    Full Text Available Introduction: In vivo magnetic resonance spectroscopy (MRS is an established technique for evaluation of malignant tumors in brain, breast, prostate, etc., However, its efficacy in the diagnosis of musculoskeletal (MSK mass lesions is yet to be established. We present our experience with MRS of these lesions. Materials and Methods: Magnetic resonance imaging (MRI, dynamic contrast-enhanced MRI and single-voxel 1 H MRS was performed in 30 consecutive patients with histologically proven benign and malignant MSK tumors/mass lesions each, on a 1.5-T magnetic resonance scanner. MRS was performed with echo times (TE of 40, 135 and 270 ms. A clearly identifiable peak at 3.2 ppm in at least two of the three spectra acquired at the three TE was taken as positive for choline. MRS imaging and enhancement patterns were compared in these two groups and were analyzed by a Radiologist blinded to the histopathological findings. Results: Ages of patients in the malignant age group ranged from 2 to 65 years (M: F - 19:11 while that of patients in the benign group ranged from 7 months to 56 years (M: F - 17:13. There were two patients with Type I curve, 18 with Type II curve and 10 with Type III curve on dynamic contrast enhanced images in the malignant group while there were no patients with Type I curve, 5 with Type II curve and 25 with Type III curve in the benign group. The sensitivity of MRS for predicting malignancy was 60%, specificity was 93.33%, positive predictive value was 90%, negative predictive value was 70% and accuracy was 76.66%. Conclusion: MRS is a promising technique for evaluation of MSK mass lesions. The accuracy at present remains low. We recommend that it be used as an adjunct to routine MRI.

  14. Isolation and quantification of pinitol in Argyrolobium roseum plant, by 1H-NMR

    Directory of Open Access Journals (Sweden)

    Neha Sharma

    2016-01-01

    Full Text Available Chemical investigations on ethanolic extract of Argyrolobium roseum led to the isolation of Pinitol as the major constituent of the plant. Pinitol is chemically known as 3-O-methyl-D-Chiro-inositol and has been found to possess anti-diabetic activity. It helps in the regeneration of beta cells, present in the areas of the pancreas called as islets – of Langerhans. These cells make and release insulin, a hormone which controls the level of glucose in the blood. Pinitol was isolated from the ethanolic extract of the plant and a sensitive & reliable method, based on Proton Nuclear Magnetic Resonance (PNMR, was developed and used as an analytical tool for quantification and identification of this relatively UV insensitive compound in the alcoholic extract of the plant. The method involves the use of pyrazinamide (an anti-tuberculosis drug, as a reference. Validation of the method was carried out by preparing a known concentration of an artificial mixture of pinitol and pyrazinamide. The recovery of pinitol in the mixture was in the range of 98.5–101.3%. Pinitol in pure form was isolated from the ethanolic extract of A. roseum by repeated column chromatography over silica gel followed by crystallization in methanol. Pinitol isolated from the plant was identified on the basis of 1H-NMR, 13C-NMR, DEPT (45°, 90° and 135° experiments and mass spectral data. The method was successfully applied for the quantitation of pinitol in various extracts of the said plant.

  15. 1H-MRSI of prostate cancer: The relationship between metabolite ratio and tumor proliferation

    Energy Technology Data Exchange (ETDEWEB)

    Wang Xizhen [Shandong Medical Imaging Research Institute, Shandong University, 324 JingWu Road, Jinan 250021 (China) and Department of Radiology, Medical Imaging Center of the Affiliated Hospital, Weifang Medical University, 288 Shengli East Street, Weifang 261042 (China)], E-mail: zhen94320@yahoo.com.cn; Wang Bin [Department of Radiology, Medical Imaging Center of the Affiliated Hospital, Weifang Medical University, 288 Shengli East Street, Weifang 261042 (China)], E-mail: binwang001@yahoo.com.cn; Gao Zhiqin [Department of Medical Biology, Weifang Medical University, 288 Shengli East Street, Weifang 261042 (China)], E-mail: zhiqin_gao@yahoo.com.cn; Liu Jingang [Department of Radiology, Medical Imaging Center of the Affiliated Hospital, Weifang Medical University, 288 Shengli East Street, Weifang 261042 (China)], E-mail: liujingang77@163.com; Liu Zuoqin [Shandong Medical Imaging Research Institute, Shandong University, 324 JingWu Road, Jinan 250021 (China)], E-mail: liuzuoqin666@yahoo.com.cn; Niu Qingliang [Department of MRI/CT, Weifang Traditional Chinese Medicine Hospital, Weifang 261041 (China)], E-mail: qingliangniu@yahoo.com.cn; Sun Zhenkui [Department of Radiology, Medical Imaging Center of the Affiliated Hospital, Weifang Medical University, 288 Shengli East Street, Weifang 261042 (China)], E-mail: sun77126@163.com; Yuan Yuxiao [Department of Radiology, Medical Imaging Center of the Affiliated Hospital, Weifang Medical University, 288 Shengli East Street, Weifang 261042 (China)], E-mail: realyyx@eyou.com

    2010-02-15

    Purpose: To investigate whether 1H-MRSI can be used to predict the proliferative activity of prostate cancer. Materials and methods: Thirty-eight patients with prostate cancer (PCa) and thirty-three patients with benign prostate hyperplasia (BPH) were included in this study. Patients were examined in supine position using a 1.5 T superconducting magnetic scanner equipped with a pelvic phased-array multi-coil and CSI-3D-PROSTATE sequence. Commercial software was used to acquire and process MR spectroscopic imaging data. Mean (Cho + Cr)/Cit ratios of PCa, BPH, and peripheral zone (PZ) were calculated. Cellularity of PCa was recorded based on hematoxylin and eosin staining. PCNA was detected using immunohistochemical techniques. Results: The mean (Cho + Cr)/Cit ratio of the peripheral zone (0.38 {+-} 0.09) was lower than that of BPH (0.51 {+-} 0.19) (P < 0.05). The average value of (Cho + Cr)/Cit ratio of prostate cancer was 3.98 {+-} 0.12. The (Cho + Cr)/Cit ratio of prostate cancer was higher than that of the peripheral zone and BPH (P < 0.05). The cellularity and PCNA LI of prostate cancer were 12.90 {+-} 4.07% and 72.1 {+-} 19.01%, respectively. The (Cho + Cr)/Cit ratio of prostate cancer positively correlated with tumor cellularity (r = 0.582, P = 0.027) and PCNA LI (r = 0.495, P = 0.022). Conclusion: The (Cho + Cr)/Cit ratio of PCa can reveal the differences in proliferative activity between PCa and BPH. MRSIs are therefore able to predict the proliferative rate of variously differentiated prostate cancers.

  16. 1H MR Spectroscopy in Friedreich's Ataxia and Ataxia with Oculomotor Apraxia Type 2

    Science.gov (United States)

    Iltis, Isabelle; Hutter, Diane; Bushara, Khalaf O.; Clark, H. Brent; Gross, Myron; Eberly, Lynn E.; Gomez, Christopher M.; Öz, Gülin

    2010-01-01

    Background and aim Friedreich's ataxia (FRDA) and ataxia with oculomotor apraxia type 2 (AOA2) are the two most frequent forms of autosomal recessive cerebellar ataxias. However, brain metabolism in these disorders is poorly characterized and biomarkers of the disease progression are lacking. We aimed at assessing the neurochemical profile of the pons, the cerebellar hemisphere and the vermis in patients with FRDA and AOA2 to identify potential biomarkers of these diseases. Methods Short-echo, single voxel proton (1H) magnetic resonance spectroscopy data were acquired from 8 volunteers with FRDA, 9 volunteers with AOA2, and 38 control volunteers at 4T. Disease severity was assessed by the Friedreich's Ataxia Rating Scale (FARS). Results Neuronal loss/dysfunction was indicated in the cerebellar vermis and hemispheres in both diseases by lower total N-acetylaspartate levels than controls. The putative gliosis marker myo-inositol was higher than controls in the vermis and pons in AOA2 and in the vermis in FRDA. Total creatine, another potential gliosis marker, was higher in the cerebellar hemispheres in FRDA relative to controls. Higher glutamine in FRDA and lower glutamate in AOA2 than controls were observed in the vermis, indicating different mechanisms possibly leading to altered glutamatergic neurotransmission. In AOA2, total N-acetylaspartate levels in the cerebellum strongly correlated with the FARS score (p < 0.01). Conclusion Distinct neurochemical patterns were observed in the two patient populations, warranting further studies with larger patient populations to determine if the alterations in metabolite levels observed here may be utilized to monitor disease progression and treatment. PMID:20713024

  17. {sup 1}H and {sup 31}P-magnetic resonance spectroscopy of cerebral infarction in rats

    Energy Technology Data Exchange (ETDEWEB)

    Yamamuro, Manabu; Katayama, Yasuo; Igarashi, Hironaka; Terashi, Akiro [Nippon Medical School, Tokyo (Japan)

    1997-04-01

    Magnetic resonance spectroscopy (MRS) allows the noninvasive study of metabolism in vivo. In order to further understand the time course of biochemical changes during cerebral infarction, we performed the MRS study with pathological analysis. The left middle cerebral artery (MCA) was occluded in spontaneously hypertensive male rats (SHR) by the method of Tamura et al. The spectra were obtained from the infarcted hemisphere by placing the surface coils over the left side of the calvarium. {sup 31}P and {sup 1}H-MRS were performed at 3 hours, 24 hours and 7 days after MCA occlusion. Ischemic lesions caused by the left MCA occlusion extended into the parietal lobe and caudate putamen. After 3 hours of ischemia, vacuolated neurophils and shrunken neurons were observed. At 24 hours, these changes were severe. After 7 days, infiltration of monocytes and capillary hyperplasia were seen, and neurons had disappeared. At the acute stage of ischemia the phosphocreatine/inorganic phosphate (PCr/Pi) peak ratio decreased. After 7 days of ischemia, these changes became obscure. The intracellular pH (pHi) decreased after 3 hours of ischemia and recovered almost to the control level at 24 hours post ischemia. Alkalosis was apparent 7 days after ischemia. This alkalosis might be due to increased permeability of the deteriorated blood brain barrier. Although the lactate level was high 24 hours post ischemia, the pHi was almost normal. The N-acetyl-aspartate/creatine ratio decreased significantly from the acute stage of stroke. This decrease correlated with pathological changes. The correlation of the magnetic resonance spectra with the histological results may open aspects for monitoring stroke therapy and a new approach to tissue characterization. (author)

  18. 1H NMR- based metabolomics approaches as non- invasive tools for diagnosis of endometriosis

    Directory of Open Access Journals (Sweden)

    Negar Ghazi

    2016-01-01

    Full Text Available Background: So far, non-invasive diagnostic approaches such as ultrasound, magnetic resonance imaging, or blood tests do not have sufficient diagnostic power for endometriosis disease. Lack of a non-invasive diagnostic test contributes to the long delay between onset of symptoms and diagnosis of endometriosis. Objective: The present study focuses on the identification of predictive biomarkers in serum by pattern recognition techniques and uses partial least square discriminant analysis, multi-layer feed forward artificial neural networks (ANNs and quadratic discriminant analysis (QDA modeling tools for the early diagnosis of endometriosis in a minimally invasive manner by 1H- NMR based metabolomics. Materials and Methods: This prospective cohort study was done in Pasteur Institute, Iran in June 2013. Serum samples of 31 infertile women with endometriosis (stage II and III who confirmed by diagnostic laparoscopy and 15 normal women were collected and analyzed by nuclear magnetic resonance spectroscopy. The model was built by using partial least square discriminant analysis, QDA, and ANNs to determine classifier metabolites for early prediction risk of disease. Results: The levels of 2- methoxyestron, 2-methoxy estradiol, dehydroepiandrostion androstendione, aldosterone, and deoxy corticosterone were enhanced significantly in infertile group. While cholesterol and primary bile acids levels were decreased. QDA model showed significant difference between two study groups. Positive and negative predict value levels obtained about 71% and 78%, respectively. ANNs provided also criteria for detection of endometriosis. Conclusion: The QDA and ANNs modeling can be used as computational tools in noninvasive diagnose of endometriosis. However, the model designed by QDA methods is more efficient compared to ANNs in diagnosis of endometriosis patients.

  19. Synthesis, structure, photoluminescence and antitumour activity of zinc complex based on 2-(2-(1H-benzo-[d]imidazol-2-yl)benzyl)-1H-benzo-[d]imidazole

    Science.gov (United States)

    Che, Zhijian; Wang, Shaoxiang; Liu, Shenggui; Li, Guobi; Wu, Qiting; Lin, Chunyu; Kong, Linglang; Wang, Sheng

    2015-01-01

    A new complex [Zn(bbb)Cl2]·DMF, where bbb is 2-(2-(1H-benzo[d]imidazol-2-yl)benzyl)-1H-benzo[d]imidazole, was synthesized and characterized by element analysis, 1H NMR and X-ray single crystal structure analyses. For complex: crystal system, triclinic, space group, P-1, a = 9.4661(13), b = 10.3534(14), c = 13.0025(18) Å, α = 73.477(2), β = 80.743(2), γ = 88.658(2)°, V = 1205.5(3) Å3, Z = 2. In this complex, the Zn2+ distorted tetrahedron geometry is coordinated by two nitrogen atoms from 2-(2-(1H-benzo[d]imidazol-2-yl)benzyl)-1H-benzo[d]imidazole and two Cl-. The complex emits yellow green luminescence with the maximal emission peak at 550 nm in DMF solution. The complex exhibits inhibition on the growth of Eca109 cancer cell with IC50 value of 8.9 ± 1.1 μM, which was lower than that of cisplatin (14.3 ± 1.4 μM). This complex has potential application in treatment of esophageal cancer.

  20. Synthesis and Biological Activity of 2-(Thiazolidin-4-One Phenyl]-1h-Phenylbenzimidazoles and 2-[4-(Azetidin-2-One-3-Chloro-4- Phenyl] -1h-Phenyl Benzimidazoles

    Directory of Open Access Journals (Sweden)

    P. Shanmugapandiyan

    2010-04-01

    Full Text Available A new series of 2-[4-(azetidin-2-one-3-Chloro-4-phenyl]-1H-Phenylbenzimidazoles and 2-(thiazolidin-4-one-Phenyl]-1H-Phenylbenzimidazoles were synthesized by the reaction of schiff base [2-(4-aminophenyl-Benzimidazole and substituted Benzaldehyde] with chloroacetyl chloride and mercaptoacetic acid respectively. The chemical structures of the synthesized compounds were confirmed by IR, 1H-NMR, mass spectral and C, H, N analysis. The synthesized compounds were screened for antibacterial (Bacillus cereus, Escherichia coli, Micrococcus luteus, Klebssiela pneumoniae, Staphylococcus aureus and Salmonella epidermidis, antifungal (Aspergillus niger and Candida albicans, analgesic activity by writhing reflex method and anti-inflammatory activity by carrageenan induced paw edema method. The synthesized compound showed significant activity of antibacterial, antifungal, analgesic and anti-inflammatory activity comparable to that of standard.

  1. Synthesis, characterization, antimicrobial, DNA-cleavage and antioxidant activities of 3-((5-chloro-2-phenyl-1H-indol-3-ylimino)methyl)quinoline-2(1H)-thione and its metal complexes

    Science.gov (United States)

    Vivekanand, B.; Mahendra Raj, K.; Mruthyunjayaswamy, B. H. M.

    2015-01-01

    Schiff base 3-((5-chloro-2-phenyl-1H-indol-3-ylimino)methyl)quinoline-2(1H)-thione and its Cu(II), Co(II), Ni(II), Zn(II) and Fe(III), complexes have been synthesized and characterized by elemental analysis, UV-Visible, IR, 1H NMR, 13C NMR and mass spectra, molar conductance, magnetic susceptibility, ESR and TGA data. The ligand and its metal complexes have been screened for their antibacterial activity against Staphylococcus aureus and Pseudomonas aeruginosa, antifungal activity against Aspergillus niger and Aspergillus flavus in minimum inhibition concentration (MIC) by cup plate method respectively, antioxidant activity using 1,1-diphenyl-2-picryl hydrazyl (DPPH), which was compared with that of standard drugs vitamin-C and vitamin-E and DNA cleavage activity using calf-thymus DNA.

  2. Design, synthesis and anti-tobacco mosaic virus (TMV) activity of 5-chloro-N-(4-cyano-1-aryl-1H-pyrazol-5-yl)-1-aryl-3-methyl-1H-pyrazole-4-carboxamide derivatives.

    Science.gov (United States)

    Xiao, Jin-Jing; Liao, Min; Chu, Ming-Jie; Ren, Zi-Li; Zhang, Xin; Lv, Xian-Hai; Cao, Hai-Qun

    2015-01-07

    A series of novel pyrazole amide derivatives 3a-3p which take TMV PC protein as the target has been designed and synthesized by the reactions of 5-chloro-1-aryl-3-methyl-1H-pyrazole-4-carboxylic acids with 5-amino-1-aryl-1H-pyrazole-4-carbonitriles. All the compounds were characterized by 1H-NMR, mass spectroscopy and elemental analysis. Preliminary bioassays indicated that all the compounds acted against the tobacco mosaic virus (TMV) with different in vivo and in vitro modes at 500 μg/mL and were found to possess promising activity. Especially, compound 3p showed the most potent biological activity against tobacco mosaic virus (TMV) compared to ningnanmycin, and a molecular docking study was performed and the binding model revealed that the pyrazole amide moiety was tightly embedded in the binding sites of TMV PC (PDB code: 2OM3).

  3. 联合应用ESI MS和1H NMR分析含笑属植物种子磷脂%Application of ESI-MS combined with 1 H NMR in analyzing seed phospolipids of six species of Michelia

    Institute of Scientific and Technical Information of China (English)

    唐安军; Naomichi BAbA

    2012-01-01

    To date,there was no example to authenticate seed phospholipids based on their fingerprinting.By means of electrospray ionization mass spectrometry(ESI MS)and proton nuclear magnetic resonance(1 H NMR)spectroscopy,phospholipids fraction extracted from seeds of six species from the genus Michelia were detected.It was firstly found that distinct difference in spectral fingerprinting region between m/z 895-910 in ESI MS and 5.30-5.40 mg/L in 1 H NMR among these six species.Thus,it suggested that the spectral differences shown by ESI MS and 1 H NMR among seeds of these six species could be applied to identify them.And in a wider sense,for analyzing seed phospholipids of other plant species,a combination of ESI MS AND NMR was an effective tool.%首次尝试利用电喷雾电离质谱(ESI MS)和氢原子核磁共振(1 H NMR)技术分析了含笑属六种植物种子的磷脂特性,发现在两个指纹图谱区发现明显的差异,即在质荷比(m/z)895-910(ESI MS)和5.30~5.40mg/L(1 H NMR)两个特异的区域存在显著差异.这些源于种子磷脂ESI/MS和1 H NMR的谱带差异可以被用来分析不同植物的种子的磷脂特征.而且,相似地,在更广的层面上,特异性的谱带差异可用于分析其他植物种子的磷脂组成和特性,辅助鉴定种子.

  4. Constant time INEPT CT-HSQC (CTi-CT-HSQC) - A new NMR method to measure accurate one-bond J and RDCs with strong 1H-1H couplings in natural abundance.

    Science.gov (United States)

    Yu, Bingwu; van Ingen, Hugo; Freedberg, Darón I

    2013-03-01

    Strong (1)H-(1)H coupling can significantly reduce the accuracy of (1)J(CH) measured from frequency differences in coupled HSQC spectra. Although accurate (1)J(CH) values can be extracted from spectral simulation, it would be more convenient if the same accurate (1)J(CH) values can be obtained experimentally. Furthermore, simulations reach their limit for residual dipolar coupling (RDC) measurement, as many significant, but immeasurable RDCs are introduced into the spin system when a molecule is weakly aligned, thus it is impossible to have a model spin system that truly represents the real spin system. Here we report a new J modulated method, constant-time INEPT CT-HSQC (CTi-CT-HSQC), to accurately measure one-bond scalar coupling constant and RDCs without strong coupling interference. In this method, changing the spacing between the two 180° pulses during a constant time INEPT period selectively modulates heteronuclear coupling in quantitative J fashion. Since the INEPT delays for measuring one-bond carbon-proton spectra are short compared to (3)J(HH), evolution due to (strong) (1)H-(1)H coupling is marginal. The resulting curve shape is practically independent of (1)H-(1)H coupling and only correlated to the heteronuclear coupling evolution. Consequently, an accurate (1)J(CH) can be measured even in the presence of strong coupling. We tested this method on N-acetyl-glucosamine and mannose whose apparent isotropic (1)J(CH) values are significantly affected by strong coupling with other methods. Agreement to within 0.5Hz or better is found between (1)J(CH) measured by this method and previously published simulation data. We further examined the strong coupling effects on RDC measurements and observed an error up to 100% for one bond RDCs using coupled HSQC in carbohydrates. We demonstrate that RDCs can be obtained with higher accuracy by CTi-CT-HSQC, which compensates the limitation of simulation method.

  5. Metabolic profile of normal glucose-tolerant subjects with elevated 1-h plasma glucose values

    Science.gov (United States)

    Pramodkumar, Thyparambil Aravindakshan; Priya, Miranda; Jebarani, Saravanan; Anjana, Ranjit Mohan; Mohan, Viswanathan; Pradeepa, Rajendra

    2016-01-01

    Aim: The aim of this study was to compare the metabolic profiles of subjects with normal glucose tolerance (NGT) with and without elevated 1-h postglucose (1HrPG) values during an oral glucose tolerance test (OGTT). Methodology: The study group comprised 996 subjects without known diabetes seen at tertiary diabetes center between 2010 and 2014. NGT was defined as fasting plasma glucose <100 mg/dl (5.5 mmol/L) and 2-h plasma glucose <140 mg/dl (7.8 mmol/L) after an 82.5 g oral glucose (equivalent to 75 g of anhydrous glucose) OGTT. Anthropometric measurements and biochemical investigations were done using standardized methods. The prevalence rate of generalized and central obesity, hypertension, dyslipidemia, and metabolic syndrome (MS) was determined among the NGT subjects stratified based on their 1HrPG values as <143 mg/dl, ≥143–<155 mg/dl, and ≥155 mg/dl, after adjusting for age, sex, body mass index (BMI), waist circumference, alcohol consumption, smoking, and family history of diabetes. Results: The mean age of the 996 NGT subjects was 48 ± 12 years and 53.5% were male. The mean glycated hemoglobin for subjects with 1HrPG <143 mg/dl was 5.5%, for those with 1HrPG ≥143–<155 mg/dl, 5.6% and for those with 1HrPG ≥155 mg/dl, 5.7%. NGT subjects with 1HrPG ≥143–<155 mg/dl and ≥155 mg/dl had significantly higher BMI, waist circumference, systolic and diastolic blood pressure, triglyceride, total cholesterol/high-density lipoprotein (HDL) ratio, triglyceride/HDL ratio, leukocyte count, and gamma glutamyl aminotransferase (P < 0.05) compared to subjects with 1HrPG <143 mg/dl. The odds ratio for MS for subjects with 1HrPG ≥143 mg/dl was 1.84 times higher compared to subjects with 1HrPG <143 mg/dl taken as the reference. Conclusion: NGT subjects with elevated 1HrPG values have a worse metabolic profile than those with normal 1HrPG during an OGTT. PMID:27730069

  6. 1H 1752 + 081: an eclipsing cataclysmic variable with a small accretion disk

    Science.gov (United States)

    Silber, Andrew D.; Remillard, Ronald A.; Horne, Keith; Bradt, Hale V.

    1994-04-01

    We announce the discovery of an eclipsing nova-like cataclysmic variable (CV) as the optical counterpart to the HEAO 1 X-ray source 1H1752 + 081. This CV has an orbital period of 1.882801 hr, a high equivalent width of H-beta, and an average mv of 16.4 out of the eclipse. A geometric model is constructed from observations of the eclipse ingress and egress in many optical bandpasses. The broad-band emission originates primarily in two regions; the disk/accretion stream 'hot spot' and a compact central component, which may be a spot on the white dwarf surface, the entire white dwarf surface or the boundary layer between the accretion disk and the white dwarf surface. Based on the durations and offsets of the two eclipses we determined the mass ratio q = 2.5 +/- 0.6 and the angle of inclination i = 77 deg +/- 2 deg. If the central component is the entire white dwarf surface the masses of the stars are M1 = 0.80 +/- 0.06 solar masses and M2 = 0.32 +/- 0.06 solar masses. The disk is faint and small (RD = 0.25 +/- 0.05 rL1, where rL1 is the distance from the primary to the L1 point), compared to other eclipsing CVs. The small disk may result from the removal of angular momentum from the accretion disk by the magnetic field of the white dwarf; this CV may be a DQ Her type with a slowly rotating white dwarf. The emission-line velocities do not show the 'Z-wave' expected from the eclipse of a Keplerian accretion disk, nor do they have the correct phasing to originate near the white dwarf. The most likely origin of the line emission is the hot spot. The secondary star is visible at wavelengths greater than or equal to 6000 A during eclipse. We estimate a spectral type approximately M6 which, together with the observed m1 = 16.94 during eclipse, results in a distance estimate of 150 +/- 27 pc.

  7. (1)H NMR Relaxation Study of a Magnetic Ionic Liquid as a Potential Contrast Agent.

    Science.gov (United States)

    Daniel, Carla I; Vaca Chávez, Fabián; Portugal, Carla A M; Crespo, João G; Sebastião, Pedro J

    2015-09-03

    A proton nuclear magnetic relaxation dispersion (1)H NMRD study of the molecular dynamics in mixtures of magnetic ionic liquid [P66614][FeCl4] with [P66614][Cl] ionic liquid and mixtures of [P66614][FeCl4] with dimethyl sulfoxide (DMSO) is presented. The proton spin-lattice relaxation rate, R1, was measured in the frequency range of 8 kHz-300 MHz. The viscosity of the binary mixtures was measured as a function of an applied magnetic field, B, in the range of 0-2 T. In the case of DMSO/[P66614][FeCl4] the viscosity was found to be independent from the magnetic field, while in the case of the [P66614][Cl]/[P66614][FeCl4] system viscosity decreased with the increase of the magnetic field strength. The spin-lattice relaxation results were analyzed for all systems taking into account the relaxation mechanisms associated with the molecular motions with correlation times in a range between 10(-11) and 10(-7)s, usually observed by NMRD, and the paramagnetic relaxation contributions associated with the presence of the magnetic ions in the systems. In the case of the DMSO/[P66614][FeCl4] system the R1 dispersion shows the relaxation enhancement due to the presence of the magnetic ions, similar to that reported for contrast agents. For the [P66614][Cl]/[P66614][FeCl4] system, the R1 dispersion presents a much larger paramagnetic relaxation contribution, in comparison with that observed for the DMSO/[P66614][FeCl4] mixtures but different from that reported for other magnetic ionic liquid system. In the [P66614][Cl]/[P66614][FeCl4] system the relaxation enhancement associated with the paramagnetic ions is clearly not proportional to the concentration of magnetic ions, in contrast with what is observed for the DMSO/[P66614][FeCl4] system.

  8. A multicenter reproducibility study of single-voxel {sup 1}H-MRS of the medial temporal lobe

    Energy Technology Data Exchange (ETDEWEB)

    Traeber, Frank; Block, Wolfgang; Guer, Okan; Schild, Hans H. [University of Bonn, Department of Radiology, Bonn (Germany); Freymann, Nikolaus; Heun, Reinhard; Jessen, Frank [University of Bonn, Department of Psychiatry, Bonn (Germany); Kucinski, Thomas [University of Hamburg, Department of Neuroradiology, Hamburg (Germany); Hammen, Thilo [University of Erlangen, Department of Psychiatry, Erlangen (Germany); Ende, Gabriele [Central Institute of Mental Health, NMR Research in Psychiatry, Mannheim (Germany); Pilatus, Ulrich [University of Frankfurt, Department of Neuroradiology, Frankfurt (Germany); Hampel, Harald [University of Munich, Department of Psychiatry, Munich (Germany)

    2006-05-15

    Proton magnetic resonance spectroscopy ({sup 1}H-MRS) has provided evidence for a reduction of N-acetyl-aspartate (NAA) in the medial temporal lobe (MTL) in cerebral disorders such as Alzheimer's Disease. Within the {sup 1}H-MRS study of the German Research Network on Dementia, we determined the multicenter reproducibility of single-voxel {sup 1}H-MRS of the MTL. At five sites with 1.5T MR systems, single-voxel {sup 1}H spectra from the MTL of an identical healthy subject were measured. The same subject was also examined at one of the sites five times to assess intracenter stability. The protocol included water-suppressed spectra with TE 272 ms and TE 30 ms and unsuppressed spectra for absolute quantification of metabolite concentrations. The intracenter reproducibility of absolute NAA concentration, expressed as coefficient of variation (CV), was 1.8%. CV for the concentrations of creatine (Cr), choline (Cho), and myoinositol (MI) and for the ratios NAA/Cr, NAA/Cho, and MI/NAA varied by 11-16%. Intercenter CV was 3.9% for NAA and were below 10% for all other metabolites and metabolic ratios. Our study demonstrates that quantitative assessment of NAA with single-voxel MRS can be performed with high intercenter reproducibility. This is the basis for applying {sup 1}H-MRS in large-scale early recognition and treatment studies in MTL affecting disorders. (orig.)

  9. Analysis of amorphous solid dispersions using 2D solid-state NMR and (1)H T(1) relaxation measurements.

    Science.gov (United States)

    Pham, Tran N; Watson, Simon A; Edwards, Andrew J; Chavda, Manisha; Clawson, Jacalyn S; Strohmeier, Mark; Vogt, Frederick G

    2010-10-04

    Solid-state NMR (SSNMR) can provide detailed structural information about amorphous solid dispersions of pharmaceutical small molecules. In this study, the ability of SSNMR experiments based on dipolar correlation, spin diffusion, and relaxation measurements to characterize the structure of solid dispersions is explored. Observation of spin diffusion effects using the 2D (1)H-(13)C cross-polarization heteronuclear correlation (CP-HETCOR) experiment is shown to be a useful probe of association between the amorphous drug and polymer that is capable of directly proving glass solution formation. Dispersions of acetaminophen and indomethacin in different polymers are examined using this approach, as well as (1)H double-quantum correlation experiments to probe additional structural features. (1)H-(19)F CP-HETCOR serves a similar role for fluorinated drug molecules such as diflunisal in dispersions, providing a rapid means to prove the formation of a glass solution. Phase separation is detected using (13)C, (19)F, and (23)Na-detected (1)H T(1) experiments in crystalline and amorphous solid dispersions that contain small domains. (1)H T(1) measurements of amorphous nanosuspensions of trehalose and dextran illustrate the ability of SSNMR to detect domain size effects in dispersions that are not glass solutions via spin diffusion effects. Two previously unreported amorphous solid dispersions involving up to three components and containing voriconazole and telithromycin are analyzed using these experiments to demonstrate the general applicability of the approach.

  10. Quantitative {sup 1}H MR spectroscopy of the brain in patients with congestive heart failure before and after cardiac transplantation

    Energy Technology Data Exchange (ETDEWEB)

    Lim, Soo Mee; Lee, Ho Kyu; Choi, Choong Gon; Lim, Tae Hwan [Asan Medical Center, Ulsan Univ. College of Medicine, Ulsan (Korea, Republic of); Lee, Jung Hee [Asan Institute for Life Sciences, Seoul (Korea, Republic of)

    1999-12-01

    To evaluate the effects of cardiac transplantation on the brain in patients with congestive heart failure (CHF), using quantitative {sup 1}H MR spectroscopy ({sup 1}H-MRS). Ten patients with CHF underwent MRI and quantitative {sup 1}H-MRS before and 1-2 and 4-9 months after cardiac transplantation. MR spectra were obtained from parietal white matter (PWM) and occipital gray matter (OGM) using PROBE (PROton Brain Exam). Changes in MR signal intensity were evaluated, and the cerebral metabolic concentrations in PWM and OGM were compared. For comparative purposes, 20 normal volunteers were included. No abnormal MR signal intensity was seen in the brain before or after cardiac transplantation. Changes in cerebral metabolic concentrations were observed on {sup 1}H-MRS; concentrations of creatine (Cr) in PWM, and of N-acetylacepartate (NAA), Cr and myo-Inositol(mI) in OGM were significantly lower before transplantation. After successful transplantation, Cr levels returned to their normal range in PWM and OGM, while a slightly increase choline (Cho) level was observed in PWM. Cerebral hypoperfusion in CHF can be evaluated using {sup 1}H-MRS. MRS may play a substantial role in monitoring the effect of cardiac transplantation.

  11. A disk wind interpretation of the strong Fe K{\\alpha} features in 1H 0707-495

    CERN Document Server

    Hagino, Kouichi; Done, Chris; Tomaru, Ryota; Watanabe, Shin; Takahashi, Tadayuki

    2015-01-01

    1H 0707-495 is the most convincing example of a supermassive black hole with an X-ray spectrum being dominated by extremely smeared, relativistic reflection. However, here we show that the iron features in its 2--10 keV spectrum are rather similar to the archetypal wind dominated source, PDS 456. We fit all the 2--10 keV spectra from 1H 0707-495 using the same wind model as used for PDS 456, but viewed at higher inclination so that the iron absorption line is broader but not so blueshifted. This gives a good overall fit to the data from 1H 0707-495, and an extrapolation of this model to higher energies also gives a good match to the NuSTAR data. Small remaining residuals may indicate that the emission from the wind is stronger than in PDS 456, consistent with the wider angle wind expected from a continuum driven wind from the super-Eddington mass accretion rate in 1H 0707-495. We suggest that the spectrum of 1H 0707-495 is sculpted more by absorption in a wind than by extreme relativistic effects in strong gr...

  12. Sequence Characterization of matrix protein (M1 in influenza A viruses (H1, H3 and H5

    Directory of Open Access Journals (Sweden)

    Jun Zhang

    2011-10-01

    Full Text Available This study brings the analysis of amino acid sequences of matrix protein (M1 from the influenza virus A (H1N1, H3N2 and H5N1 during 2007-2208. 741 sequences of M1 were compared, of them, H1N1 388; H3N2 251 and H5N1 102. Even though, the M1 is relatively conserved among the influenza A viruses, we found some variations in the M1 among the viruses, H1N1, H3N2 and H5N1. The nuclear localization signal at amino acid 101 to 105 is RKLKR for H1N1 and H3N2, but for H5N1 is KKLKR. All differences of amino acid in M1 of H1, H3 and H5 were listed. 80 sequences of M1 of H1N1 H3N2 and H5N1 were used for phylogenetic analysis. There is no reasontantment found in the M1 among these subtypes. Further study is needed to study the differences of the function of M1 among H1N1, H3N2 and H5N1. The M1 of H5N1 may contribute to the high pathogenesis to this virus.

  13. Studies on Lignin Structure of Wheat Straw by 1H-13C 2-D NMR Spectroscopy%1H-13C 2-D NMR光谱技术在麦草木素结构研究中的应用

    Institute of Scientific and Technical Information of China (English)

    葛培锦; 曲音波; 赵建

    2006-01-01

    对麦草二氧六环木素分别进行了1H-NMR、13C-NMR和2D-HMQC NMR光谱分析.研究结果表明:二维2D-HMQC NMR光谱技术可较好揭示麦草木素的结构特征,克服1H-NMR和 13C-NMR光谱的吸收峰重叠以及多糖的干扰问题.

  14. Parallel Solid-Phase Synthesis of disubstituted 3-(1H-benzo[d]imidazol-2-yl)imidazolidine-2,4-diones and 3-(1H-benzo[d]imidazol-2-yl)-2-thioxoimidazolidin-4-ones.

    Science.gov (United States)

    Dadiboyena, Sureshbabu; Nefzi, Adel

    2011-12-28

    A multistep approach to construct novel 3-(1H-benzo[d]imidazol-2-yl)imidazolidine-2,4-diones and 3-(1H-benzo[d]imidazol-2-yl)-2-thioxoimidazolidin-4-ones from commercially available amino acids, amines, and carboxylic acids is described. Coupling of Fmoc-amino acid to resin-bound aminobenzimidazole provided following Fmoc elimination free amine. Treatment of the free amine with 1,1'-carbonyldiimidazole or 1,1'-thiocarbonyldiimidazole furnished the corresponding hydantoins and thiohydantoins via intramolecular cyclization. The desired aminobenzimidazole tethered hydantoin or thiohydantoins were isolated in good yields.

  15. Synthesis of 1H-benzoxazine-2,4-diones from heterocyclic anhydrides: evaluation of antioxidant and antimicrobial activities

    Directory of Open Access Journals (Sweden)

    Juan I. Sarmiento-Sánchez

    2014-01-01

    Full Text Available A facile one-step synthesis of 1H-benzoxazine-2,4-diones from heterocyclic anhydrides and TMSA was described. This paper determines their antimicrobial activity against nine human bacterial pathogens by the broth microdilution method; antioxidant activity by DPPH• inactivation and a ferric-reducing power assay; and toxicity by a brine shrimp, Artemia salina, assay. The 1H-benzoxazine-2,4-dione yields were in the range of 57 to 98%. The novel compound 1H-pyrazino[2,3-][1,3]oxazine-2,4-dione 4c showed the highest antioxidant capacity (DPPH 35.4% and FRAP 0.063 µmol TEs/µmol.

  16. Fatty acids profile of Sacha Inchi oil and blends by 1H NMR and GC-FID.

    Science.gov (United States)

    Vicente, Juarez; de Carvalho, Mario Geraldo; Garcia-Rojas, Edwin E

    2015-08-15

    This study aimed at the characterization of blends of Sacha Inchi oil (SIO) with different ratios of SO (soybean oil) and CO (corn oil) by nuclear magnetic resonance ((1)H NMR), compared with the data obtained by gas chromatography with a flame ionization detector (GC-FID). The (1)H NMR and GC-FID data from different ratios of SIO were adjusted by a second order polynomial equation. The two techniques were highly correlated (R(2) values ranged from 0.995 to 0.999), revealing that (1)H NMR is an efficient methodology for the quantification of omega-3 fatty acids in oils rich in omega-6 fatty acids or vice versa such as SO and CO and, on the other hand, can be used to quantify ω-6 in oils rich in ω-3, such as SIO.

  17. The application of "click chemistry" for the decoration of 2(1H)-pyrazinone scaffold: generation of templates.

    Science.gov (United States)

    Kaval, Nadya; Ermolat'ev, Denis; Appukkuttan, Prasad; Dehaen, Wim; Kappe, C Oliver; Van der Eycken, Erik

    2005-01-01

    The "click chemistry" approach has been explored on the 2-(1H)-pyrazinone scaffold for the generation of pharmacologically interesting heterocyclic moieties. Huisgen 1,3-dipolar cycloaddition has been evaluated as the key step for the construction of the 1,2,3-triazole ring at the C-3 position of 2-(1H)-pyrazinones. Two different pathways have been successfully evaluated: (1) via C-C or C-O linkage of the acetylenic part to the C-3 position of the 2-(1H)-pyrazinone scaffold or (2) via azide introduction in the C-3 position. The subsequent application of "click chemistry" resulted in the formation of hitherto unknown skeletons. Microwave irradiation has successfully been applied in different steps of the sequence.

  18. Application of 1H NMR for the characterisation of cocoa beans of different geographical origins and fermentation levels.

    Science.gov (United States)

    Caligiani, Augusta; Palla, Luigi; Acquotti, Domenico; Marseglia, Angela; Palla, Gerardo

    2014-08-15

    This study reports for the first time the use of (1)H NMR technique combined with chemometrics to study the metabolic profile of cocoa (Theobroma cacao L.) beans of different varieties, origin and fermentation levels. Results of PCA applied to cocoa bean (1)H NMR dataset showed that the main factor influencing the cocoa bean metabolic profile is the fermentation level. In fact well fermented brown beans form a group clearly separated from unfermented, slaty, and underfermented, violet, beans, independently of the variety or geographical origin. Considering only well fermented beans, the metabolic profile obtained by (1)H NMR permitted to discriminate between some classes of samples. The National cocoa of Ecuador, known as Arriba, showed the most peculiar characteristics, while the samples coming from the African region showed some similar traits. The dataset obtained, representative of all the classes of soluble compounds of cocoa, was therefore useful to characterise fermented cocoa beans as a function of their origin and fermentation level.

  19. Synthesis and Crystal Structure of N'-(4-fluorobenzylidene)-2-(1H-1,2,4-triazole-1-yl) acetohydrazide

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    N'-(4-fluorobenzylidene)-2-(1H-1,2,4-triazole-1-yl)acetohydrazide was synthesized by the reaction of 4-fluorobenzaldehyde with 2-(1H-1,2,4-triazole-1-yl) acetohydrazide. The structure was confirmed via elemental analysis, MS,1H NMR, IR, and X-ray diffraction. It crystallized in a monoclinic system with space group P2 ( 1 ), a =0.4905(1) nm, b=0.8160(2) nm, c=1.4105(3) nm,β=93.33(3)°,Z=2, V=0.5636(2) nm3, Dc =1.457 Mg/m3,μ=0.112 mm-1 , F(000) =256, and final R1 =0. 0685. Several intermolecular hydrogen-bond interactions existed in the crystal structure, facilitating the stabilization of the compound.

  20. E2FBP1/hDril1 modulates cell growth through downregulation of promyelocytic leukemia bodies.

    Science.gov (United States)

    Fukuyo, Y; Mogi, K; Tsunematsu, Y; Nakajima, T

    2004-07-01

    Promyelocytic leukemia nuclear bodies (PML-NBs) comprise multiple regulatory factors and play crucial roles in the maintenance of cellular integrity, while unregulated activation of PML-NBs induces death and premature senescence. Hence, the function of PML-NBs must be directed properly; however, the mechanism that regulates PML-NBs remains unclear. In this paper, we show that PML-NBs are disintegrated by an AT-rich interaction domain family protein E2FBP1/hDril1 through specific desumoylation of promyelocytic leukemia protein (PML) in vivo and in vitro. RNA interference-mediated downregulation of E2FBP1/hDril1 results in hyperplasis of PML-NBs and consequent commitment to PML-dependent premature senescence. Thus, the function of E2FBP1/hDril1 is required for maintenance of survival potential of the cells. Our data suggest a novel mechanism to govern cellular integrity through the modulation of nuclear depots.