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Sample records for 1h 31p 77se

  1. Noninvasive assessment of spontaneous cardiomyopathy of syrian hamster by 1H- and 31P-TMR

    Sequential changes in 1H-NMR (180 MHz) and 31P-NMR (32 MHz) were examined by simultaneously measuring them from the juvenile stage (72 days after birth) to the time of occurrence of cardiomyopathy (155 days after birth) with Syrian hamsters having cardiomyopathy and their sex- and age-matched littermates. The ratio of water to lipids and the ratio of phosphocreatine to ATP were obtained by 1H-NMR and 31P-NMR, respectively. These ratios were two-dimensionally plotted, thereby making it possible to differentiate cardiomyopathy from normal heart. NMR results were in good agreement with biochemical results. (Namekawa, K.)

  2. Wilson's disease: 31P and 1H MR spectroscopy and clinical correlation

    Proton (1H) magnetic resonance spectroscopy (MRS) changes are noted in Wilson's disease (WD). However, there are no studies regarding membrane phospholipid abnormality using 31P MRS in these patients. We aimed to analyze the striatal spectroscopic abnormalities using 31P and 1H MRS in WD. Forty patients of WD (treated, 29; untreated,11) and 30 controls underwent routine MR image sequences and in vivo 2-D 31P and 1H MRS of basal ganglia using an image-selected technique on a 1.5-T MRI scanner. Statistical analysis was done using Student's t test. The mean durations of illness and treatment were 6.2 ± 7.4 and 4.8 ± 5.9 years, respectively. MRI images were abnormal in all the patients. 1H MRS revealed statistically significant reduction of N-acetyl aspartate (NAA)/choline (Cho) and NAA/creatine ratios in striatum (1H MRS) of treated patients compared to controls. The mean values of phosphomonoesters (PME) (p 31P MRS study. The duration of illness correlated well with increased PME/PDE [p < 0.001], PME/TPh [p < 0.05], and PDE/TPh [p < 0.05] and decreased NAA/Cho [p < 0.05] ratios. There was correlation of MRI score and reduced NAA/Cho ratio with disease severity. The PME/PDE ratio (right) was elevated in the treated group [p < 0.001] compared to untreated group. There is reduced breakdown and/or increased synthesis of membrane phospholipids and increased neuronal damage in basal ganglia in patients with WD. (orig.)

  3. 1H and 31P nuclear magnetic resonance spectroscopy of erythrocyte extracts in myotonic muscular dystrophy

    Extracts freshly prepared from erythrocytes of patients with myotonic muscular dystrophy, their unaffected siblings, and normal control subjects were examined with both 1H and 31P nuclear magnetic resonance spectroscopy. A moderate variability was found in the relative amounts of various nonphosphorylated compounds among patients and control subjects; however, no significant differences were found between the groups. As for the phosphorylated compounds, the sum of ADP+ATP was found significantly elevated in the myotonic muscular dystrophy patients

  4. Molecular neurodevelopment: An in vivo31P-1H MRSI study

    Goldstein, Gerald; Panchalingam, Kanagasabai; McClure, Richard J.; Stanley, Jeffrey A.; Calhoun, Vince D.; Pearlson, Godfrey D.; Pettegrew, Jay W.

    2009-01-01

    Synaptic development and elimination are normal neurodevelopmental processes which if altered could contribute to various neuropsychiatric disorders. 31P-1H magnetic resonance spectroscopic imaging and structural MRI exams were conducted on 106 healthy children ages 6–18 years in order to identify neuromolecular indices of synaptic development and elimination. Over the age range studied, age-related changes in high-energy phosphate (phosphocreatine), membrane phospholipid metabolism (precurso...

  5. 31 P and two-dimensional 31 P-1 H NMR analysis of brain extracts in animal models of multiple sclerosis

    We report here the study of the brain phospholipid content of normal and myelin deficient (md) rats, which develop a physiological impairment at about 15-20 days, and die at 20-25 days of age. The aim is to gain insights into the lipid composition of developing brain, and also to reveal of there exist some early event in the phospholipid metabolism that produces a pathological condition similar to the formation of demyelination plaques in multiple sclerosis. 31 P NMR allows one to detect phospholipids selectively out of a complex lipid mixture in crude extracts. Two-dimensional (2D) 31 P-1H NMR with isotropic proton mixing seems to be a superior technique for assignment of phospholipid 31 P resonances. (author)

  6. Interleaved localized 1H/31P nuclear magnetic resonance spectroscopy of skeletal muscle

    Nuclear magnetic resonance (NMR) has been used as a spectroscopic method in physics and chemistry before it was developed to become a diagnostic imaging tool in medicine. When NMR spectroscopy is applied to human tissue, metabolism can be studied in normal physiological and pathological states in vivo. Metabolite concentrations and rates can be monitored dynamically and with localization of a defined region of interest. The 'window' which is opened for observation, i.e. which quantities are measured, depends on the nucleus used for RF excitation. Mechanisms of adenosine tri-phosphate (ATP) resynthesis, as a direct source of energy for muscle contraction, are phosphocreatine (PCr) splitting, glycolysis, beta-oxidation and, finally, oxidative phosphorylation. Whilst the dependency of these processes' fractional contribution to muscular energy supply on exercise type and duration is well known, quantitative models of the regulating mechanisms involved are still subject of current research. A large fraction of the established knowledge about metabolism is based on biochemical analysis of tissue acquired invasively (e.g. microdialysis and open-flow microperfusion) or representing averaged metabolic concentrations for the whole body (via serum metabolites or gas exchange analysis). Localized NMR spectroscopy, however, is capable of non-invasively acquiring time-resolved data from a defined volume of interest, in vivo. In contrast to the vast majority of MRS studies investigating metabolism, where spectra of a single nucleus (commonly 1H, 31P or 13C) were acquired or several MR spectra with different nuclei were measured in separate experiments, this work opens an additional 'window' on muscle metabolism by interleaved localized acquisition of 1H and 31P NMR spectra from human calf muscle in vivo, during rest, exercise and recovery, in a single experiment. Using this technique, the time courses of the concentrations of phosphocreatine, inorganic phosphate (Pi), ATP, total

  7. {sup 1}H and {sup 31}P-magnetic resonance spectroscopy of cerebral infarction in rats

    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)

  8. A practical guide for the setup of a 1H-31P-13C double cross-polarization (DCP) experiment.

    Ciesielski, Wlodzimierz; Kassassir, Hassan; Potrzebowski, Marek J

    2011-01-01

    O-phospho-L-threonine is a convenient sample to setup a (1)H-(31)P-(13)C double cross-polarization (DCP) Hartmann-Hahn match. The (1)H-(31)P-(13)C technique is extremely sensitive to the rate of the sample spinning. Both zero-quantum (ZQ) and double-quantum (DQ) cross-polarization operate at an average spinning rate (6-7 kHz). At higher spinning rates (10 kHz), the DQCP mechanism dominates and leads to a reduction of signal intensity, in particular for lower (31)P RF field strength. The application of two shape pulses during the second cross-polarization greatly improves the signal to noise ratio allowing the recording of better quality spectra. (31)P-(13)C spectrally induced filtering in combination with cross-polarization (SPECIFIC-CP) experiments can be carried out under ZQCP and DQCP conditions if careful attention is paid to the choice of RF field amplitudes and carriers Ω. Application of 1D and 2D (1)H-(31)P-(13)C experiments is demonstrated on model samples; disodium ATP hydrate and O-phospho-L-tyrosine. PMID:21440422

  9. Analysis of metabolites in human brain tumors and cerebral infarctions using 31P- and 1H-magnetic resonance spectroscopy

    31P- and 1H-MRS with a 2.0 tesla MRI/S system was used to monitor the cerebral energy levels, phospholipid metabolism, intracellular pH, and lactate and amino acid levels in patients with brain tumors and cerebral infarctions. Studies of human brain tumors have suggested that the 31P-MRS of malignant brain tumors show low concentrations of phosphocreatine (PCr) and β-ATP, high levels of phosphomonoester (PME) and inorganic Pi, and an alkaline pH. The Pi, PME, and intracellular pH of malignant lymphoma were higher than those of other brain tumors. 1H-MRS showed an increase of lactate in malignant brain tumors and epidermoids. After ACNU administration, the tumor 31P-MRS showed transient reduction and elevation of Pi on five patients with malignant gliomas. Intracellular pH also showed a transient reduction during radiotherapy. 1H-MRS showed a reduction of lactate at the beginning of therapy and showed a marked re-elevation of lactate with tumor regrowth. After radiotherapy, the normal brain 31P-MRS showed transient elevation and reduction of Pi. Intracellular pH also showed a transient elevation during radiotherapy. To investigate the mechanism of hyperbaric oxygen therapy (HBO) in cerebral ischemia, changes of brain lactate level were estimated by 1H-MRS. Although the Lactate/Creatine ratio decreased consistently over time in all patients, it decreased more rapidly in the patients receiving HBO therapy than in those without such therapy. 1H-MRS demonstrated that HBO therapy may improve metabolism in the ischemic brain and reduces the lactate levels. 31P- and 1H-MRS are practical tools for the clinical analysis of cerebral disorders as well as for deciding on therapeutic procedures and evaluating the response. (K.H.)

  10. A retunable surface coil for high field 31P and 1H magnetic resonance evaluations of the living mouse leg

    This study presents a retunable surface coil that can be adjusted to at least two Larmor frequencies sequentially without the need to remove the coil from the magnet and while avoiding interference between channels. A prototype 1H/31P surface coil for the analysis of the in vivo mouse leg under electrical stimulation was designed for operation at 11.75 T. The coil has a high-quality factor of over 100 for both operational frequencies. To demonstrate the capabilities of this simple design, in vivo experiments were conducted to acquire high-resolution 1H images and 31P spectra of the C57BL/6 mouse leg, both with high temporal resolution. Proton diffusion tensor imaging was also performed to evaluate rodent skeletal muscle architecture. This design makes the acquisition of physiological data about both muscle structure and energetics (PCr, ATP and Pi) possible in a single experimental session

  11. Myosin catalyzed ATP hydrolysis elucidated by 31P NMR kinetic studies and 1H PFG-diffusion measurements

    Song, Zhiyan; Parker, Kari J.; Enoh, Idorenyin; Zhao, Hua; Olubajo, Olarongbe

    2009-01-01

    We conducted 31P NMR kinetic studies and 1H-diffusion measurements on myosin-catalyzed hydrolysis of adenosine triphosphate (ATP) under varied conditions. The data elucidate well the overall hydrolysis rate and various factors that significantly impact the reaction. We found that the enzymatic hydrolysis of ATP to adenosine diphosphate (ADP) was followed by ADP hydrolysis, and different nucleotides such as ADP and guanosine triphosphate (GTP) acted as competitors of ATP. Increasing ATP or Mg2...

  12. Proton 1H- and Phosphorus 31P-MR spectroscopy (MRS in asymptomatic HIV-positive patients

    Gundolf Schuettfort

    2014-11-01

    Full Text Available Introduction: HIV infection is accompanied by a variety of neurological disorders. Depression of cell-mediated immunity is followed by the development of central nervous system opportunistic infections/tumours, and frequently by the occurrence of the AIDS dementia complex (ADC. However, the pathophysiology of the emergence of neuro-AIDS is still unknown. Despite the development of cognitive impairments, the early diagnosis, objectification and quantification of the existence and extent of this impairment during infection are difficult to recognize in each individual case. To support the early diagnosis of ADC, there is a need for additional, non-invasive diagnostic methods. In this study, it is of interest to answer the clinically relevant question of whether magnetic resonance spectroscopy can detect changes in the cerebral metabolism of asymptomatic HIV-positive patients and is possibly suitable for the early diagnosis and prevention of HIV encephalopathy. Methods: A group of 13 asymptomatic, HIV-positive patients with combined antiretroviral therapy (cART and 13 healthy controls were examined with 2D 1H-MRS and 3D 31P-MRS at 3T. The patients were treated with cART for at least 12 months. Changes in the absolute concentrations of phosphorylated metabolites (ATP, N-acetyl-aspartate, creatine, myo-Isonitol, glutamate/glutamine and choline-containing compounds were compared with that of control subjects. Results: Asymptomatic HIV-positive patients had significantly lower N-acetyl-aspartate in the white matter in a frontal and parietal target region. The other evaluated metabolites in the 1H MRS showed no significant difference between the HIV-positive patients and healthy controls. The 31P-MRS detected significant elevated values regarding the choline-containing compounds PEth, GPE and PCho. Conclusions: This spectroscopic study revealed a significantly lower N-acetyl-aspartate in the white matter in a frontal and parietal cerebral target region

  13. Wilson's disease: {sup 31}P and {sup 1}H MR spectroscopy and clinical correlation

    Sinha, Sanjib; Taly, A.B.; Prashanth, L.K. [National Institute of Mental Health and Neurosciences (NIMHANS), Department of Neurology, Bangalore (India); Ravishankar, S.; Vasudev, M.K. [National Institute of Mental Health and Neurosciences (NIMHANS), Department of Neuroimaging and Interventional Radiology, Bangalore (India)

    2010-11-15

    Proton ({sup 1}H) magnetic resonance spectroscopy (MRS) changes are noted in Wilson's disease (WD). However, there are no studies regarding membrane phospholipid abnormality using {sup 31}P MRS in these patients. We aimed to analyze the striatal spectroscopic abnormalities using {sup 31}P and {sup 1}H MRS in WD. Forty patients of WD (treated, 29; untreated,11) and 30 controls underwent routine MR image sequences and in vivo 2-D {sup 31}P and {sup 1}H MRS of basal ganglia using an image-selected technique on a 1.5-T MRI scanner. Statistical analysis was done using Student's t test. The mean durations of illness and treatment were 6.2 {+-} 7.4 and 4.8 {+-} 5.9 years, respectively. MRI images were abnormal in all the patients. {sup 1}H MRS revealed statistically significant reduction of N-acetyl aspartate (NAA)/choline (Cho) and NAA/creatine ratios in striatum ({sup 1}H MRS) of treated patients compared to controls. The mean values of phosphomonoesters (PME) (p < 0.0001), phosphodiesters (PDE) (p < 0.0001), and total phosphorus (TPh) (p < 0.0001) were elevated in patients compared to controls. Statistically significant elevated levels of ratio of PME/PDE (p = 0.05) observed in the striatum were noted in treated patients as compared to controls in the {sup 31}P MRS study. The duration of illness correlated well with increased PME/PDE [p < 0.001], PME/TPh [p < 0.05], and PDE/TPh [p < 0.05] and decreased NAA/Cho [p < 0.05] ratios. There was correlation of MRI score and reduced NAA/Cho ratio with disease severity. The PME/PDE ratio (right) was elevated in the treated group [p < 0.001] compared to untreated group. There is reduced breakdown and/or increased synthesis of membrane phospholipids and increased neuronal damage in basal ganglia in patients with WD. (orig.)

  14. 1H and 31P magnetic resonance spectroscopic imaging of white matter signal hyperintensity areas in elderly subjects

    White matter signal hyperintensities (WMSH) are commonly seen on MRI of elderly subjects. The purpose of this study was to characterize metabolic changes in the white matter of elderly subjects with extensive WMSH. We used water-suppressed proton (1H) magnetic resonance spectroscopic imaging (MRSI) to compare six subjects with extensive WMSH with eight age-matched elderly subjects with minimal or absent WMSH, and phosphorus (31P) MRSI to compare nine subjects with extensive WMSH and seven age-matched elderly subjects without extensive WMSH. Relative to region-matched tissue in elderly controls, extensive WMSH were associated with increased signal from choline-containing metabolites, no significant change of signal from N-acetylaspartate, and a trend to a decreased phosphomonoester (PME) resonance. These findings suggest that WMSH may be associated with an alteration of brain myelin phospholipids in the absence of axonal damage. There were no differences in energy phosphates, consistent with lack of ongoing brain ischemia. Within the group with extensive WMSH, PME resonance measures were significantly lower in WMSH than in contralateral normal-appearing white matter. These results provide information on pathophysiology of WMSH and a basis for comparison with WMSH in Alzheimer's disease, vascular dementia, multiple sclerosis, and other diseases. (orig.). With 4 figs., 4 tabs

  15. Analysis of metabolites in human brain tumors and cerebral infarctions using {sup 31}P- and {sup 1}H-magnetic resonance spectroscopy

    Hirakawa, Wataru [Kagoshima Univ. (Japan). Faculty of Medicine

    1996-08-01

    {sup 31}P- and {sup 1}H-MRS with a 2.0 tesla MRI/S system was used to monitor the cerebral energy levels, phospholipid metabolism, intracellular pH, and lactate and amino acid levels in patients with brain tumors and cerebral infarctions. Studies of human brain tumors have suggested that the {sup 31}P-MRS of malignant brain tumors show low concentrations of phosphocreatine (PCr) and {beta}-ATP, high levels of phosphomonoester (PME) and inorganic Pi, and an alkaline pH. The Pi, PME, and intracellular pH of malignant lymphoma were higher than those of other brain tumors. {sup 1}H-MRS showed an increase of lactate in malignant brain tumors and epidermoids. After ACNU administration, the tumor {sup 31}P-MRS showed transient reduction and elevation of Pi on five patients with malignant gliomas. Intracellular pH also showed a transient reduction during radiotherapy. {sup 1}H-MRS showed a reduction of lactate at the beginning of therapy and showed a marked re-elevation of lactate with tumor regrowth. After radiotherapy, the normal brain {sup 31}P-MRS showed transient elevation and reduction of Pi. Intracellular pH also showed a transient elevation during radiotherapy. To investigate the mechanism of hyperbaric oxygen therapy (HBO) in cerebral ischemia, changes of brain lactate level were estimated by {sup 1}H-MRS. Although the Lactate/Creatine ratio decreased consistently over time in all patients, it decreased more rapidly in the patients receiving HBO therapy than in those without such therapy. {sup 1}H-MRS demonstrated that HBO therapy may improve metabolism in the ischemic brain and reduces the lactate levels. {sup 31}P- and {sup 1}H-MRS are practical tools for the clinical analysis of cerebral disorders as well as for deciding on therapeutic procedures and evaluating the response. (K.H.)

  16. Bevacizumab impairs oxidative energy metabolism and shows antitumoral effects in recurrent glioblastomas: a 31P/1H MRSI and quantitative magnetic resonance imaging study

    HATTINGEN, ELKE; Jurcoane, Alina; Bähr, Oliver; Rieger, Johannes; Magerkurth, Jörg; Anti, Sandra; Steinbach, Joachim P.; Pilatus, Ulrich

    2011-01-01

    Bevacizumab shows unprecedented rates of response in recurrent glioblastomas (GBM), but the detailed mechanisms are still unclear. We employed in vivo magnetic resonance spectroscopic imaging (MRSI) and quantitative magnetic resonance imaging to investigate whether bevacizumab alters oxygen and energy metabolism and whether this effect has antitumoral activity in recurrent GBM. 31P and 1H MRSI, apparent diffusion coefficient (ADC), and high-resolution T2 and T2′ mapping (indirect marker of ox...

  17. 1H and 31P nuclear magnetic resonance investigation of the interaction between 2,3-diphosphoglycerate and human normal adult hemoglobin

    High-resolution 1H and 31P nuclear magnetic resonance spectroscopy has been used to investigate the binding of 2,3-diphosphoglycerate to human normal adult hemoglobin and the molecular interactions involved in the allosteric effect of the 2,3-diphosphoglycerate molecule on hemoglobin. Individual hydrogen ion NMR titration curves have been obtained for 22-26 histidyl residues of hemoglobin and for each phosphate group of 2,3-diphosphoglycerate with hemoglobin in both the deoxy and carbonmonoxy forms. The results indicate that 2,3-diphosphoglycerate binds to deoxyhemoglobin at the central cavity between the two β chains and the binding involves the β2-histidyl residues. Moreover, the results suggest that the binding site of 2,3-diphosphoglycerate to carbonmonoxyhemoglobin contains the same (or at least some of the same) amino acid residues responsible for binding in the deoxy form. As a result of the specific interactions with 2,3-diphosphoglycerate, the β2-histidyl residues make a significant contribution to the alkaline Bohr effect under these experimental conditions. These results give the first experimental demonstration that long-range electrostatic and/or conformation effects of the binding could play an important role in the allosteric effect of 2,3-diphosphoglycerate on hemoglobin. The 31P nuclear magnetic resonance titration data for each phosphate group of 2,3-diphosphoglycerate have been used to calculate the pK values of the phosphate groups in 2,3-diphosphoglycerate bound to deoxy- and carbon-monoxyhemoglobin and the proton uptake by 2,3-diphosphoglycerate upon ligand binding to hemoglobin

  18. Structural and dynamic differences between normal and transforming N-ras gene products: A 31P and isotope-edited 1H NMR study

    [15B]Glycine was biosynthetically incorporated into normal cellular N-ras p21 and a position 12 transforming mutant, in order to produce p21 proteins containing several site-specific NMR probes at or near activating positions in the guanine nucleotide binding domain. The authors have previously assigned all five glycine resonances located in loops directly involved in binding of guanosine diphosphate in the wild-type p21 protein. In this report, the corresponding glycine resonances in the p21 mutant have been assigned, and spectral differences between normal and mutant p21-guanosine diphosphate (p21-GDP) complexes have been investigated. The combined 1H15N and 31P NMR results show that substitution of aspartate for glycine-12 produces perturbations in the phosphoryl binding domain, near the point of the mutation. Although many of the remaining glycines were unaffected, spectral differences were also observed outside the GDP binding domain. Two of the five active-site glycines in wild-type p21-GDP have very slow amide proton exchange rates with water. The active=site glycine are located in solvent-exposed loops, so their apparent solvent inaccessibility may result from strong hydrogen bond formation between glycine amide protons and bound guanine diphosphate and/or other nearby groups in p21

  19. Modeling sickle cell vasoocculsion in the rat leg: Quantification of trapped sickle cells and correlation with 31P metabolic and 1H magnetic resonance imaging changes

    The authors have developed an animal model to elucidate the acute effects of perfusion abnormalities on muscle metabolism induced by different density-defined classes of erythrocytes isolated from sickle cell anemia patients. Technetium-99m (99mTc)-labeled, saline-washed normal (AA), homozygous sickle (SS), or high-density SS (SS4) erythrocytes were injected into the femoral artery of the rat and quantitative 99mTc imaging, 31P magnetic resonance spectroscopy by surface coil at 2 teslas, and 1H magnetic resonance imaging at 0.15 tesla were performed. Between 5 and 25 μl of SS4 cells was trapped in the microcirculation of the thigh. In contrast, fewer SS discocytes (SS2) or AA cells were trapped. After injection of SS4 cells an initial increase in inorganic phosphate was observed in the region of the thigh served by the femoral artery, intracellular pH decreased, and subsequently the proton relaxation time T1 reached a broad maximum at 18-28 hr. When T1 obtained at this time was plotted against the volume of cells trapped, an increase of T1 over the control value of 411 ± 48 msec was found that was proportional to the number of cells trapped. They conclude that the densest SS cells are most effective at producing vasoocclusion. The extent of the change detected by 1H magnetic resonance imaging is dependent on the amount of cells trapped in the microcirculation and the magnitude of the initial increase of inorganic phosphate

  20. Quantitative nuclear magnetic resonance spectrometry II. Purity of phosphorus-based agrochemicals glyphosate (N-(phosphonomethyl)-glycine) and profenofos (O-(4-bromo-2-chlorophenyl) O-ethyl S-propyl phosphorothioate) measured by 1H and 31P QNMR spectrometry

    The purities of the widely-used herbicide glyphosate (N-(phosphonomethyl)glycine), and the insecticide profenofos (O-(4-bromo-2-chlorophenyl) O-ethyl S-propyl phosphorothioate) were determined by 1H and 31P quantitative nuclear magnetic resonance (QNMR) spectrometry using an internal standard. QNMR does not need a standard reference of the same target analyte, in contrast to chromatographic methods, but only a compound containing the nucleus of interest. Sodium acetate and sodium phosphate of known purity were chosen as internal standards for 1H NMR and 31P NMR), respectively for the water soluble glyphosate and a single internal standard, trimethyl phosphate for both 1H and 31P NMR quantitative analysis of the organic soluble profenofos. These standards have NMR peaks that do not interfere with those of the analyte, they are chemically inert and are soluble in the deuterated solvent. The average purity of glyphosate obtained by 1H NMR (97.07%, σ=0.68) agreed with that by 31P NMR (96.53%, σ=0.90; ANOVA, P=0.074) for the five batches provided by the manufacturer according to the procedures for chemical registration in Australia. The standard deviations of seven independent analyses of a single batch by 1H NMR and 31P NMR were σ=0.24% and σ=0.33%, respectively, values which confirm the exceptional precision of the method. The purity of profenofos by 1H NMR (94.63%, σ=0.14) also agreed with that by 31P NMR (94.62%, σ=0.59; ANOVA, P=0.97). Uncertainty budgets for the measured purities of glyphosate and profenofos show that the uncertainty in the purity of the internal standard is a major contributor to the uncertainty of the result. NMR was also used to establish the impurity profile of both compounds, and quantify the impurities present

  1. Bevacizumab impairs oxidative energy metabolism and shows antitumoral effects in recurrent glioblastomas: a 31P/1H MRSI and quantitative magnetic resonance imaging study.

    Hattingen, Elke; Jurcoane, Alina; Bähr, Oliver; Rieger, Johannes; Magerkurth, Jörg; Anti, Sandra; Steinbach, Joachim P; Pilatus, Ulrich

    2011-12-01

    Bevacizumab shows unprecedented rates of response in recurrent glioblastomas (GBM), but the detailed mechanisms are still unclear. We employed in vivo magnetic resonance spectroscopic imaging (MRSI) and quantitative magnetic resonance imaging to investigate whether bevacizumab alters oxygen and energy metabolism and whether this effect has antitumoral activity in recurrent GBM. (31)P and (1)H MRSI, apparent diffusion coefficient (ADC), and high-resolution T2 and T2' mapping (indirect marker of oxygen extraction) were investigated in 16 patients with recurrent GBM at 3 Tesla before and 1.5-2 months after initiation of therapy with bevacizumab. Changes of metabolite concentrations and of the quantitative values in the tumor and normal appearing brain tissue were calculated. The Wilcoxon signed-ranks test was used to evaluate differences for tumor/edema versus control as well as changes before versus after commencement of therapy. Survival analyses were performed for significant parameters. Tumor T2', pH, ADC, and T2 decreased significantly in patients responding to bevacizumab therapy (n = 10). Patients with at least 25% T2' decrease during treatment showed longer progression-free and overall survival durations. Levels of high-energy metabolites were lower at baseline; these persisted under therapy. Glycerophosphoethanolamine as catabolic phospholipid metabolite increased in responders. The MRSI data support the hypothesis that bevacizumab induces relative tumor hypoxia (T2' decrease) and affects energy homeostasis in recurrent GBM, suggesting that bevacizumab impairs vascular function. The antiangiogenic effect of bevacizumab is predictive of better outcome and seems to induce antitumoral activity in the responding GBMs. PMID:21890539

  2. Hepatic lipid profiling of deer mice fed ethanol using {sup 1}H and {sup 31}P NMR spectroscopy: A dose-dependent subchronic study

    Fernando, Harshica; Bhopale, Kamlesh K.; Boor, Paul J.; Ansari, G.A. Shakeel; Kaphalia, Bhupendra S., E-mail: bkaphali@utmb.edu

    2012-11-01

    Chronic alcohol abuse is a 2nd major cause of liver disease resulting in significant morbidity and mortality. Alcoholic liver disease (ALD) is characterized by a wide spectrum of pathologies starting from fat accumulation (steatosis) in early reversible stage to inflammation with or without fibrosis and cirrhosis in later irreversible stages. Previously, we reported significant steatosis in the livers of hepatic alcohol dehydrogenase (ADH)-deficient (ADH{sup −}) vs. hepatic ADH-normal (ADH{sup +}) deer mice fed 4% ethanol daily for 2 months [Bhopale et al., 2006, Alcohol 39, 179–188]. However, ADH{sup −} deer mice fed 4% ethanol also showed a significant mortality. Therefore, a dose-dependent study was conducted to understand the mechanism and identify lipid(s) involved in the development of ethanol-induced fatty liver. ADH{sup −} and ADH{sup +} deer mice fed 1, 2 or 3.5% ethanol daily for 2 months and fatty infiltration in the livers were evaluated by histology and by measuring dry weights of extracted lipids. Lipid metabolomic changes in extracted lipids were determined by proton ({sup 1}H) and {sup 31}phosphorus ({sup 31}P) nuclear magnetic resonance (NMR) spectroscopy. The NMR data was analyzed by hierarchical clustering (HC) and principle component analysis (PCA) for pattern recognition. Extensive vacuolization by histology and significantly increased dry weights of total lipids found only in the livers of ADH{sup −} deer mice fed 3.5% ethanol vs. pair-fed controls suggest a dose-dependent formation of fatty liver in ADH{sup −} deer mouse model. Analysis of NMR data of ADH{sup −} deer mice fed 3.5% ethanol vs. pair-fed controls shows increases for total cholesterol, esterified cholesterol, fatty acid methyl esters (FAMEs), triacylglycerides and unsaturation, and decreases for free cholesterol, phospholipids and allylic and diallylic protons. Certain classes of neutral lipids (cholesterol esters, fatty acyl chain (-COCH{sub 2}-) and FAMEs) were

  3. Hepatic lipid profiling of deer mice fed ethanol using 1H and 31P NMR spectroscopy: A dose-dependent subchronic study

    Chronic alcohol abuse is a 2nd major cause of liver disease resulting in significant morbidity and mortality. Alcoholic liver disease (ALD) is characterized by a wide spectrum of pathologies starting from fat accumulation (steatosis) in early reversible stage to inflammation with or without fibrosis and cirrhosis in later irreversible stages. Previously, we reported significant steatosis in the livers of hepatic alcohol dehydrogenase (ADH)-deficient (ADH−) vs. hepatic ADH-normal (ADH+) deer mice fed 4% ethanol daily for 2 months [Bhopale et al., 2006, Alcohol 39, 179–188]. However, ADH− deer mice fed 4% ethanol also showed a significant mortality. Therefore, a dose-dependent study was conducted to understand the mechanism and identify lipid(s) involved in the development of ethanol-induced fatty liver. ADH− and ADH+ deer mice fed 1, 2 or 3.5% ethanol daily for 2 months and fatty infiltration in the livers were evaluated by histology and by measuring dry weights of extracted lipids. Lipid metabolomic changes in extracted lipids were determined by proton (1H) and 31phosphorus (31P) nuclear magnetic resonance (NMR) spectroscopy. The NMR data was analyzed by hierarchical clustering (HC) and principle component analysis (PCA) for pattern recognition. Extensive vacuolization by histology and significantly increased dry weights of total lipids found only in the livers of ADH− deer mice fed 3.5% ethanol vs. pair-fed controls suggest a dose-dependent formation of fatty liver in ADH− deer mouse model. Analysis of NMR data of ADH− deer mice fed 3.5% ethanol vs. pair-fed controls shows increases for total cholesterol, esterified cholesterol, fatty acid methyl esters (FAMEs), triacylglycerides and unsaturation, and decreases for free cholesterol, phospholipids and allylic and diallylic protons. Certain classes of neutral lipids (cholesterol esters, fatty acyl chain (-COCH2-) and FAMEs) were also mildly increased in ADH− deer mice fed 1 or 2% ethanol. Only small

  4. Interaction Study of an Amorphous Solid Dispersion of Cyclosporin A in Poly-Alpha-Cyclodextrin with Model Membranes by 1H-, 2H-, 31P-NMR and Electron Spin Resonance

    Jean-Claude Debouzy

    2014-01-01

    Full Text Available The properties of an amorphous solid dispersion of cyclosporine A (ASD prepared with the copolymer alpha cyclodextrin (POLYA and cyclosporine A (CYSP were investigated by 1H-NMR in solution and its membrane interactions were studied by 1H-NMR in small unilamellar vesicles and by 31P 2H NMR in phospholipidic dispersions of DMPC (dimyristoylphosphatidylcholine in comparison with those of POLYA and CYSP alone. 1H-NMR chemical shift variations showed that CYSP really interacts with POLYA, with possible adduct formation, dispersion in the solid matrix of the POLYA, and also complex formation. A coarse approach to the latter mechanism was tested using the continuous variations method, indicating an apparent 1 : 1 stoichiometry. Calculations gave an apparent association constant of log Ka = 4.5. A study of the interactions with phospholipidic dispersions of DMPC showed that only limited interactions occurred at the polar head group level (31P. Conversely, by comparison with the expected chain rigidification induced by CYSP, POLYA induced an increase in the fluidity of the layer while ASD formation led to these effects almost being overcome at 298 K. At higher temperature, while the effect of CYSP seems to vanish, a resulting global increase in chain fluidity was found in the presence of ASD.

  5. Synthesis and multinuclear (1H, 13C, 31P, 119Sn) NMR study of trimethyland; triphenyl-tin (IV) with cyclic dithiophosphate ligands

    Patricia García y García; Marcela López Cardoso; María del Carmen Pérez Redondo; Patricia Martínez Salas; Ave María Cotero Villegas; Raymundo Cea Olivares

    2004-01-01

    En este trabajo se informa la síntesis y caracterización; estructural de seis nuevos ditiofosfatos de trimetil- y trifenil-estaño (IV).; Los compuestos 1-6 fueron caracterizados por IR, EM IE y RMN multinuclear,; (1H, 13C, 19P y 119Sn). Los seis compuestos manifiestan un; comportamiento monomérico, con una penta-coordinación del átomo de; estaño y un comportamiento monometálico biconectivo de los ligantes.; Los compuestos 1-4 presentan en solución una rápida interconversión;...

  6. 31P and 1H NMR studies of the structure of enzyme-bound substrate complexes of lobster muscle arginine kinase: Relaxation measurements with Mn(II) and Co(II)

    The paramagnetic effects of Mn(II) and Co(II) on the spin-lattice relaxation rates of 31P nuclei of ATP and ADP and of Mn(II) on the spin-lattice relaxation rate of the δ protons of arginine bound to arginine kinase from lobster tail muscle have been measured. Temperature variation of 31P relaxation rates in E-MnADP and E-MnATP yields activation energies (ΔE) in the range 6-10 kcal/mol. Thus, the 31P relaxation rates in these complexes are exchange limited and cannot provide structural information. However, the relaxation rates in E-CoADP and E-CoATP exhibit frequency dependence and ΔE values in the range 1-2 kcal/mol; i.e., these rates depend upon 31P-Co(II) distances. These distances were calculated to be in the range 3.2-4.5 angstrom, appropriate for direct coordination between Co(II) and the phosphoryl groups. The paramagnetic effect of Mn(II) on the 1H spin-lattice relaxation rate of the δ protons of arginine in the E-MnADP-Arg complex was also measured at three frequencies. From the frequency dependence of the relaxation rate an effective τC of 0.6 ns has also been calculated, which is most likely to be the electron spin relaxation rate (τS1) for Mn(II) in this complex. The distance estimated on the basis of the reciprocal sixth root of the average relaxation rate of the δ protons was 10.9 ± 0.3 angstrom

  7. 1H, 13C and 31P-NMR spectroscopic study of glucose metabolism of muscle larva Trichinella spiralis (U.S.A. strain), and the effects of the end-products on the host (mouse)

    1H- and 13C-nuclear magnetic resonance (NMR) spectroscopy was used to identify and quantitate metabolites excreted by muscle larva Trichinella spiralis maintained aerobically in the presence of D- (13C6) glucose and (1, 1'-13C2) succinate. End-products of glucose metabolism studied by 1H-NMR were lactate, acetate, succinate, proionate, n-valerate and alanine, at the molar ratio of 1:2:1:0.6:0.5:0.6. 13C-NMR measurement proved that all the products originated from the glucose in the medium via the phosphoenolpyruvate carboxykinase-succinate pathway and the tricarboxylic acid cycle. In vivo 31P-NMR spectra were also taken by the surface coil method from the leg muscle of mice which had been infected with T. spiralis. Intracelluar pH and relative amount of ATP in the leg muscle of the infected mice were found to decrease significantly as compared with that of control mice. (author)

  8. In vivo 31P magnetic resonance spectroscopy and 1H magnetic resonance imaging of human bladder carcinoma on nude mice: effects of tumour growth and treatment with cis-dichloro-diamine platinum

    De Certaines, J D; Albrectsen, J; Larsen, V A;

    1992-01-01

    phosphate and phosphomonoesters and a decrease of phosphocreatine. Fast growing tumours and early stage of regrowth after treatment presented a higher phosphocreatine/beta NTP ratio. Following CDDP treatment, 31P metabolite ratios and pH were significantly altered compared with age-matched controls, as...... early as 6 hours after treatment. Although necrotic area was clearly visible in MRI, no treatment effect could be detected on the images of treated tumours....

  9. In vivo 31P magnetic resonance spectroscopy and 1H magnetic resonance imaging of human bladder carcinoma on nude mice: effects of tumour growth and treatment with cis-dichloro-diamine platinum

    De Certaines, J D; Albrectsen, J; Larsen, V A;

    1993-01-01

    phosphate and phosphomonoesters and a decrease of phosphocreatine. Fast growing tumours and early stage of regrowth after treatment presented a higher phosphocreatine/beta NTP ratio. Following CDDP treatment, 31P metabolite ratios and pH were significantly altered compared with age-matched controls, as...... early as 6 hours after treatment. Although necrotic area was clearly visible in MRI, no treatment effect could be detected on the images of treated tumours....

  10. Polarity of annealing and structural analysis of the RNase H resistant alpha-5'-d[TACACA].beta-5'-r[AUGUGU] hybrid determined by high-field 1H, 13C, and 31P NMR analysis

    The novel hybrid duplex alpha-5'-d[TACACA]-3'.beta-5'-r[AUGUGU]-3' was analyzed extensively by 1D and 2D NMR methods. Two forms of the duplex exist in about an 80:20 ratio. Analysis of the exchangeable imino protons of the major component revealed that three AU and one AT base pair are present in addition to two GC base pairs, confirming that the duplex anneals in parallel orientation. The presence of the AT base pair, which can only be accounted for by a parallel duplex, was confirmed by a selective INEPT experiment, which correlated the thymidine imino proton to its C5 carbon. The lesser antiparallel form could be detected by exchangeable and nonexchangeable proton resonances in both strands. An exchange peak was observed in the NOESY spectrum for the thymidine methyl group resonance in both the predominant and lesser conformations, indicating the lifetime of the individual structures was on the millisecond time scale. The nonexchangeable protons of the predominant duplex were assigned by standard methods. The sugar pucker of the ribonucleosides was determined to be of the S type by a pseudorotation analysis according to Altona, with the J-couplings measured from the multiplet components of the phase-sensitive COSY experiment. The NOE pattern observed for the alpha-deoxynucleosides also suggested an S-type sugar pucker. The adoption of an S-type sugar pucker for both strands indicates that, in contrast to RNA.DNA duplexes formed exclusively from beta-nucleotides, the alpha-DNA.beta-RNA duplex may form a B-type helix. The 31P resonances of the alpha and beta strands have very different chemical shifts in the hybrid duplex and the difference persists above the helix melting temperature, indicating an intrinsic difference in 31P chemical shift for nucleotides differing only in the configuration about the glycosidic bond

  11. Anestésicos locais: interação com membranas de eritrócitos de sangue humano, estudada por ressonância magnética nuclear de 1H e 31P

    Fraceto Leonardo Fernandes

    2004-01-01

    Full Text Available The literature carries many theories about the mechanism of action of local anesthetics (LA. We can highlight those focusing the direct effect of LA on the sodium channel protein and the ones that consider the interaction of anesthetic molecules with the lipid membrane phase. The interaction between local anesthetics and human erythrocyte membranes has been studied by ¹H and 31P nuclear magnetic resonance spectroscopy. It was found that lidocaine (LDC and benzocaine (BZC bind to the membranes, increase the mobility of the protons of the phospholipid's acyl chains, and decrease the mobility and/or change the structure of the polar head groups. The results indicate that lidocaine molecules are inserted across the polar and liquid interface of the membrane, establishing both electrostatic (charged form and hydrophobic (neutral form interactions. Benzocaine locates itself a little deeper in the bilayer, between the interfacial glycerol region and the hydrophobic core. These changes in mobility or conformation of membrane lipids could affect the Na+-channel protein insertion in the bilayer, stabilizing it in the inactivated state, thus causing anesthesia.

  12. Phase diagram of soybean phosphatidylcholine-diacylglycerol-water studied by x-ray diffraction and 31P- and pulsed field gradient 1H-NMR: evidence for reversed micelles in the cubic phase.

    Orädd, G; Lindblom, G; Fontell, K; Ljusberg-Wahren, H

    1995-05-01

    The phase equilibria of the system soybean phosphatidylcholine, diacylglycerol, and water has been determined using a combination of classical methods together with x-ray diffraction and NMR techniques. In particular, the extent of the phase regions of the lamellar, the reversed hexagonal, and the cubic phases have been determined. By pulsed field gradient 1H-NMR, the diffusion coefficients of all three components in a cubic phase composed of soybean phosphatidylcholine, diacylglycerol, and heavy water have been determined at 25 and 59 degrees C and also for the corresponding cubic phase composed of the chemically more well defined synthetic components 1,2-dioleoyl-sn-glycero-3-phosphocholine (DOPC), 1,2-dioleoylglycerol (DOG), and heavy water. The extension of the phase region of the cubic phase did not seem to change appreciably for the two ternary systems studied. The translational diffusion coefficient of DOPC in this cubic phase is more than an order of magnitude smaller (3 x 10(-13) m2 s-1, 59 degrees C) than the lateral diffusion coefficient of DOPC in an oriented lipid bilayer (5 x 10(-12) m2 s-1, 35 degrees C), whereas the diffusion coefficients of water and DOG were found to be about two orders of magnitude larger than DOPC at 59 degrees C. It is concluded that the cubic phase is built built up of closed reversed micelles in accordance with the suggestion from previous x-ray diffraction studies. PMID:7612827

  13. Internally Stabilized Selenocysteine Derivatives: Syntheses, $^7^7$Se NMR and Biomimetic Studies

    Phadnis, Prasad P; Mugesh, G.

    2005-01-01

    Selenocystine $([Sec]_2)$ and aryl-substituted selenocysteine (Sec) derivatives are synthesized, starting from commercially available amino acid L-serine. These compounds are characterized by a number of analytical techniques such as NMR $(^1H, ^1^3C and ^7^7Se)$ and TOF mass spectroscopy. This study reveals that the introduction of amino/imino substituents capable of interacting with selenium may stabilize the Sec derivatives. This study further suggests that the oxidation-elimination reacti...

  14. 2006 Rose Site 31P

    US Fish and Wildlife Service, Department of the Interior — Underwater Site 31P was established off Rose Atoll, American Samoa by Dr. James Maragos, U.S. Fish & Wildlife Service, on August 22, 1999. The site was...

  15. 2012 Rose Site 31P

    US Fish and Wildlife Service, Department of the Interior — Underwater Site 31P was established off Rose Atoll, American Samoa by Dr. James Maragos, U.S. Fish & Wildlife Service, on August 22, 1999. The site was...

  16. 2004 Rose Site 31P

    US Fish and Wildlife Service, Department of the Interior — Underwater Site 31P was established off Rose Atoll, American Samoa by Dr. James Maragos, U.S. Fish & Wildlife Service, on August 22, 1999. The site was...

  17. 2005 Rose Site 31P

    US Fish and Wildlife Service, Department of the Interior — Underwater Site 31P was established off Rose Atoll, American Samoa by Dr. James Maragos, U.S. Fish (5) = between meters 4 and 5). Quantitative analysis of the...

  18. 1999 Rose Site 31P

    US Fish and Wildlife Service, Department of the Interior — Underwater Site 31P was established off Rose Atoll, American Samoa by Dr. James Maragos, U.S. Fish & Wildlife Service, on August 22, 1999. The site was...

  19. 77Se NMR studies on ovine erythrocyte glutathione peroxidase

    To facilitate 77Se NMR observation of the endogenous active site selenium in ovine erythrocyte glutathione peroxidase (GSHPx), lambs have been maintained on an artificial diet deficient in selenium and supplemented with 0.2 ppm 92atom% 77Se , as selenite. After 5 months, preparations of GSHPx showed that incorporation of selenium from the artificial diet represented 88% of the GSHPx selenium. Each monthly bleeding of two sheep routinely yielded 20mg of pure 77Se-enriched GSHPx. Limitations on the solubility of the enzyme have so far prevented observation of 77Se resonances from the intact enzyme. Upon denaturation, a broad resonance is observed at 277 ppm, indicating that the selenium is involved in mixed selenide sulfide bonds both inter and intramolecularly. Reduction of the SeS bonds with dithiothreitol resulted in an upfield shift of the 77Se resonance to -212 ppm at pH 8 and -55ppm at pH4.2, consistent with formation of Se- and SeH respectively. It is concluded that the selenium is most probably in the SeS or Se- form in the intact enzyme. Relaxation time measurements were made at field strengths of 4.7 and 9.4T, which demonstrated the dominance of chemical shift anisotropy (CSA) relaxation for the selenium in GSHPx. A value of ≤ 262 ppm was determined for the CSA of the iodoacetamide derivative of GSHPx

  20. Synthesis of [(77)Se]-methylselenocysteine when preparing sauerkraut in the presence of [(77)Se]-selenite. Metabolic transformation of [ (77)Se]-methylselenocysteine in Wistar rats determined by LC-IDA-ICP-MS.

    Sánchez-Martínez, María; Pérez-Corona, Teresa; Martínez-Villaluenga, Cristina; Frías, Juana; Peñas, Elena; Porres, Jesús M; Urbano, Gloria; Cámara, Carmen; Madrid, Yolanda

    2014-12-01

    The use of enriched Se isotopes as tracers has provided important information on Se metabolism. However, selenium isotopes are expensive and difficult to obtain. A simple and cheap strategy based on the production of [(77)Se]-methylselenocysteine ([(77)Se]-MeSeCys) when preparing sauerkraut in the presence of [(77)Se]-selenite was developed. The resulting [(77)Se]-MeSeCys was used for evaluating the metabolic transformation of MeSeCys in Wistar rats, by feeding them with an AIN-93 M diet containing 20 % sauerkraut enriched in [(77)Se]-MeSeCys. Organs (liver, kidney, brain, testicles, and heart) were obtained after seven days of treatment and subjected to total selenium and selenium-speciation analysis by high-performance liquid chromatography coupled with isotope-dilution-analysis inductively-coupled-plasma mass spectrometry (HPLC-IDA-ICP-MS). Analysis of (77)Se-labeled organs revealed a prominent increase (more than 100 % Se-level enhancement) of selenium in the kidney and heart, whereas in the liver selenium concentration only increased by up to 20 % and it remained constant in the brain and testicles. (77)Se-enriched-sauerkraut supplementation does not alter the concentration of other essential elements in comparison to controls except for in the heart and kidney, in which selenium was positively correlated with Mg, Zn, Cu, and Mo. HPLC-ICP-MS analysis of hydrolyzed extracts after carbamidomethylation of the (77)Se-labeled organs revealed the presence of [(77)Se]-SeCys and an unknown Se-containing peak, the identity of which could not be verified by electrospray-ionization (ESI)-MS-MS. Low amounts of [(77)Se]-MeSeCys were found in (77)Se-labeled liver and kidney extracts, suggesting the incorporation of this selenium species in its intact form. PMID:25311192

  1. Clinical protocols for 31P MRS of the brain and their use in evaluating optic pathway gliomas in children

    Introduction: In vivo 31P Magnetic Resonance Spectroscopy (MRS) measures phosphorus-containing metabolites that play an essential role in many disease processes. An advantage over 1H MRS is that total choline can be separated into phosphocholine and glycerophosphocholine which have opposite associations with tumour grade. We demonstrate 31P MRS can provide robust metabolic information on an acceptable timescale to yield information of clinical importance. Methods: All MRI examinations were carried out on a 3T whole body scanner with all 31P MRS scans conducted using a dual-tuned 1H/31P head coil. Once optimised on phantoms, the protocol was tested in six healthy volunteers (four male and two female, mean age: 25 ± 2.7). 31P MRS was then implemented on three children with optic pathway gliomas. Results: 31P MRS on volunteers showed that a number of metabolite ratios varied significantly (p < 0.05 ANOVA) across different structures of the brain, whereas PC/GPC did not. Standard imaging showed the optic pathway gliomas were enhancing on T1-weighted imaging after contrast injection and have high tCho on 1H MRS, both of which are associated with high grade lesions. 31P MRS showed the phosphocholine/glycerophosphocholine ratio to be low (<0.6) which suggests low grade tumours in keeping with their clinical behaviour and the histology of most biopsied optic pathway gliomas. Conclusion: 31P MRS can be implemented in the brain as part of a clinical protocol to provide robust measurement of important metabolites, in particular providing a greater understanding of cases where tCho is raised on 1H MRS

  2. In vivo magnetic resonance studies of human brain energy metabolism by 31P-spectroscopy

    Magnetic resonance (MR) spectroscopy is a very powerful tool for obtaining biochemical information from structurally and functionally intact biological tissues. Following the introduction of high field (1.5 Tesla) wholebody systems it is possible to perform spectroscopic studies on human beings. Thus, MR-spectroscopy may become a very important research tool in physiology, clinical diagnosis and treatment follow-up. So far the human studies have concentrated on the phosphorus (31P) and (1H) nuclei. (author)

  3. Ex vivo identification of atherosclerotic plaque calcification by a 31P solid-state magnetic resonance imaging technique.

    Hallock, Kevin J; Hamilton, James A

    2006-12-01

    Calcified tissue is a common component of atherosclerotic plaques, and occurs most often in mature plaques. The process of calcification is a poorly understood risk factor that may contribute to a plaque's vulnerability to sudden rupture. In this study a solid-state imaging sequence, termed single-point imaging (SPI), was used to observe calcification directly in ex vivo atherosclerotic plaques. Standards were used to validate the ability of (31)P SPI to detect and differentiate calcification from crystalline cholesterol, phospholipids, and other plaque components. After suitable experimental parameters were found, human carotid specimens obtained by endarterectomy were imaged ex vivo by (31)P solid-state imaging and standard (1)H methods. In contrast to (1)H imaging methods, (31)P imaging detected only the calcification in the plaque. PMID:17089379

  4. Neutron-capture experiment on 77Se with EXILL at ILL Grenoble

    Lorenz Ch.

    2015-01-01

    Full Text Available The neutron capture reaction at 77Se has been studied with cold neutrons in the course of the EXILL campaign at the high-flux reactor of the Institut Laue-Langevin Grenoble. A simulation of the detector array with Geant4 has been accomplished and evaluated. The detector response has been deduced and measured spectra were unfolded, which have been compared with simulations using γDex to determine strength functions.

  5. Nuclear-Overhauser-enhanced MR imaging of (31)P-containing metabolites: multipoint-Dixon vs. frequency-selective excitation.

    Rink, Kristian; Berger, Moritz C; Korzowski, Andreas; Breithaupt, Mathies; Biller, Armin; Bachert, Peter; Nagel, Armin M

    2015-12-01

    The purpose of this study is to develop nuclear-Overhauser-enhanced (NOE) [(1)H]-(31)P magnetic resonance imaging (MRI) based on 3D fully-balanced steady-state free precession (fbSSFP). Therefore, two implementations of a 3D fbSSFP sequence are compared using frequency-selective excitation (FreqSel) and multipoint-Dixon (MP-Dixon). (31)P-containing model solutions and four healthy volunteers were examined at field strengths of B0=3T and 7T. Maps of the distribution of phosphocreatine (PCr), inorganic phosphate (Pi), and adenosine 5´-triphosphate (ATP) in the human calf were obtained with an isotropic resolution of 1.5cm (1.0cm) in an acquisition time of 5min (10min). NOE-pulses had the highest impact on the PCr acquisitions enhancing the signal up to (82 ± 13) % at 3T and up to (37 ± 9) % at 7T. An estimation of the level of PCr in muscle tissue from [(1)H]-(31)P MRI data yielded a mean value of (33 ± 8) mM. In conclusion, direct [(1)H]-(31)P imaging using FreqSel as well as MP-Dixon is possible in clinically feasible acquisition times. FreqSel should be preferred for measurements where only a single metabolite resonance is considered. MP-Dixon performs better in terms of SNR if a larger spectral width is of interest. PMID:26248272

  6. Early detection of cerebral infarction by 31P spectroscopic imaging

    Recent advances in magnetic resonance spectroscopy permit noninvasive study of brain metabolism in vivo, 31P spectroscopic imaging being the method for evaluation of localized phosphorous metabolism. Experimentally, an ischemic-hypoxic brain insult is characterized by depletion of high energy metabolites. These changes are seen immediately after an ischemic insult. We had the opportunity of carrying out 31P spectroscopic imaging of hyperacute cerebral infarction, while MRI and CT were negative. Cerebral infarction of the middle cerebral artery territory was suggested by 31P spectroscopic imaging, which was closely consistent with a later-developing region of low density on CT. In cerebral infarction, early detection of the lesion is a useful pointer to the patient's prognosis, making 31P spectroscopic imaging a potential tool. (orig.)

  7. 31P NMR Study on Some Phosphorus-Containing Compounds

    2000-01-01

    31P NMR has become a widely applied spectroscopic probe of the structure of phosphorus-containing compounds. Meanwhile, the application of 31P NMR has been rapidly expanded to biochemistry and medicinal chemistry of phosphorus-containing compounds because the growing importance of the phosphorus compounds is now widely realized. We report here the results of 31P NMR study on some phosphorus-containing compounds, namely, O-alkyl O-4-nitrophenyl methyl phosphonates with different alkyl chain-length (MePO-n), 4-nitrophenyl alkylphenylphosphinates with different alkyl chain-length (PhP-n), diethyl phosphono- acetonitrile anion and diethyl phosphite anion . Our results indicate that 31P NMR can not only be applied to not only the study of the hydrolytic reactions of MePO-8 and PhP-8 but also be applied to the study of the presence of the anions of diethylphosphonoacetonitrile and diethyl phosphite in nucleophilic reactions.

  8. 31P Solid-state MAS NMR spectra

    The structures of the silicoaluminiophosphates MCM-1 and MCM9 were characterized by 27Al and 31P MAS NMR. The structural identity of MCM-1 and its silicon-free homologue AlPO4-H3 is demonstrated. The presence of a structural mixture in MCM-9 is confirmed. 31P MAS NMR spectra of MCM-9 could be interpreted as a superposition of spectra of VPI-5, AlPO4-H3 and SAPO-11 phases. (author). 12 refs.; 3 figs.; 1 tab

  9. 77Se nuclear magnetic resonance of topological insulator Bi2Se3

    Georgieva, Nataliya M.; Rybicki, Damian; Guehne, Robin; Williams, Grant V. M.; Chong, Shen V.; Kadowaki, Kazuo; Garate, Ion; Haase, Jürgen

    2016-05-01

    Topological insulators constitute a new class of materials with an energy gap in the bulk and peculiar metallic states on the surface. We report on new features resulting from the bulk electronic structure, based on a comprehensive nuclear magnetic resonance (NMR) study of 77Se on Bi2Se3 and Cu0.15Bi2Se3 single crystals. First, we find two resonance lines and show that they originate from the two inequivalent Se lattice sites. Second, we observe unusual field-independent linewidths and attribute them to an unexpectedly strong internuclear coupling mediated by bulk electrons. In order to support this interpretation, we present a model calculation of the indirect internuclear coupling and show that the Bloembergen-Rowland coupling is much stronger than the Ruderman-Kittel-Kasuya-Yosida coupling. Our results call for a revision of earlier NMR studies and add information concerning the bulk electronic properties.

  10. Bio-fortification and isotopic labelling of Se metabolites in onions and carrots following foliar application of Se and 77Se

    Kápolna, Emese; Laursen, Kristian H.; Husted, Søren;

    2012-01-01

    The aims were to bio-fortify onions by foliar application of selenium (Se) and to intrinsically label bioactive Se-metabolites in onion and carrot by enriched, stable 77Se for use in human physiological studies. Onion bulbs and leaves were enriched in Se by repeated foliar spraying of 10 or 100μg......Seml−1 solutions of sodium selenite (Se(IV)) or sodium selenate (Se(VI)). ICP-MS analysis of onion leaves and bulbs showed that the Se concentration was enhanced by up to a factor of approximately 50 and 200 in bulbs and leaves, respectively. HPLC–ICP-MS analysis of proteolytic plant extracts showed......Se. The 77Se- labelled metabolites in onions were predominantly γ-glutamyl-77Se-selenomethyl-selenocysteine (γ-glu-Me77SeCys), 77Se-methylselenocysteine (Me77SeCys) and 77Se-selenomethionine (77SeMet). Furthermore, we report here for the first time the finding in carrots of the bioactive Me77Se...

  11. 31P NMR spectra in monitoring of hematological malignancies

    The investigations of 31P spectra of sera of patients with hematological malignancies are a preliminary clinical trials over the introduction of NMRS to monitoring of the therapy. The aim was to investigate possible diagnostic and prognostic importance of phospholipid metabolism changes, as well as investigation in vitro of possible changes during chemotherapy. Altogether were obtained 450 phosphorus spectra. Studies were carried out on AMX 300 Bruker spectrometer 7.05 T. 31P spectra were performed in 40 healthy volunteers, 33 patients with acute leukemia, 20 with multiple myeloma and 33 suffering from malignant lymphomas at the time of diagnosis and repeated up to 13 times during chemotherapy. 31P MRS spectra of normal serum to consist of 3 peaks including a downfield peak due to Pi and 2 additional upfield field peaks from phospholipids phosphatidyletanolamine with sphingomyelin (PE+SM) and phosphatidylcholine (PC). Long-term follow-up studies showed a good correlation between this 31P MRS evaluation of sera and the response of the disease to the therapy. At the time of a diagnose spectra showed strongly reduced peak areas and intensities from phospholipids (PC and PE+SM). During chemotherapy were observed important changes in spectra: 1) in responding patients the spectral profile changed to resemble that of normal serum with increased peak intensities of PC and of PE+SM, 2) in non-responding individuals peak intensities of PC and PE+SM were reduced. (author)

  12. Exploring new Routes for Identifying Phosphorus Species in Terrestrial and Aquatic Ecosystems with 31P NMR

    Vestergren, Johan; Persson, Per; Sundman, Annelie; Ilstedt, Ulrik; Giesler, Reiner; Schleucher, Jürgen; Gröbner, Gerhard

    2014-05-01

    Phosphorus (P) is the primary growth-limiting nutrient in some of the world's biomes. Rock phosphate is a non-renewable resource and the major source of agricultural fertilizers. Predictions of P consumption indicate that rock phosphate mining may peak within 35 years, with severe impacts on worldwide food production1. Organic P compounds constitute a major fraction of soil P, but little is known about the dynamics and bioavailability of organic P species. Our aim is to develop new liquid and solid state 31P-NMR (nuclear magnetic resonance) techniques to identify P-species in water and soils; information required for correlating P speciation with plant and soil processes2, and eventually to improve P use. Soil organic P is frequently extracted using NaOH/EDTA, followed by characterization of the extract by solution 31P-NMR. However, the obtained NMR spectra usually have poor resolution due to line broadening caused by the presence of paramagnetic ions. Therefore, we successfully developed an approach to avoid paramagnetic line broadening by precipitation of metal sulfides. Sulfide precipitation dramatically reduces NMR line widths for soil extracts, without affecting P-composition. The resulting highly improved resolution allowed us to apply for the first time 2D 1H,31P-NMR methods to identify different P monoesters in spectral regions which are extremely crowded in 1D NMR spectra.3 By exploiting 2D 1H-31P NMR spectra of soil extracts we were able to unambiguously identify individual organic P species by combining 31P and 1H chemical shifts and coupling constants. This approach is even suitable for a structural characterization of unknown P-components and for tracing degradation pathways between diesters and monoesters3,4.Currently we apply our approach on boreal4 and tropical soils with focus on Burkina Faso. In addition we also monitor P-species in aqueos ecosystems. For this purpose stream water from the Krycklan catchment in northern Sweden5 has been used to

  13. Overall structure and sugar dynamics of a DNA dodecamer from homo- and heteronuclear dipolar couplings and 31P chemical shift anisotropy

    The solution structure of d(CGCGAATTCGCG)2 has been determined on the basis of an exceptionally large set of residual dipolar couplings. In addition to the heteronuclear 13C-1H and 15N-1H and qualitative homonuclear 1H-1H dipolar couplings, previously measured in bicelle medium, more than 300 quantitative 1H-1H and 22 31P-1H dipolar restraints were obtained in liquid crystalline Pf1 medium, and 22 31P chemical shift anisotropy restraints. High quality DNA structures can be obtained solely on the basis of these new restraints, and these structures are in close agreement with those calculated previously on the basis of 13C-1H and 15N-1H dipolar couplings. In the newly calculated structures, 31P-1H dipolar and 3JsubH3'Psub couplings and 31P CSA data restrain the phosphodiester backbone torsion angles. The final structure represents a quite regular B-form helix with a modest bending of ∼10 deg., which is essentially independent of whether or not electrostatic terms are used in the calculation. Combined, the number of homo- and heteronuclear dipolar couplings significantly exceeds the number of degrees of freedom in the system. Results indicate that the dipolar coupling data cannot be fit by a single structure, but are compatible with the presence of rapid equilibria between C2'-endo and C3'-endo deoxyribose puckers (sugar switching). The C2'-H2'/H2'' dipolar couplings in B-form DNA are particularly sensitive to sugar pucker and yield the largest discrepancies when fit to a single structure. To resolve these discrepancies, we suggest a simplified dipolar coupling analysis that yields N/S equilibria for the ribose sugar puckers, which are in good agreement with previous analyses of NMR JHH couplings, with a population of the minor C3'-endo form higher for pyrimidines than for purines

  14. Accurate calculation of (31)P NMR chemical shifts in polyoxometalates.

    Pascual-Borràs, Magda; López, Xavier; Poblet, Josep M

    2015-04-14

    We search for the best density functional theory strategy for the determination of (31)P nuclear magnetic resonance (NMR) chemical shifts, δ((31)P), in polyoxometalates. Among the variables governing the quality of the quantum modelling, we tackle herein the influence of the functional and the basis set. The spin-orbit and solvent effects were routinely included. To do so we analysed the family of structures α-[P2W18-xMxO62](n-) with M = Mo(VI), V(V) or Nb(V); [P2W17O62(M'R)](n-) with M' = Sn(IV), Ge(IV) and Ru(II) and [PW12-xMxO40](n-) with M = Pd(IV), Nb(V) and Ti(IV). The main results suggest that, to date, the best procedure for the accurate calculation of δ((31)P) in polyoxometalates is the combination of TZP/PBE//TZ2P/OPBE (for NMR//optimization step). The hybrid functionals (PBE0, B3LYP) tested herein were applied to the NMR step, besides being more CPU-consuming, do not outperform pure GGA functionals. Although previous studies on (183)W NMR suggested that the use of very large basis sets like QZ4P were needed for geometry optimization, the present results indicate that TZ2P suffices if the functional is optimal. Moreover, scaling corrections were applied to the results providing low mean absolute errors below 1 ppm for δ((31)P), which is a step forward in order to confirm or predict chemical shifts in polyoxometalates. Finally, via a simplified molecular model, we establish how the small variations in δ((31)P) arise from energy changes in the occupied and virtual orbitals of the PO4 group. PMID:25738630

  15. COMPRESSION GARMENTS AND RECOVERY FROM ECCENTRIC EXERCISE: A 31P-MRS STUDY

    Michael I. Trenell

    2006-03-01

    Full Text Available The low oxidative demand and muscular adaptations accompanying eccentric exercise hold benefits for both healthy and clinical populations. Compression garments have been suggested to reduce muscle damage and maintain muscle function. This study investigated whether compression garments could benefit metabolic recovery from eccentric exercise. Following 30-min of downhill walking participants wore compression garments on one leg (COMP, the other leg was used as an internal, untreated control (CONT. The muscle metabolites phosphomonoester (PME, phosphodiester (PDE, phosphocreatine (PCr, inorganic phosphate (Pi and adenosine triphosphate (ATP were evaluated at baseline, 1-h and 48-h after eccentric exercise using 31P-magnetic resonance spectroscopy. Subjective reports of muscle soreness were recorded at all time points. The pressure of the garment against the thigh was assessed at 1-h and 48-h following exercise. There was a significant increase in perceived muscle soreness from baseline in both the control (CONT and compression (COMP leg at 1-h and 48-h following eccentric exercise (p < 0.05. Relative to baseline, both CONT and COMP showed reduced pH at 1-h (p < 0.05. There was no difference between CONT and COMP pH at 1-h. COMP legs exhibited significantly (p < 0.05 elevated skeletal muscle PDE 1-h following exercise. There was no significant change in PCr/Pi, Mg2+ or PME at any time point or between CONT and COMP legs. Eccentric exercise causes disruption of pH control in skeletal muscle but does not cause disruption to cellular control of free energy. Compression garments may alter potential indices of the repair processes accompanying structural damage to the skeletal muscle following eccentric exercise allowing a faster cellular repair

  16. Muscle metabolism of professional athletes using 31P-spectroscopy

    Purpose: The aim of the study was to examine muscle metabolism in athletes by 31P-spectroscopy (MRS) and to evaluate to what degree the respective resonance spectrum correlates with the kind of muscle exercise. Material and Methods: Twelve runners and 12 young ice skaters were studied by 31P-spectroscopy of the gastrocnemic medialis muscle and the vastus medialis muscle using a surface coil at 1.5 T. Results: Sprinters displayed a higher phosphocreatinine/inorganic phosphate (PCr/Pi) and PCr/β-ATP ratios than marathon runners. The respective parameters for middle distance runners were in between. Ice skaters could prospectively be divided into sprint- and long-distance runners by our results which correlated with the athletes' training performance. Conclusion: 31P-spectroscopy can evaluate the distribution of muscle fiber types. Thus, the athlete's potential for sprint- or long-distance running can be determined. Additional studies will have to demonstrate to what extent training may change muscle fiber distribution. (orig.)

  17. 77Se Chemical Shift Tensor of L-selenocystine: Experimental NMR Measurements and Quantum Chemical Investigations of Structural Effects

    Struppe, Jochem; Zhang, Yong; Rozovsky, Sharon

    2015-01-01

    The genetically encoded amino acid selenocysteine and its dimeric form, selenocystine, are both utilized by nature. They are found in active sites of selenoproteins, enzymes that facilitate a diverse range of reactions, including the detoxification of reactive oxygen species and regulation of redox pathways. Due to selenocysteine and selenocystine’s specialized biological roles, it is of interest to examine their 77Se NMR properties and how those can in turn be employed to study biological sy...

  18. Simultaneous tracing of 76Se-selenite and 77Se-selenomethionine by absolute labeling and speciation

    Nutritional selenocompounds are transformed into the assumed common intermediate selenide, which is utilized for the synthesis of selenoenzymes or transformed into methylated metabolites for excretion. Hence, selenocompound metabolites can be traced only with labeled selenium. Here we applied a new tracer method for the metallomics of biometals using simultaneous speciation of each metallome labeled with different homo-elemental isotopes to metabolism and availability of selenium. Rats were depleted of endogenous natural abundance selenium by feeding a single selenium stable isotope (82Se-selenite) and then administered 76Se-selenite and 77Se-selenomethionine (77Se-SeMet)simultaneously. Biological samples were subjected to quantification and speciation analysis by HPLC-ICPMS. Metabolites of the labeled 76Se and 77Se and interaction with endogenous selenium were traced and examined without interference from the corresponding endogenous natural abundance isotopes. Differences in the distribution and metabolism among organs and between the two nutritional selenocompounds were compared under exactly identical biological and analytical conditions: (1) selenite was distributed more efficiently than SeMet in organs and body fluids except the pancreas. (2) SeMet was taken up by organs in its intact form. (3) Selenium of SeMet origin was distributed selectively in the pancreas and mostly bound to a protein together with intact SeMet. (4) Selenosugars A and B but not trimethylselenonium (TMSe) were detected in the liver. (5) Selenosugar B and TMSe were detected in the kidneys

  19. 31P-NMR studies on perfused mouse liver

    From a metabolic viewpoint, the most important organ in the body is the liver. In contrast to more specialized organs such as heart and kidney which perform only one major function, the liver performs a number of major metabolic functions. Two of the most important functions are the catabolism and storage of foodstuffs (in the form of glycogen) and the control of most of the constituents of the blood (in particular, the blood glucose level). Most of these functions are localized within a single type of cell. One way that the liver is able to regulate these diverse reactions is by the control of the ATP level in the cell. Encouraged by the recent success of many groups in using 31P-NMR to provide a continuous and non-destructive monitor of ATP levels in isolated cells, skeletal muscle, and perfused organs such as heart and kidney, 31P-NMR was used to investigate ATP levels in perfused liver of mice

  20. Differential cross sections measurement of 31P(p,pγ1)31P reaction for PIGE applications

    Jokar, A.; Kakuee, O.; Lamehi-Rachti, M.

    2016-09-01

    Differential cross sections of proton induced gamma-ray emission from the 31P(p,pγ1)31P (Eγ = 1266 keV) nuclear reaction were measured in the proton energy range of 1886-3007 keV at the laboratory angle of 90°. For these measurements a thin Zn3P2 target evaporated onto a self-supporting C film was used. The gamma-rays and backscattered protons were detected simultaneously. An HPGe detector placed at an angle of 90° with respect to the beam direction was employed to collect gamma-rays while an ion implanted Si detector placed at a scattering angle of 165° was used to detect backscattered protons. Simultaneous collection of gamma-rays and RBS spectra is a great advantage of this approach which makes differential cross-section measurements independent on the collected beam charge. The obtained cross-sections were compared with the previously only measured data in the literature. The validity of the measured differential cross sections was verified through a thick target benchmarking experiment. The overall systematic uncertainty of cross section values was estimated to be better than ±9%.

  1. 31P-MR spectroscopic imaging in hypertensive heart disease

    Hypertensive heart disease (HHD) causes structural changes (e.g., fibrosis) that result in diastolic and systolic myocardial dysfunction. Alterations of 31P metabolism and cardiac energy impairments were assessed in patients with HHD by MR spectroscopy (MRS) and correlated with left ventricular systolic function. Thirty-six patients with HHD and 20 healthy controls (mean age 35.2±10.7 years) were examined with 31P-MRS at 1.5 T by using an ECG-gated CSI sequence. Twenty-five patients (mean age 64.3±9.3 years) had diastolic dysfunction, but preserved systolic function (HHD-D), whereas 11 patients (62.3±11.4 years) suffered from additional impaired systolic function (HHD-S). In both patient groups, the PCr/γ-ATP ratio was lower than in the controls (controls: 2.07±0.17; P<0.001), and in HHD-S was lower than in HHD-D (1.43±0.21 vs. 1.65±0.25; P=0.012). PCr/γ-ATP ratios were linearly correlated with LVEF (Pearson's r: 0.39; P=0.025). In the HHD-S group, the PDE/γ-ATP ratio was significantly lower (0.56±0.36) than in the controls (1.14±0.42; P=0.001). In contrast to the group of HHD-D patients, whose slightly decreased PCr/γ-ATP ratios compared to controls may be explained by age differences, the more distinct changes observed in HHD-S patients indicate an altered energy metabolism. The observed metabolic changes were related to functional impairments, as indicated by a reduced LVEF. Reduced PDE/ATP ratios indicate changes in the phospholipid metabolism. (orig.)

  2. 31P MR spectroscopic measurement of intracellular pH in normal human hearts

    To assess the usefulness of intracellular pH (pHi), calculated by determining the shift of a high-energy metabolite such as inorganic phosphate (Pi) of γ-ATP after performing MRS with ECG-gated two-dimensional 31P CSI (chemical shift imaging), as a parameter for the overall state of the intracellular milieu. Proto decoupled 31P CSI was performed on a 1.5-T scanner using a 1H31P dual-tuned surface coil. Cardiac MRS data were obtained from eight normal volunteers aged 24-32 years with no history of heart disease. From the spectra obtained from several regions of the heart, peack position and peak area were estimated. The metabolic ratios of α-, β-, γ-ATP, PCr, Pi, phosphodiester and diphosphoglycerate were calculated, and pHi was estimated from the chemical shift of Pi and γ-ATP resonance. We then compared the data for the anterior myocardium with those previously published. The major phosphorous metabolites identified in these human hearts were as follows: PCr, at -0.1 to +0.1 ppm; three phosphate peaks from ATP, with a chemical shift centered at about -2.7 ppm (γ-ATP), -7.8 ppm (α-ATP), and -16.3 ppm (β-ATP); and phosphodiester (PDE) at 2-3 ppm, inorganic phosphate (Pi) at 4.5-5.4 ppm, and diphosphoglycerate (DPG) at 5.4-6.3 ppm. The PCr/β-ATP ratio was 2.20±0.17 and the PDE/β-ATP ratio, 1.04±0.09 pHi readings were 7.31±0.23 (calculated by the shift of Pi) and 6.81±0.20 (calculated by the shift of γ-ATP). Pi/PCR was 0.539, a ratio higher than that mentioned in previously published reports. The measurement of intracellular metabolism was affected by various kinds of factors. We believe, however, that pHi readings indicate the overall state of the cardiac intracellular milieu. An unexpected pHi readings, seen at MRS, may reflect errors in the MR procedure itself and, or in the analytical method

  3. Etiology and functional status of liver cirrhosis by 31P MR spectroscopy

    Monika Dezortova; Pavel Taimr; Antonin Skoch; Julius Spicak; Milan Hajek

    2005-01-01

    AIM: To assess the functional status and etiology of liver cirrhosis by quantitative 31p magnetic resonance spectroscopy (MRS).METHODS: A total of 80 patients with liver cirrhosis of different etiology and functional status described by Child-Pugh score were examined and compared to 11 healthy volunteers. MR examination was performed on a 1.5 T imager using a 1H/31P surface coil by the 2D chemical shift imaging technique.Absolute concentrations of phosphomonoesters (PME),phosphodiesters (PDE), inorganic phosphate (Pi) and adenosine triphosphate (ATP) were measured.RESULTS: MRS changes reflected the degree of liver dysfunction in all the patients as well as in individual etiological groups. The most important change was a decrease of PDE. It was possible to distinguish alcoholic,viral and cholestatic etiologies based on MR spectra.Alcoholic and viral etiology differed in PDE (alcoholic,viral, controls: 6.5±2.3, 6.5±3.1, 10.8±2.7 mmol/L,P<0.001) and ATP (alcoholic, viral, controls: 2.9±0.8, 2.8±0.9, 3.7±1.0 mmol/L, P<0.01) from the control group.Unlike viral etiology, patients with alcoholic etiology also differed in Pi (alcoholic, controls: 1.2±0.4, 1.6±0.6mmol/L, P<0.05) from controls. No significant changes were found in patients with cholestatic disease and controls; nevertheless, this group differed from both alcoholic and viral groups (cholestatic, alcoholic, viral: 9.4±2.7, 6.5±2.3, 6.5±3.1 mmol/L, P<0.005) in PDE.CONCLUSION: 31p MRS can significantly help in noninvasive separation of different etiological groups leading to liver cirrhosis. In addition, MRS changes reflect functional liver injury.

  4. 31P MR spectroscopy of the liver showing dose dependent adenosine triphosphate decreases after radiation induced hepatic injury

    Objective: To study the relationship between ATP level changes detected by hepatic 31P MRS with the pathologic changes of liver in rabbits and to investigate the diagnostic value of ATP level changes in acute hepatic radiation injury. Methods: A total of 30 rabbits received different radiation doses (ranging from 5,10,20 Gy) to establish acute hepatic injury models. Blood hepatic function tests, 31P MRS and pathological examinations were carded out 24 h after irradiation. The degree of injury was evaluated according to hepatocyte pathology. Ten healthy rabbits served as controls. The MR examination was performed on a 1.5 T imager using a 1H-31P surface coil with 2D chemical shift imaging technique. The relative quantities of phosphomonoesters (PME), phosphodiesters (PDE), inorganic phosphate (Pi) and adenosine triphosphate (ATP) were measured. Analysis of variance was used to compare the results of 31P MRS and histopathology under various acute hepatic radiation injuries, and SNK was used further to conduct comparison between each other if there was significant difference. Results: The ATP relative quantification in control (n=10), mild (n=12), moderate (n=11), and severe (n=7) injury groups according to pathological grading were 1.83±0.33, 1.58±0.25, 1.32±0.07 and 1.02±0.18, with significant differences among them (F=22.878, P<0.01), and it decreased progressively with the increased degree of injury. The PDE index showed no significant trend for the evaluation of hepatic radiation injury. The area under the peak of β-ATP decreased with the increased severity of radiation injury. Conclusions: The relative quantification of hepatic ATP levels can reflect the pathological severity of acute hepatic radiation injury. The decreasing hepatic ATP levels may be used as biomarker of acute liver injury following radiation. (authors)

  5. Chiral trimethylsilylated C2-symmetrical diamines as phosphorous derivatizing agents for the determination of the enantiomeric excess of chiral alcohols by 1H NMR

    Alexakis Alexandre

    2006-03-01

    Full Text Available Abstract The use of organophosphorus derivatising agents, prepared from C2 symmetric trimethylsilylated diamines, for the 1H NMR and 31P NMR determination of the enantiomeric composition of chiral alcohols is described.

  6. 31P NMR spectroscopy measurements of hum ovarian carcinoma xenografts

    /sup 31/P NMR spectroscopy was used to study lipid and energy metabolism as well as tumour pH in three human ovarian carcinoma xenograft lines with widely differing growth rate, necrotic fraction and differentiation status. Two of the liines showed decreasing PCr (phosphocreatine) and NTPbhta (nucleoside triphosphates bhta) resonances and an increasing P/sub i/ (inorganic phosphate) resonance with increasing tumour volume in the volume range 100-4000 mm/sup 3/. This decrease in bioenergetic status was accompanied by a decrease in tumour pH from about 7.15 to about 6.95. The volume-dependence of these spectral parametes probably reflected increased nutritional deprivation and development of hypoxia and necrosis during tumour growth. The third xenograft line did not show changes in the intensity of any of the resonances during tumour growth. The spectral parameters differed significantly among the xenograft lines at given tumour volumes, but no correlations with volume-doubling time, necrotic fraction of differentiation status were found

  7. Application of 31P MR spectroscopy to the brain tumors

    To evaluate the clinical feasibility and obtain useful parameters of 31P magnetic resonance spectroscopy (MRS) study for making the differential diagnosis of brain tumors. Twenty-eight patients with brain tumorous lesions (22 cases of brain tumor and 6 cases of abscess) and 11 normal volunteers were included. The patients were classified into the astrocytoma group, lymphoma group, metastasis group and the abscess group. We obtained the intracellular pH and the metabolite ratios of phosphomonoesters/phosophodiesters (PME/PDE), PME/inorganic phosphate (Pi), PDE/Pi, PME/adenosine triphosphate (ATP), PDE/ATP, PME/phosphocreatine (PCr), PDE/PCr, PCr/ATP, PCr/Pi, and ATP/Pi, and evaluated the statistical significances. The brain tumors had a tendency of alkalization (pH = 7.28 ± 0.27, p = 0.090), especially the pH of the lymphoma was significantly increased (pH = 7.45 ± 0.32, p = 0.013). The brain tumor group showed increased PME/PDE ratio compared with that in the normal control group (p 0.012). The ratios of PME/PDE, PDE/Pi, PME/PCr and PDE/PCr showed statistically significant differences between each brain lesion groups (p 1'P MRS, and the pH, PME/PDE, PDE/Pi, PME/PCr, and PDE/PCr ratios are helpful for differentiating among the different types of brain tumors.

  8. Solid-state 31P NMR spectroscopy of bacteriophage M13 and tobacco mosaic virus.

    Magusin, P.C.M.M.

    1995-01-01

    In this thesis, the results of various 31P NMR experiments observed for intact virus particles of bacteriophage M13 and Tobacco Mosaic Virus (TMV), are presented. To explain the results in a consistent way, models are developed and tested. 31P nuclei in M13 and TMV are only present in the phosphodiesters of the encapsulated nucleic acid molecule. Therefore, 31P NMR spectroscopy reveals structural and dynamic properties of the nucleic acid backbone selectively without isotope labeling, even th...

  9. Kinetics of the in vivo31P 1H nuclear overhauser effect of the human-calf-muscle phosphocreatine resonance

    Bachert, Peter; Bellemann, Matthias E.

    In 31P 1H double-resonance experiments in a 1.5 T whole-body MR system, we observed in vivo the truncated driven, transient, and steady-state 31P- 1H nuclear Overhauser effect of the phosphocreatine resonance in 31P MR spectra of human gastrocnemius muscle. Maximum signal enhancements of 0.52 ± 0.01, 0.20 ± 0.01, and 0.79 ± 0.02 were measured, respectively. Fitting the data with theoretical functions which solve the multispin Solomon equations for N protons (S spins) dipolar coupled to a 31P nucleus (I spin) yields cross-relaxation times {2}/{[Σ i=1-N σIS(i) ] } in the order of 20 s. In vivo experiments are feasible for studying relaxation mechanisms in coupled 31P 1H spin systems in intact tissue.

  10. Nematicity and in-plane anisotropy of superconductivity in β -FeSe detected by 77Se nuclear magnetic resonance

    Baek, S.-H.; Efremov, D. V.; Ok, J. M.; Kim, J. S.; van den Brink, Jeroen; Büchner, B.

    2016-05-01

    The recent study of 77Se nuclear magnetic resonance (NMR) in a β -FeSe single crystal proposed that ferro-orbital order breaks the 90∘ C4 rotational symmetry, driving nematic ordering. Here, we report an NMR study of the impact of small strains generated by gluing on nematic state and spin fluctuations. We observe that the local strains strongly affect the nematic transition, considerably enhancing its onset temperature. On the contrary, no effect on low-energy spin fluctuations was found. Furthermore we investigate the interplay of the nematic phase and superconductivity. Our study demonstrates that the twinned nematic domains respond unequivalently to superconductivity, evidencing the twofold C2 symmetry of superconductivity in this material. The obtained results are well understood in terms of the proposed ferro-orbital order.

  11. Determination of absolute concentrations of cardiac high-energy phosphates using 31P-MR-spectroscopy and SLOOP in healthy and diseased myocardium

    Purpose: A quantitative 31P-MR-spectroscopic technique was used to assess the energy metabolism in healthy and diseased myocardium. Methods: 31P-spectra were acquired on a 1.5 T scanner using a 3D-chemical shift imaging technique. Based on the anatomical information provided by 1H-images, SLOOP (Spatial Localization with Optimal Pointspread Function) allows to obtain spectra from defined compartments. With SLOOP a free voxel shape with adaption to anatomic structures, e.g. the myocardium, is possible. Absolute values for phosphocreatine (PCr) and adenosine triphosphate (ATP) were determined using an external standard. Results: 31P-spectra showed only minimal contamination by surrounding tissue. The standard deviation for the determined values of healthy volunteers was low. Compared to healthy volunteers, reduced PCr and ATP concentrations were seen for dilative cardiomyopathies and coronary artery disease and unchanged concentrations were observed for hypertensive heart disease. Conclusion: 31P-MR-spectroscopy with SLOOP allows a non-invasive, quantitative analysis of cardiac energy metabolism. (orig.)

  12. Metabolism of perfused pig intercostal muscles evaluated by 31P-magnetic resonance spectroscopy

    Pedersen, Brian Lindegaard; Arendrup, Henrik; Secher, Niels H;

    2006-01-01

    consumption and 31P-magnetic resonance spectroscopy (31P-MRS). When perfused at rest with Krebs-Ringer buffer, the preparation maintained physiological levels of phosphocreatine (PCr), inorganic phosphate (Pi), ATP and pH at a stable oxygen consumption of 0.51 +/- 0.01 micromol min(-1) g(-1) for more than 2 h...

  13. 肝脏31P-MR波谱成像的临床应用%Clinical Applications of Hepatic 31P-MR Spectrocscopy

    吴苾; 宋彬; 杨洋

    2005-01-01

    目的总结磁共振31磷波谱成像(31phosphorus MR spectroscopy, 31P-MRS)的原理及在肝脏疾病诊断中的临床应用. 方法回顾分析国内、外应用31P-MRS诊断肝脏疾病的文献. 结果在肝炎、肝硬变、肝脏肿瘤、肝移植术后及梗阻性黄疸等各种肝脏疾病患者中,31P-MR波谱出现异常,评价31P-MR波谱对疾病的诊治有重要临床意义. 结论 31P-MRS作为一种研究活体肝脏细胞水平的能量代谢和生化指标变化的非侵入检查方法,正得到越来越广泛的临床应用.

  14. Estudo do metabolismo energético muscular em atletas por 31P-ERM Muscular energetic metabolism study in athletes by 31P-MRS

    Maria Gisele dos Santos; Jose Manuel González de Suso; Angel Moreno; Miquel Cabanas; Carles Arus

    2004-01-01

    OBJETIVO: Caracterizar as reservas energéticas de metabólitos fosforilados no músculo esquelético de atletas mediante 31P-ERM. MÉTODOS: Amostra deste estudo foi formada por 14 atletas de alto nível do Centro de Alto Rendimento Esportivo (CAR, Sant Cugat del Vallés, Espanha). O padrão de metabólitos fosforilados foi medido no músculo vasto medial por 31P-ERM. A suplementação oral foi realizada durante 14 dias, na forma de 20g de monohidrato de creatina. Os atletas foram determinados conforme a...

  15. Investigation of sea microorganisms of the genus Alteromonas by 31P-NMR of high resolution

    Comparative analysis of the 31P-NMR spectra of intact cells of bacteria belonging to the genus Alteromonas, the producers of alkaline phosphatase was carried out. Differences in the content of phosphate-containing compounds were detected in individual species of the genus Alteromonas. By comparing the data on 31P-NMR spectra, the electron micrographs and phosphatase activities, the possibility of revealing the presence of capsules was shown. Peculiar features of the 31P-NMR spectra of alteromonades, as compared with other taxonomic groups of microorganisms, have been discussed

  16. Electron-photon angular correlations in electron-helium collisions for 31P excitations

    Electron-photon angular correlations have been measured by detecting, in delayed coincidence, electrons inelastically scattered from helium and photons emitted in decays from the 31P level. The measurements have been carried out using both the 31P-11S (53.7nm) line and the 31P-21S (501.6nm) line. Analysis of the data yields the ratio of differential cross sections for exciting 31P magnetic sublevels and the absolute value of the relative phase between the corresponding excitation amplitudes for electron scattering angles between 100 and 300 at incident electron energies in the range 50 eV to 150 eV. Data of the atomic orientation is also presented. The results are compared with the predictions of the first Born approximation and a recent multichannel eikonal calculation. (author)

  17. 31P NMR study of phosphate metabolites in intact developing seeds of wheat, soybean and mustard

    The study of 31P NMR spectra of intact developing seeds of wheat, soybean and mustard and its possible use for assessing the relative degree of hypoxia under in vivo conditions are reported. 7 refs., 2 figs

  18. Feasibility of Rapid-Sequence 31P Magnetic Resonance Spectroscopy in Cardiac Patients

    Purpose: To determine the clinical feasibility of rapid-sequence phosphorus-31 magnetic resonance spectroscopy (31P -MRS) of the heart with cardiac patients using a 5T clinical MR system. Material and Methods: Twenty cardiac patients, i.e. dilated cardiomyopathy (DCM)3 cases, hypertrophic cardiomyopathy (HCM) 3 cases, hypertensive heart diseases (HHD) 3 cases, and aortic regurgitation (AR) case were examined using rapid cardiac 31P-MRS. Complete three-dimensional localization was performed using a two-dimensional phosphorus chemical-shift imaging sequence in combination with 30-mm axial slice-selective excitation. The rapid-sequence 31P-MRS procedure was phase encoded in arrays of 8x8 steps with an average of 4 acquisitions. The total examination time, including proton imaging and shimming, for the rapid cardiac 31P-MRS procedure, ranged from 0 to 5 min, depending on the heart rate. Student's t test was used to compare creatine phosphate (PCr)/adenosine triphosphate (ATP) ratios from the cardiac patients with those of the control subjects (n≅13). Results: The myocardial PCr/ATP ratio obtained by rapid 31P-MRS was significantly lower (P 31P-MRS may be a valid diagnostic tool for patients with cardiac disease

  19. Clinical evaluation of the cerebral energy metabolism with 31P chemical shift imaging in neurosurgical disorders

    Cerebral energy metabolism was evaluated by means of 31P chemical shift imaging (CSI) using the 2.0 T whole-body MRIS system. 31P CSI was carried out by means of Spectroscopic Imaging by Dephasing Amplitude Changing method, four-dimensional CSI, and three-dimensional CSI. Twenty three patients with cerebral infarction and 21 patients with hypertensive intracerebral hemorrhage were examined. In cerebral infarction, an acute infarction was seen as a low-signal area in the PCr and ATP images and as a high-signal area in the Pi image. A subacute and chronic infarction was seen as a low-signal area in all the images -- 31P, PCr, ATP, Pi, PDE and PME. Intracellular acidosis was noticed within 2 days after onset. The intracellular pH became alkaline at the subacute and chronic stages of infarction. The chronological changes in the phosphorus metabolites were evaluated by means of these methods. In hypertensive intracerebral hemorrhage, hematoma and perifocal edema in the acute stage were seen as low-signal areas in the 31P, PCr, and ATP images, and as high-signal areas in the Pi image. In the chronic stage, a hematoma was seen as a low-signal area in all the images -- 31P, PCr, ATP and Pi. 31P CSI is thus a practical tool for studying phosphate metabolites clinically. Changes in the phosphorus metabolism relative to the anatomy of interest were detected by the use of these methods. (author)

  20. Phosphole complexes of Gold(I) halides: Comparison of solution and solid-state structures by a combination of solution and CP/MAS 31P NMR spectroscopy and x-ray crystallography

    A series of complexes of 1-phenyldibenzophosphole (DBP), 1-phenyl-3,4,-dimethylphosphole (DMPP), and triphenylphosphine of the type LnAuX (n = 1, L = DBP, DMPP, Ph3P, X = Cl, Br, I; n = 3, L = DBP, X = Cl, Br, I; n = 3, L = Ph3P, X = Cl; n = 4, L = DBP, DMPP, X = PF6) have been prepared and characterized. The structures of (DBP)AuCl (1), (DBP)3AuCl (2), and (DMPP)AuCl (3) have been determined from three-dimensional x-ray data collected by counter methods. Crystal structure of the complexes is reported. The CP/MAS 31P(1H) NMR spectrum of complex 1 shows two resonances in a 1:1 intensity ratio, and the CP/MAS 31P(1H) NMR spectrum of complex 3 shows three resonances in a 1:1:1 intensity ratio for reasons that are not yet understood. Though the three phospholes are crystallographically inequivalent (d(AuP) = 2.359 (1), 2.382 (1), and 2.374 (2) angstrom) the molecule has effective Cs symmetry as evidenced by the observation of two 31P resonances in a 2:1 intensity ratio in its CP/MAS 31P(1H) NMR spectrum. Variable-temperature 31P(1H) NMR spectra obtained on solutions of LAuCl + L in various ratios were analyzed to determine the nature of the species present in solution and to gain information regarding their relative stabilities as a function of the nature of the phosphine. 79 refs., 8 figs., 9 tabs

  1. Biochemical metabolic changes assessed by 31P magnetic resonance spectroscopy after radiation-induced hepatic injury in rabbits

    Ri-Sheng Yu; Liang Hao; Fei Dong; Jian-Shan Mao; Jian-Zhong Sun; Ying Chen; Min Lin; Zhi-Kang Wang; Wen-Hong Ding

    2009-01-01

    AIM:To compare the features of biochemical metabolic changes detected by hepatic phosphorus-31 magnetic resonance spectroscopy (31P MRS) with the liver damage score (LDS) and pathologic changes in rabbits and to investigate the diagnostic value of 31P MRS in acute hepatic radiation injury.METHODS:A total of 30 rabbits received different radiation doses (ranging 5-20 Gy) to establish acute hepatic injury models.Blood biochemical tests,31P MRS and pathological examinations were carried out 24 h after irradiation.The degree of injury was evaluated according to LDS and pathology.Ten healthy rabbits served as controls.The MR examination was performed on a 1.5 T imager using a 1H/31P surface coil by the 2D chemical shift imaging technique.The relative quantities of phosphomonoesters (PME),phosphodiesters (PDE),inorganic phosphate (Pi) and adenosine triphosphate (ATP) were measured.The data were statistically analyzed.RESULTS:(1) Relative quantification of phosphorus metabolites:(a) ATP:there were significant differences (P<0.05) (LDS-groups:control group vs mild group vs moderate group vs severe group,1.83±0.33 vs 1.55±0.24 vs 1.27±0.09 vs 0.98±0.18;pathological groups:control group vs mild group vs moderate group vs severe group,1.83±0.33 vs 1.58±0.25 vs 1.32±0.07 vs 1.02 ± 0.18) of ATP relative quantification among control group,mild injured group,moderate injured group,and severe injured group according to both LDS grading and pathological grading,respectively,and it decreased progressively with the increased degree of injury (r=-0.723,P=0.000).(b) PME and Pi;the relative quantification of PME and Pi decreased significantly in the severe injured group,and the difference between the control group and severe injured group was significant (P<0.05) (PME:LDScontrol group vs LDS-severe group,0.86±0.23 vs 0.58±0.22,P=0.031;pathological control group vs pathological severe group,0.86±0.23 vs 0.60±0.21,P=0.037;Pi:LDS-control group vs LDS-severe group,0.74±0.18 vs

  2. Availability and metabolism of 77Se-methylseleninic acid compared simultaneously with those of three related selenocompounds

    Nutritional selenocompounds are considered to be transformed into the common intermediate selenide for utilization as selenoenzymes and/or for excretion as selenosugar and trimethylselenonium (TMSe). Therefore, selenocompounds can only be traced with a labeled selenium atom. Methylseleninic (MSAIV) has been proposed to be a third nutritional selenium source, the other two being inorganic selenocompounds and organic selenoamino acids, and to be a proximate selenochemical for producing the assumed biologically active form methylselenol. Here we applied a new tracer method to compare the availability and metabolism of MSAIV with those of three related selenocompounds under exactly identical host and tracing conditions. 82Se-Selenite, 78Se-selenate, 77Se-MSAIV and 76Se-methylselenonic acids (MSAVI) were simultaneously administered orally, each at the dose of 25 μg Se/kg body weight, to rats that had been depleted of endogenous natural abundance selenium with a single stable isotope (8Se). Time-related changes in the concentrations and/or distributions of the four labeled isotopes in the serum, liver, kidney, pancreas, lung and urine were determined simultaneously by inductively coupled argon plasma mass spectrometry (ICP MS) and/or HPLC-ICP MS. The availability with different isotope ratios was in the decreasing order of selenate > selenite = MSAIV > MSAVI. Although selenate and MSAVI were distributed in organs and urine partly in their intact forms, MSAIV and selenite were not detected in the intact forms at all. MSAIV and MSAVI but not selenite or selenate produced TMSe in organs other than the liver, suggesting the transformation of MSAIV into methylselenol, and then either into selenide for the synthesis of selenoproteins and selenosugar or directly into TMSe. Thus, selenosugar and TMSe were produced widely in the organs. However, TMSe was not detected in the liver. The organ- and selenium source-specific production of TMSe was discussed as to the differences in

  3. Advancement of 31P Magnetic Resonance Spectroscopy Using GRAPPA Reconstruction on a 3D Volume

    Clevenger, Tony

    The overall objective of this research is to improve currently available metabolic imaging techniques for clinical use in monitoring and predicting treatment response to radiation therapy in liver cancer. Liver metabolism correlates with inflammatory and neoplastic liver diseases, which alter the intracellular concentration of phosphorus- 31 (31P) metabolites [1]. It is assumed that such metabolic changes occur prior to physical changes of the tissue. Therefore, information on regional changes of 31P metabolites in the liver, obtained by Magnetic Resonance Spectroscopic Imaging (MRSI) [1,2], can help in diagnosis and follow-up of various liver diseases. Specifically, there appears to be an immediate need of this technology for both the assessment of tumor response in patients with Hepatocellular Carcinoma (HCC) treated with Stereotactic Body Radiation Therapy (SBRT) [3--5], as well as assessment of radiation toxicity, which can result in worsening liver dysfunction [6]. Pilot data from our lab has shown that 31P MRSI has the potential to identify treatment response five months sooner than conventional methods [7], and to assess the biological response of liver tissue to radiation 24 hours post radiation therapy [8]. While this data is very promising, commonly occurring drawbacks for 31P MRSI are patient discomfort due to long scan times and prone positioning within the scanner, as well as reduced data quality due to patient motion and respiration. To further advance the full potential of 31P MRSI as a clinical diagnostic tool in the management of liver cancer, this PhD research project had the following aims: I) Reduce the long acquisition time of 3D 31P MRS by formulating and imple- menting an appropriate GRAPPA undersampling scheme and reconstruction on a clinical MRI scanner II) Testing and quantitative validation of GRAPPA reconstruction on 3D 31P MRSI on developmental phantoms and healthy volunteers At completion, this work should considerably advance 31P MRSI

  4. Use of enriched 74Se and 77Se in combination with isotope pattern deconvolution to differentiate and determine endogenous and supplemented selenium in lactating rats

    A quantitative methodology has been developed to differentiate between endogenous and supplemented selenium in lactating rats using two enriched selenium isotopes. Lactating rats were fed for 2 weeks with formula milk containing one enriched Se isotope, 77Se, as the metabolic tracer. The isotopic composition of selenium in serum and urine samples was then measured by collision cell ICP-MS after the addition of a solution containing another enriched isotope, 74Se, as quantitation tracer, before analysis. Isotope pattern deconvolution allowed the transformation of measured Se isotopic abundances into concentrations of natural abundance (endogenous) selenium and enriched 77Se (supplemented) present in the samples. The proposed methodology was validated using serum and urine reference materials spiked with both 77Se and 74Se. The obtained results are discussed in terms of selenium exchange and half-life in lactating rats (11-12 days) and selenium levels in serum in comparison with non-supplemented rats and control rats after maternal feeding. (orig.)

  5. Use of enriched {sup 74}Se and {sup 77}Se in combination with isotope pattern deconvolution to differentiate and determine endogenous and supplemented selenium in lactating rats

    Gonzalez Iglesias, H.; Fernandez Sanchez, M.L.; Garcia Alonso, J.I.; Sanz-Medel, A. [University of Oviedo, Department of Physical and Analytical Chemistry, Faculty of Chemistry, Oviedo (Spain)

    2007-10-15

    A quantitative methodology has been developed to differentiate between endogenous and supplemented selenium in lactating rats using two enriched selenium isotopes. Lactating rats were fed for 2 weeks with formula milk containing one enriched Se isotope, {sup 77}Se, as the metabolic tracer. The isotopic composition of selenium in serum and urine samples was then measured by collision cell ICP-MS after the addition of a solution containing another enriched isotope, {sup 74}Se, as quantitation tracer, before analysis. Isotope pattern deconvolution allowed the transformation of measured Se isotopic abundances into concentrations of natural abundance (endogenous) selenium and enriched {sup 77}Se (supplemented) present in the samples. The proposed methodology was validated using serum and urine reference materials spiked with both {sup 77}Se and {sup 74}Se. The obtained results are discussed in terms of selenium exchange and half-life in lactating rats (11-12 days) and selenium levels in serum in comparison with non-supplemented rats and control rats after maternal feeding. (orig.)

  6. Monitoring of the insecticide trichlorfon by phosphorus-31 nuclear magnetic resonance (31P NMR) spectroscopy

    Trichlorfon is an organophosphorus insecticide, which is extensively being used for protection of fruit crops. Trichlorfon is a thermal labile compound, which cannot be easily determined by gas chromatography (GC) and has no suitable group for sensitive detection by high performance liquid chromatography (HPLC). In this study, a 31P nuclear magnetic resonance (31P NMR) has been described for monitoring of trichlorfon without any separation step. The quantitative works of 31P NMR spectroscopy has been performed in the presence of an internal standard (hexamethylphosphoramide). Limit of detection (LOD) for this method has been found to be 55 mg L-1, without any sample preparation, and the linear working range was 150-5500 mg L-1. Relative standard deviation (R.S.D.%) of the method for three replicates within and between days was obtained ≤9%. The average recovery efficiency was approximately 99-112%. This method was applied for monitoring trichlorfon in a commercial insecticide sample and tomato sample

  7. 31P-MRS of skeletal muscle is not a sensitive diagnostic test for mitochondrial myopathy

    Jeppesen, Tina Dysgaard; Quistorff, Bjørn; Wibrand, Flemming;

    2007-01-01

    Clinical phenotypes of persons with mitochondrial DNA (mtDNA) mutations vary considerably. Therefore, diagnosing mitochondrial myopathy (MM) patients can be challenging and warrants diagnostic guidelines. (31)phosphorous magnetic resonance spectroscopy ((31)P-MRS) have been included as a minor...... investigated for the following: 1) (31)P-MRS of lower arm and leg muscles before and after exercise, 2) resting and peak-exercise induced increases of plasma lactate, 3) muscle morphology and -mitochondrial enzyme activity, 4) maximal oxygen uptake (VO(2max)), 5) venous oxygen desaturation during handgrip...... impaired citrate synthase-corrected complex I activity. Resting PCr/P(i) ratio and leg P(i) recovery were lower in MM patients vs. healthy subjects. PCr and ATP production after exercise were similar in patients and healthy subjects. Although the specificity for MM of some (31)P-MRS variables was as high...

  8. 脑肿瘤31P MRS研究进展

    吴光耀; 孙骏谟; 雷皓

    2004-01-01

    31P MRS(Phosphours-31 MR Spectroscopy),可以非损伤性地动态检测到生物体内多种含磷代谢物,反应脑肿瘤和肿瘤治疗过程中磷脂代谢、能量代谢和细胞内pH值的变化.本文阐述了含磷代谢物的生物学意义,脑肿瘤活体和离体31P MRS的变化特征和研究进展,31P MRS在脑肿瘤疗效监测中的价值.

  9. A comparison of MR elastography and 31P MR spectroscopy with histological staging of liver fibrosis

    Conventional imaging techniques are insensitive to liver fibrosis. This study assesses the diagnostic accuracy of MR elastography (MRE) stiffness values and the ratio of phosphomonoesters (PME)/phosphodiesters (PDE) measured using 31P spectroscopy against histological fibrosis staging. The local research ethics committee approved this prospective, blinded study. A total of 77 consecutive patients (55 male, aged 49 ± 11.5 years) with a clinical suspicion of liver fibrosis underwent an MR examination with a liver biopsy later the same day. Patients underwent MRE and 31P spectroscopy on a 1.5 T whole body system. The liver biopsies were staged using an Ishak score for chronic hepatitis or a modified NAS fibrosis score for fatty liver disease. MRE increased with and was positively associated with fibrosis stage (Spearman's rank = 0.622, P 31P MR spectroscopy and fibrosis stage. circle Magnetic resonance elastography (MRE) and MR spectroscopy can both assess the liver. (orig.)

  10. GC-ICP-MS determination of dimethylselenide in human breath after ingestion of (77)Se-enriched selenite: monitoring of in-vivo methylation of selenium.

    Kremer, Daniel; Ilgen, Gunter; Feldmann, Jörg

    2005-10-01

    The amount of volatile dimethylselenide (DMSe) in breath has been monitored after ingestion of sub-toxic amounts of selenium (300 microg (77)Se, as selenite) by a healthy male volunteer. The breath samples were collected in Tedlar bags every hour in the first 12 h and then at longer intervals for the next 10 days. The samples were subjected to speciation analysis for volatile selenium compounds by use of cryotrapping-cryofocussing-GC-ICP-MS. Simultaneously, all urine was collected and subjected to total selenium determination by use of ICP-MS. By monitoring m/z 82 and 77, background or dietary selenium and selenium from the administered selenite were simultaneously determined in the urine and in the breath-dietary selenium only was measured by monitoring m/z 82 whereas the amount of spiked (77)Se (99.1% [enriched spike]) and naturally occurring selenium (7.6% [natural abundance]) were measured by monitoring m/z 77. Quantification of DMSe was performed by using DMSe gas samples prepared in Tedlar bags (linear range 10-300 pg, R (2)=0.996, detection limit of Se as DMSe was 10 pg Se, or 0.02 ng L(-1), when 0.5 L gas was collected). Dimethylselenide was the only selenium species detected in breath samples before and after the ingestion of (77)Se-enriched selenite. Additional DM(77)Se was identified as early as 15 min after ingestion of the isotopically-labelled selenite. Although the maximum concentration of (77)Se in DMSe was recorded 90 min after ingestion, the natural isotope ratio for selenium in DMSe (77/82) was not reached after 20 days. The concentration of DMSe correlated with the total Se concentration in the urine during the experiment (R (2)=0.80). Furthermore, the sub-toxic dose of 300 microg selenium led to a significant increase of DMSe and renal excretion of background selenium, confirming that selenium ingested as selenite is homeostatically controlled by excretion. The maximum concentration of DMSe resulting from the spiked selenite was 1.4 ng Se L(-1

  11. GC-ICP-MS determination of dimethylselenide in human breath after ingestion of {sup 77}Se-enriched selenite: monitoring of in-vivo methylation of selenium

    Kremer, Daniel [University of Aberdeen, Department of Chemistry, College of Physical Sciences, Aberdeen, Scotland (United Kingdom); Johannes Gutenberg University Mainz, Environmental Geochemistry, Mainz (Germany); Ilgen, Gunter [University of Bayreuth, Central Analytics, Bayreuth Center for Ecology and Environmental Research (BayCEER), Bayreuth (Germany); Feldmann, Joerg [University of Aberdeen, Department of Chemistry, College of Physical Sciences, Aberdeen, Scotland (United Kingdom)

    2005-10-01

    The amount of volatile dimethylselenide (DMSe) in breath has been monitored after ingestion of sub-toxic amounts of selenium (300 {mu}g {sup 77}Se, as selenite) by a healthy male volunteer. The breath samples were collected in Tedlar bags every hour in the first 12 h and then at longer intervals for the next 10 days. The samples were subjected to speciation analysis for volatile selenium compounds by use of cryotrapping-cryofocussing-GC-ICP-MS. Simultaneously, all urine was collected and subjected to total selenium determination by use of ICP-MS. By monitoring m/z 82 and 77, background or dietary selenium and selenium from the administered selenite were simultaneously determined in the urine and in the breath - dietary selenium only was measured by monitoring m/z 82 whereas the amount of spiked {sup 77}Se (99.1% [enriched spike]) and naturally occurring selenium (7.6% [natural abundance]) were measured by monitoring m/z 77. Quantification of DMSe was performed by using DMSe gas samples prepared in Tedlar bags (linear range 10-300 pg, R {sup 2}=0.996, detection limit of Se as DMSe was 10 pg Se, or 0.02 ng L{sup -1}, when 0.5 L gas was collected). Dimethylselenide was the only selenium species detected in breath samples before and after the ingestion of {sup 77}Se-enriched selenite. Additional DM{sup 77}Se was identified as early as 15 min after ingestion of the isotopically-labelled selenite. Although the maximum concentration of {sup 77}Se in DMSe was recorded 90 min after ingestion, the natural isotope ratio for selenium in DMSe (77/82) was not reached after 20 days. The concentration of DMSe correlated with the total Se concentration in the urine during the experiment (R {sup 2}=0.80). Furthermore, the sub-toxic dose of 300 {mu}g selenium led to a significant increase of DMSe and renal excretion of background selenium, confirming that selenium ingested as selenite is homeostatically controlled by excretion. The maximum concentration of DMSe resulting from the

  12. Feasibility of Rapid-Sequence {sup 31}P Magnetic Resonance Spectroscopy in Cardiac Patients

    Chida, K.; Otani, H.; Saito, H.; Nagasaka, T.; Kagaya, Y.; Kohzuki, M.; Zuguchi, M.; Shirato, K. [Tohoku Univ., School of Health Sciences, Sendai (Japan). Dept. of Radiological Technology

    2005-07-01

    Purpose: To determine the clinical feasibility of rapid-sequence phosphorus-31 magnetic resonance spectroscopy ({sup 31}P -MRS) of the heart with cardiac patients using a 5T clinical MR system. Material and Methods: Twenty cardiac patients, i.e. dilated cardiomyopathy (DCM)3 cases, hypertrophic cardiomyopathy (HCM) 3 cases, hypertensive heart diseases (HHD) 3 cases, and aortic regurgitation (AR) case were examined using rapid cardiac {sup 31}P-MRS. Complete three-dimensional localization was performed using a two-dimensional phosphorus chemical-shift imaging sequence in combination with 30-mm axial slice-selective excitation. The rapid-sequence {sup 31}P-MRS procedure was phase encoded in arrays of 8x8 steps with an average of 4 acquisitions. The total examination time, including proton imaging and shimming, for the rapid cardiac {sup 31}P-MRS procedure, ranged from 0 to 5 min, depending on the heart rate. Student's t test was used to compare creatine phosphate (PCr)/adenosine triphosphate (ATP) ratios from the cardiac patients with those of the control subjects (n{approx_equal}13). Results: The myocardial PCr/ATP ratio obtained by rapid {sup 31}P-MRS was significantly lower (P <0.001) in DCM patients (1.82{+-}0.33, mean{+-}SD), and in patients with global myocardial dysfunction (combined data for 20 patients:.89{+-}0.32) than in normal volunteers (2.96{+-}0.59). These results are similar to previous studies. Conclusion: Rapid-sequence {sup 31}P-MRS may be a valid diagnostic tool for patients with cardiac disease.

  13. Phosphatidylcholine contributes to in vivo 31P MRS signal from the human liver

    To demonstrate the overlap of the hepatic and bile phosphorus (31P) magnetic resonance (MR) spectra and provide evidence of phosphatidylcholine (PtdC) contribution to the in vivo hepatic 31P MRS phosphodiester (PDE) signal, suggested in previous reports to be phosphoenolpyruvate (PEP). Phantom measurements to assess the chemical shifts of PEP and PtdC signals were performed at 7 T. A retrospective analysis of hepatic 3D 31P MR spectroscopic imaging (MRSI) data from 18 and five volunteers at 3 T and 7 T, respectively, was performed. Axial images were inspected for the presence of gallbladder, and PDE signals in representative spectra were quantified. Phantom experiments demonstrated the strong pH-dependence of the PEP chemical shift and proved the overlap of PtdC and PEP (∝2 ppm relative to phosphocreatine) at hepatic pH. Gallbladder was covered in seven of 23 in vivo 3D-MRSI datasets. The PDEgall/γ-ATPliver ratio was 4.8-fold higher (p = 0.001) in the gallbladder (PDEgall/γ-ATPliver = 3.61 ± 0.79) than in the liver (PDEliver/γ-ATPliver = 0.75 ± 0.15). In vivo 7 T 31P MRSI allowed good separation of PDE components. The gallbladder is a strong source of contamination in adjacent 31P MR hepatic spectra due to biliary phosphatidylcholine. In vivo 31P MR hepatic signal at 2.06 ppm may represent both phosphatidylcholine and phosphoenolpyruvate, with a higher phosphatidylcholine contribution due to its higher concentration. (orig.)

  14. Phosphatidylcholine contributes to in vivo {sup 31}P MRS signal from the human liver

    Chmelik, Marek; Bogner, Wolfgang; Gajdosik, Martin; Gruber, Stephan; Trattnig, Siegfried [Medical University of Vienna, MR Centre of Excellence, Department of Biomedical Imaging and Image-guided Therapy, Vienna (Austria); Valkovic, Ladislav [Medical University of Vienna, MR Centre of Excellence, Department of Biomedical Imaging and Image-guided Therapy, Vienna (Austria); Institute of Measurement Science, Slovak Academy of Sciences, Department of Imaging Methods, Bratislava (Slovakia); Wolf, Peter; Krebs, Michael [Medical University of Vienna, Division of Endocrinology and Metabolism, Department of Internal Medicine III, Vienna (Austria); Halilbasic, Emina; Trauner, Michael [Medical University of Vienna, Division of Gastroenterology and Hepatology, Department of Internal Medicine III, Vienna (Austria); Krssak, Martin [Medical University of Vienna, MR Centre of Excellence, Department of Biomedical Imaging and Image-guided Therapy, Vienna (Austria); Medical University of Vienna, Division of Endocrinology and Metabolism, Department of Internal Medicine III, Vienna (Austria)

    2015-07-15

    To demonstrate the overlap of the hepatic and bile phosphorus ({sup 31}P) magnetic resonance (MR) spectra and provide evidence of phosphatidylcholine (PtdC) contribution to the in vivo hepatic {sup 31}P MRS phosphodiester (PDE) signal, suggested in previous reports to be phosphoenolpyruvate (PEP). Phantom measurements to assess the chemical shifts of PEP and PtdC signals were performed at 7 T. A retrospective analysis of hepatic 3D {sup 31}P MR spectroscopic imaging (MRSI) data from 18 and five volunteers at 3 T and 7 T, respectively, was performed. Axial images were inspected for the presence of gallbladder, and PDE signals in representative spectra were quantified. Phantom experiments demonstrated the strong pH-dependence of the PEP chemical shift and proved the overlap of PtdC and PEP (∝2 ppm relative to phosphocreatine) at hepatic pH. Gallbladder was covered in seven of 23 in vivo 3D-MRSI datasets. The PDE{sub gall}/γ-ATP{sub liver} ratio was 4.8-fold higher (p = 0.001) in the gallbladder (PDE{sub gall}/γ-ATP{sub liver} = 3.61 ± 0.79) than in the liver (PDE{sub liver}/γ-ATP{sub liver} = 0.75 ± 0.15). In vivo 7 T {sup 31}P MRSI allowed good separation of PDE components. The gallbladder is a strong source of contamination in adjacent {sup 31}P MR hepatic spectra due to biliary phosphatidylcholine. In vivo {sup 31}P MR hepatic signal at 2.06 ppm may represent both phosphatidylcholine and phosphoenolpyruvate, with a higher phosphatidylcholine contribution due to its higher concentration. (orig.)

  15. 31P magnetic resonance spectroscopy of skeletal muscle in patients with fibromyalgia

    Jacobsen, Søren; Jensen, K E; Thomsen, C;

    1992-01-01

    31Phosphorous nuclear magnetic resonance (31P NMR) spectroscopy of painful calf muscle was performed in 12 patients with fibromyalgia (FS) and 7 healthy subjects during rest, aerobic and anaerobic exercising conditions, and postexercise recovery. Ratios of inorganic phosphate and creatinine...... phosphate (Pi/PCr) and pH were calculated from the collected 31P NMR spectra. Resting values of Pi/PCr were normal in the patients. Patients delivered only 49% of the muscle power of the controls (p = 0.005). Patients and controls had similar rates of Pi/PCr and pH changes during work and recovery. The...

  16. 13 C and 31 P NMR use in phosphinite synthesis and rhodium cationic catalysts accompaniment

    Several studies on rigid cyclic frameworks have been developed recently. This work shows the use of 13 C and 31 P NMR analysis for identifying and characterizing the molecular structures of phosphinites, thiophosphinites and rhodium catalysts. The phosphinites were synthesized and rhodium complexes prepared from them, aiming the catalysts synthesis for hydrogenation processes. Synthesizing phosphinites and thiophosphinites, alcohols on their racemic form were used, therefore, the catalysts were obtained as diasteroisomers. 13 C and 31 P NMR data are discussed in details and chemical shifts are also analysed

  17. Effects of all-trans-retinol on human tumor cell growth: /sup 31/P NMR studies

    The effects of all-trans-retinol on the cell line HCT-8R, from human colon adenocarcinoma, have been examined. Dose-response curve shows that retinol inhibits cell growth starting from vitamin concentration as low as 10/sup -10/M. No cytotoxic effects were observed at the used concentrations. /sup 31/P NMR spectra of intact HCT-8R cells showed slight modifications in the ATP metabolism. More relevant modifications on the lipid components are also hypothizable on the basis of /sup 31/P NMR spectra analysis of freshly prepared perchloric acid extracts

  18. Estudo do metabolismo energético muscular em atletas por 31P-ERM Muscular energetic metabolism study in athletes by 31P-MRS

    Maria Gisele dos Santos

    2004-04-01

    Full Text Available OBJETIVO: Caracterizar as reservas energéticas de metabólitos fosforilados no músculo esquelético de atletas mediante 31P-ERM. MÉTODOS: Amostra deste estudo foi formada por 14 atletas de alto nível do Centro de Alto Rendimento Esportivo (CAR, Sant Cugat del Vallés, Espanha. O padrão de metabólitos fosforilados foi medido no músculo vasto medial por 31P-ERM. A suplementação oral foi realizada durante 14 dias, na forma de 20g de monohidrato de creatina. Os atletas foram determinados conforme as suas características físicas (peso, altura, índice de massa corporal (IMC, consumo máximo de oxigênio (VO2 Max. em dois grupos: placebo (maltodextrina e suplementação com creatina. O protocolo de exercício foi realizado no interior do túnel de ressonância (160 x 52 cm, a 60 ciclos por minuto para ambas as pernas. RESULTADOS: Os resultados demonstraram um aumento significativo da fosfocreatina (PCr durante o exercício, após o período de suplementação, denotando uma redução do seu consumo no grupo que recebeu suplementação com creatina; não houve diminuição significativa do pH intracelular e fosfato inorgânico após a suplementação. CONCLUSÃO: O protocolo de exercício realizado pelos fundistas no Centro de Diagnóstico de Pedralbes permitiu detectar mediante 31P-ERM, no grupo que foi suplementado com creatina, uma diminuição do consumo de PCr durante os períodos de exercício.BACKGROUND: The aim of this study was to characterize the muscular reservoirs of phosphorilated energetic components of athletes using 31P-MRS. METHODS: The sample was formed by 14 elite athletes from the Center for High Sportive Performance (CAR, Sant Cugat del Vallés, Spain. The pattern of the phosphorilated metabolites was measured from the muscle vastus medialis by 31P-MRS. Oral supplementation of 20 g of Creatine monohydrate was given during 14 days. Two groups of athletes were formed according to their physical characteristics (weight

  19. Hepatic 31P-MR Spectroscopy Analysis of Normal Adults%健康成人肝脏31P-MR波谱研究

    崔恩铭; 谭理连; 李志铭; 汪银玉; 刘克; 黄勇; 林凡

    2007-01-01

    目的:探讨健康成人肝脏31P-MR波谱及代谢生化信息特点.方法:分析20例健康志愿者31P-MR波谱检查肝脏代谢化合物信息及细胞内pH值,并将本组研究对象按年龄分为3组,分别为青年组(20~34岁)、中年组(35~49岁)和老年组(50~65岁),统计分析各年龄组间肝脏代谢物水平是否有差异.结果:20例研究对象肝脏31P-MRS均能显示磷酸单脂(PME) 、无机磷(Pi) 、磷酸双脂(PDE) 、磷酸肌酸(PCr)、γ-ATP、α-ATP和β-ATP共7种代谢产物峰(从左到右),其波峰化学位移分别为0.7~1.9、0.44~-0.75、-1.45~-2.65、-4.81~-6.13、-7.3~-8.46、-12.7~-14.05和-21.45~-22.77 ppm,其峰下积分面积分别为0.8±0.57、0.97±0.68、2.51±1.59、0.61±0.5、2.11±0.99和1.14±0.85,计算肝组织PH值为7.35±0.04.经方差分析,各年龄组间PME、Pi、PDE、γ-ATP、α- ATP和β-ATP代谢物峰下面积和细胞内PH值均无统计学差异(P》0.05),肝脏代谢化合物含量、能量状况及细胞内PH值不随年龄改变而变化.结论:肝脏31P-MRS能无创、直接检测肝代谢过程的生化信息及能量状况,对了解肝脏代谢情况具有重要临床价值.

  20. Structure and motion of phospholipids in human plasma lipoproteins. A 31P NMR study

    The structure and motion of phospholipids in human plasma lipoproteins have been studied by using 31P NMR. Lateral diffusion coefficients, DT, obtained from the viscosity dependence of the 31P NMR line widths, were obtained for very low density lipoprotein (VLDL), low-density lipoprotein (LDL), high-density lipoproteins (HDL2, HDL3), and egg PC/TO microemulsions at 25 degree C, for VLDL at 40 degree C, and for LDL at 45 degree C. In order to prove the orientation and/or order of the phospholipid head-group, estimates of the residual chemical shift anistropy, Δσ, have been obtained for all the lipoproteins and the microemulsions from the viscosity and field dependence for the 31P NMR line widths. These results suggest differences in the orientation and/or ordering of the head-group in the HDLs. The dynamic behavior of the phosphate moiety in LDL and HDL3 has been obtained from the temperature dependence of the 31P spin-lattice relaxation rates. Values of the correlation time for phosphate group reorientation and the activation energy for the motion are nearly identical in LDL and HDL3 and are similar to values obtained for phospholipid bilayers. This argues against long-lived protein-lipid interactions being the source of either the slow diffusion in LDL or the altered head-group orientation in the HDLs

  1. In vivo 31P NMR spectroscopic studies on brain metabolic deterioration

    A custom-built 31P NMR spectrometer with 5.6 Tesla, horizontal magnet was used to determine the changes of in vivo phosphorus metabolism of the rat brain in various pathological conditions. 31P NMR spectroscopy readily demonstrated cerebral metabolic deterioration and/or recovery in vivo, in terms of the changes in relative concentrations of phosphate metabolites such as adenosine triphosphate (ATP), phosphocreatine (PCr) and inorganic phosphate (Pi), and the alterations of intracellular pH (pHi) calculated from the chemical shift of the Pi peak relative to the PCr peak, following different kinds of brain insults. 25-minute hypoxia caused the decrease in PCr and the increase in Pi with ATP's unchanged. After 15-minute global ischemia, PCr and ATP peaks completely disappeared, which recovered after the restoration of cerebral blood flow. 31P NMR spectroscopy clearly showed metabolic deterioration associated with focal cerebral infarction in the rat with middle cerebral artery occluded 24 hours previously. Severe impact trauma provoked progressive deterioration of cerebral phosphorus metabolism. This alteration was notified even at the first five-minute spectrum. The author has demonstrated that in vivo 31P NMR spectroscopic measurement would be useful and fascinating to evaluate in vivo phosphorus metabolism at various pathological states repeatedly and noninvasively. (author)

  2. Study of radiation induced changes of phosphorus metabolism in mice by 31P NMR spectroscopy

    The aim of this study was to examine whether 31P NMR can efficiently detect X-ray radiation induced changes of energy metabolism in mice. Exposure to ionizing radiation causes changes in energy supply that are associated with the tissue damage because of oxidative stress and uncoupled oxidative phosphorylation. This has as a consequence decreased phosphocreatine to adenosine triphosphate ratio (Pcr/ATP) as well as increased creatine kinase (CK) and liver enzymes (transaminases AST and ALT) levels in serum. In this study, experimental mice that received 7 Gy of X-ray radiation and a control group were studied by 31P NMR spectroscopy and biochemically by measuring CK and liver enzyme levels in plasma. Mice (irradiated and control) were measured at regular time intervals for the next three weeks after the exposure to radiation. A significant change in the Pcr/ATP ratio, determined from corresponding peaks of 31P NMR spectra, was observed in the 7 Gy group 2 days or more after the irradiation, while no significant change in the Pcr/ATP ratio, was observed in the control group. This result was supported by parallel measurements of CK levels that were highly increased immediately after the irradiation which correlates with the observed decrease of the Pcr/ATP ratio and with it associated drop of muscle energy supply. The 31P NMR measurements of the Pcr/ATP ratio can in principle serve as an instantaneous and noninvasive index for assessment of the received dose of irradiation

  3. Rose Atoll Site 31P 2/22/2012 38-39M

    US Fish and Wildlife Service, Department of the Interior — Onemetersquare 1 meter x 1 meter benthic substrate at Rose Atoll, site 31P 14 32.568S, 168 09.417W, between 38 and 39 meters along a permanent transect.

  4. Rose Atoll Site 31P 6/21/2005 (6)M

    US Fish and Wildlife Service, Department of the Interior — One-meter-square (1 meter x 1 meter) benthic substrate at Rose Atoll, site 31P (14 32.568S, 168 09.417W), at meter 6 along a permanent transect.

  5. Rose Atoll Site 31P 6/21/2005 (2)M

    US Fish and Wildlife Service, Department of the Interior — One-meter-square (1 meter x 1 meter) benthic substrate at Rose Atoll, site 31P (14 32.568S, 168 09.417W), at meter 2 along a permanent transect.

  6. Rose Atoll Site 31P 6/21/2005 (3)M

    US Fish and Wildlife Service, Department of the Interior — One-meter-square (1 meter x 1 meter) benthic substrate at Rose Atoll, site 31P (14 32.568S, 168 09.417W), at meter 3 along a permanent transect.

  7. Rose Atoll Site 31P 6/21/2005 (5)M

    US Fish and Wildlife Service, Department of the Interior — One-meter-square (1 meter x 1 meter) benthic substrate at Rose Atoll, site 31P (14 32.568S, 168 09.417W), at meter 5 along a permanent transect.

  8. Rose Atoll Site 31P 6/21/2005 (1)M

    US Fish and Wildlife Service, Department of the Interior — One-meter-square (1 meter x 1 meter) benthic substrate at Rose Atoll, site 31P (14 32.568S, 168 09.417W), at meter 1 along a permanent transect.

  9. Rose Atoll Site 31P 7/30/2004 4-5M

    US Fish and Wildlife Service, Department of the Interior — One-meter-square (1 meter x 1 meter) benthic substrate at Rose Atoll, site 31P (14 32.568S, 168 09.417W), between 4 and 5 meters along a permanent transect.

  10. Rose Atoll Site 31P 6/21/2005 (13)M

    US Fish and Wildlife Service, Department of the Interior — One-meter-square (1 meter x 1 meter) benthic substrate at Rose Atoll, site 31P (14 32.568S, 168 09.417W), at meter 13 along a permanent transect.

  11. Rose Atoll Site 31P 6/21/2005 (34)M

    US Fish and Wildlife Service, Department of the Interior — One-meter-square (1 meter x 1 meter) benthic substrate at Rose Atoll, site 31P (14 32.568S, 168 09.417W), at meter 34 along a permanent transect.

  12. Organic matter and pH affect the analysis efficiency of (31)P-NMR.

    Zhang, Wenqiang; Jin, Xin; Rong, Nan; Li, Jie; Shan, Baoqing

    2016-05-01

    Solution (31)P nuclear magnetic resonance spectroscopy ((31)P-NMR) is a useful method to analyze organic phosphorus (Po), but a general procedure for the analysis method is lacking. The authors used solution (31)P-NMR, which was found to be an effective method for analysis of Po in Haihe River sediment, to analyze the Po in the surface sediment in Eastern China at the regional scale, and found that the NaOH-ethylenediaminetetraacetic acid (EDTA) extraction rate was affected by environmental factors. At the regional scale, the extraction rate showed a positive relationship with loss on ignition, when the extraction rate was lower than 60%. The extraction rate had no relationship with the loss on ignition when the extraction rate was higher than 60%. The extraction rate showed a negative relationship with pH, which means that the extraction rate was higher in acidic sediment and lower in alkaline sediment. The ratio of TC/TN (the ratio of total carbon to total nitrogen) was considered to represent the origin of organic matter in the sediment. The extraction rate was high when the TC/TN ratio was lower than 20, meanwhile the extraction rate decreased as the TC/TN ratio increased. The results show that the origin of organic matter in sediment significantly affects the NaOH-EDTA extraction rate. This study will give theoretical support for building an effective and general solution (31)P-NMR analysis method. PMID:27155430

  13. Rose Atoll Site 31P 6/21/2005 (38)M

    US Fish and Wildlife Service, Department of the Interior — One-meter-square (1 meter x 1 meter) benthic substrate at Rose Atoll, site 31P (14 32.568S, 168 09.417W), at meter 38 along a permanent transect.

  14. Rose Atoll Site 31P 2/22/2012 22-23M

    US Fish and Wildlife Service, Department of the Interior — Onemetersquare 1 meter x 1 meter benthic substrate at Rose Atoll, site 31P 14 32.568S, 168 09.417W, between 22 and 23 meters along a permanent transect.

  15. Rose Atoll Site 31P 2/22/2012 36-37M

    US Fish and Wildlife Service, Department of the Interior — Onemetersquare 1 meter x 1 meter benthic substrate at Rose Atoll, site 31P 14 32.568S, 168 09.417W, between 36 and 37 meters along a permanent transect.

  16. {sup 31}P-MR spectroscopy in children and adolescents with a familial risk of schizophrenia

    Rzanny, R.; Reichenbach, J.R.; Pfleiderer, S.O.R.; Kaiser, W.A. [Institut fuer Diagnostische und Interventionelle Radiologie, Abteilung MT, Klinikum der Friedrich-Schiller-Universitaet Jena, Philosophenweg 3, 07741 Jena (Germany); Klemm, S.; Blanz, B. [Klinik fuer Kinder- und Jugendpsychiatrie, Klinikum der Friedrich-Schiller-Universitaet Jena, Bachstrasse 18, 07741 Jena (Germany); Schmidt, B.; Volz, H.-P. [Klinik fuer Psychiatrie, Klinikum der Friedrich-Schiller-Universitaet Jena, Bachstrasse 18, 07741 Jena (Germany)

    2003-04-01

    Based on a previous report [9] on alterations of membrane phosphorus metabolism in asymptomatic family members of schizophrenic patients, the aim of the present study was to extend and improve the evaluation and data processing of {sup 31}P spectroscopic data obtained from a larger study population by including an analysis of the broad spectral component (BC) of membrane phospholipids (PL). Eighteen children and siblings of patients with schizophrenia and a gender- and age-matched control group of 18 healthy subjects without familial schizophrenia were investigated with phosphorus magnetic resonance spectroscopy ({sup 31}P-MRS) by using image selected in vivo spectroscopy (ISIS) in the dorsolateral prefrontal regions (DLPFR) of the brain. Spectral analysis was performed by using both the full and truncated FID to estimate metabolic peak ratios of different {sup 31}P metabolites and the intensity and linewidth of the broad component. A significantly higher PDE level (p<0.01) and increased linewidth of the PDE components were observed for the high-risk group compared with the control group (p=0.02). No significant differences were observed for PME as well as for other {sup 31}P-metabolites. No differences were observed between the left and right hemispheres for different normalised {sup 31}P-metabolic levels. Decreased intensities (p=0.03) and smaller linewidths (p=0.01) were obtained for the broad component in the high-risk group. Impairments of membrane metabolism that are typical for schizophrenic patients are partially observed in adolescent asymptomatic family members of schizophrenics, including increased levels of low molecular PDE compounds indicating increased membrane degradation processes, no changes for PME, and decreased intensities and linewidths of the BC indicating changes in the composition and fluidity of membrane phospholipids. Despite limitations to completely suppress fast-relaxing components by dismissing initial FID data points, the

  17. 31P-MR spectroscopy in children and adolescents with a familial risk of schizophrenia

    Based on a previous report [9] on alterations of membrane phosphorus metabolism in asymptomatic family members of schizophrenic patients, the aim of the present study was to extend and improve the evaluation and data processing of 31P spectroscopic data obtained from a larger study population by including an analysis of the broad spectral component (BC) of membrane phospholipids (PL). Eighteen children and siblings of patients with schizophrenia and a gender- and age-matched control group of 18 healthy subjects without familial schizophrenia were investigated with phosphorus magnetic resonance spectroscopy (31P-MRS) by using image selected in vivo spectroscopy (ISIS) in the dorsolateral prefrontal regions (DLPFR) of the brain. Spectral analysis was performed by using both the full and truncated FID to estimate metabolic peak ratios of different 31P metabolites and the intensity and linewidth of the broad component. A significantly higher PDE level (p31P-metabolites. No differences were observed between the left and right hemispheres for different normalised 31P-metabolic levels. Decreased intensities (p=0.03) and smaller linewidths (p=0.01) were obtained for the broad component in the high-risk group. Impairments of membrane metabolism that are typical for schizophrenic patients are partially observed in adolescent asymptomatic family members of schizophrenics, including increased levels of low molecular PDE compounds indicating increased membrane degradation processes, no changes for PME, and decreased intensities and linewidths of the BC indicating changes in the composition and fluidity of membrane phospholipids. Despite limitations to completely suppress fast-relaxing components by dismissing initial FID data points, the spectroscopic results indicate additional changes in the membrane metabolism of high-risk subjects beyond changes of synthesis and degradation. (orig.)

  18. Main: 1H82 [RPSD[Archive

    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 ...

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    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: 1H86 [RPSD[Archive

    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 ...

  1. Main: 1H83 [RPSD[Archive

    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 ...

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    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 ...

  3. Main: 1H49 [RPSD[Archive

    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 ...

  4. Bio-fortification and isotopic labelling of Se metabolites in onions and carrots following foliar application of Se and 77Se

    Kapolna, Emese; Laursen, Kristian Holst; Husted, Søren; Larsen, Erik H

    2011-01-01

    The aims were to bio-fortify onions by foliar application of selenium (Se) and to intrinsically label bioactive Se-metabolites in onion and carrot by enriched, stable77Se for use in human physiological studies. Onion bulbs and leaves were enriched in Se by repeated foliar spraying of 10 or 100 μg Se mL-1 solutions of sodium selenite (Se(IV)) or sodium selenate (Se(VI)). ICP-MS analysis of onion leaves and bulbs showed that the Se concentration was enhanced by up to a factor of approximately 5...

  5. THE STUDY OF LEUKAEMIA SERUM BY 31P NMR%白血病人血清的31P NMR研究

    吴昌琳; 黄永仁; 蔡侧骥

    2001-01-01

    运用31P核磁共振波谱(NMRS)研究血清中磷脂的代谢变化,并探讨该法对白血病诊断的可行性.方法采用MSL-300MHz型超导核磁共振仪测量白血病人及健康人血清标本,通过分析比较血清中磷脂酰胆碱(PC)信号及磷脂酰乙醇胺和(神经)鞘磷脂(PE+SM)信号相对积分面积,了解各自血清中的磷脂含量水平.结果,白血病人血清中的磷脂信号强度相对正常人明显偏低,反映了对应的PC及(PE+SM)含量相对正常人偏低,尤其对初发未治疗的病人,差别更加明显.结论,本法可作为研究血清中磷脂的变化、代谢情况及白血病人临床诊断的新方法.%To investigate the feasibility of serum 31P NMRS in the study phospholipid metabolites and diagnosis of leukaemia. Method: Serum sample of leukaemia patients and healthy controls were collected and measured by 31P NMRS with MSL-300MHz spectrometer. The phospholipid contents were known by contraxt relatively integral area of PC signal and (PE+SM) signal. Results: In spectra of serum of leukaemia patients, the phospholipid signal intensities were significantly decreases. It reflected lower phosphatidylcholine and phosphatidylcholine and sphingomyelin content in serum of leukemia patients, especially for original untreatment patient. Conclusions: These results suggest that serum 31P NMRS may likely become a promising new method for the study of phospholipid changes or metabolites and identifying the presence of leukaemia.

  6. Coal structure at reactive sites by sup 1 H- sup 13 C- sup 19 F double cross polarization (DCP)/MAS sup 13 C NMR spectroscopy

    Hagaman, E.W.; Woody, M.C. (Oak Ridge National Lab., TN (USA))

    1989-01-01

    The solid state NMR technique, {sup 1}H-{sup 13}C-{sup 31}P double cross polarization (DCP)/MAS {sup 13}C-NMR spectroscopy, uses the direct dipolar interaction between {sup 13}C-{sup 31}P spin pairs in organophosphorus substances to identify the subset of carbons within a spherical volume element of 0.4 nm radius centered on the {sup 31}P atom. In combination with chemical manipulation of coals designed to introduce phosphorus containing functionality into the organic matrix, the NMR experiment becomes a method to examine selectively the carbon bonding network at the reactive sites in the coal. This approach generates a statistical structure description of the coal at the reaction centers in contrast to bulk carbon characterization using conventional {sup 1}H-{sup 13}C CP/MAS {sup 13}C NMR spectroscopy. 3 refs.

  7. CD and 31P NMR studies of tachykinin and MSH neuropeptides in SDS and DPC micelles

    Schneider, Sydney C.; Brown, Taylor C.; Gonzalez, Javier D.; Levonyak, Nicholas S.; Rush, Lydia A.; Cremeens, Matthew E.

    2016-02-01

    Secondary structural characteristics of substance P (SP), neurokinin A (NKA), neurokinin B (NKB), α-melanocyte stimulating hormone peptide (α-MSH), γ1-MSH, γ2-MSH, and melittin were evaluated with circular dichroism in phosphite buffer, DPC micelles, and SDS micelles. CD spectral properties of γ1-MSH and γ2-MSH as well as 31P NMR of DPC micelles with all the peptides are reported for the first time. Although, a trend in the neuropeptide/micelle CD data appears to show increased α-helix content for the tachykinin peptides (SP, NKA, NKB) and increased β-sheet content for the MSH peptides (α-MSH, γ1-MSH, γ2-MSH) with increasing peptide charge, the lack of perturbed 31P NMR signals for all neuropeptides could suggest that the reported antimicrobial activity of SP and α-MSH might not be related to a membrane disruption mode of action.

  8. In-vivo31P-MR spectroscopy of the calf muscles in arterial occlusive disease

    Muscle metabolism was measured in 7 patients with arterial occlusive disease and symptoms of intermittent claudication both before and after percutaneous vascular neurolysis by means of dynamic 31 P-MR spectroscopy. Phosphorus spectra of the involved calf muscles were determined before, during and after defined treadmill exercise. In addition to pH values the phosphocreatine content was measured during activity and recovery phases. There was close correlation in these patients between the increase in claudication distance and more rapid regeneration of phosphocreatine following neurolysis. However, none of the patients achieved normal values of phosphate metabolism. By means of the non-invasive 31 P-MR spectroscopy it was possible for the first time to demonstrate the biochemiscal changes associated with neurolytic lumbar sympathetic blockade. (orig.)

  9. Simultaneous electromyography and 31P nuclear magnetic resonance spectroscopy--with application to muscle fatigue

    Vestergaard-Poulsen, P; Thomsen, C; Sinkjaer, T;

    1992-01-01

    changes in human muscle. The aim of this study was to develop a method by which EMG and NMR spectroscopy measurements could be performed simultaneously. All measurements were performed in a whole body 1.5 Tesla NMR scanner. A calf muscle ergometer, designed for use in a whole body NMR scanner, was used......The electromyogram (EMG) is often used to study human muscle fatigue, but the changes in the electromyographic signals during muscle contraction are not well understood in relation to muscle metabolism. The 31P NMR spectroscopy is a semi-quantitative non-invasive method for studying the metabolic....... The subject had the left foot strapped to the ergometer. The anterior tibial EMG was recorded by bipolar surface electrodes. A surface coil was strapped to the anterior tibial muscle next to the EMG electrodes. Simultaneous measurements of surface EMG and surface coil 31P NMR spectroscopy were...

  10. Erythrocytes in muscular dystrophy. Investigation with 31P nuclear magnetic resonance spectroscopy

    Phosphorus 31 nuclear magnetic resonance (31P NMR) signals were recorded from intact human erythrocytes for 16 hours. Total phosphate concentration, which was estimated as the sum of the individual 31P signals, was 25% lower in erythrocytes from men with myotonic dystrophy than in control erythrocytes. The inorganic-phosphate fraction contained the highest average phosphate concentration over the 16-hour period, and made the major contribution to the difference in total phosphate between the two groups. This result was not observed in erythrocytes from either women with myotonic dystrophy or patients with Duchenne's dystrophy and may be due to a change in cell membrane permeability to inorganic phosphate, which lead to lower steady-state concentrations of the intracellular phosphates

  11. Erythrocytes in muscular dystrophy. Investigation with 31P nuclear magnetic resonance spectroscopy

    Phosphorus 31 nuclear magnetic resonance (31P NMR) signals were recorded from intact human erythrocytes for 16 hours. Total phosphate concentration, which was estimated as the sum of the individual 31P signals, was 25% lower in erythrocytes from men with myotonic dystrophy than in control erythrocytes. The inorganic-phosphate fraction contained the highest average phosphate concentration over the 16-hour period, and made the major contribution to the difference in total phosphate between the two groups. This result was not observed in erythrocytes from either women with myotonic dystrophy or patients with Duchenne's dystrophy and may be due to a change in cell membrane permeability to inorganic phosphate, which leads to lower steady-state concentrations of the intracellular phosphates

  12. Simultaneous 31P NMR spectroscopy and EMG in exercising and recovering human skeletal muscle: technical aspects

    Vestergaard-Poulsen, P; Thomsen, C; Sinkjaer, T;

    1994-01-01

    skeletal muscle, a relationship that is still poorly understood. This study describes the optimization of skeletal muscle 31P-MRS in a whole-body magnet, involving surface coil design, utilization of adiabatic radio frequency pulses and advanced time-domain fitting, to the technical design of SEMG. A...... nonmagnetic ergometer was used for ankle dorsiflexions that activated only the anterior tibial muscle as verified by post exercise imaging. The coil design and the adiabatic sech/tanh pulse improved sensitivity by 45% and 56% respectively, compared with standard techniques. Simultaneous electromyographic...... recordings did not deteriorate the NMR spectra. The VARPRO time domain fitting routine was very suitable for estimating31P muscle spectra. With these methods it was possible to accurately estimate parameters describing metabolic and electrical changes during rest, exercise and the entire recovery period with...

  13. Application of localized 31P MRS saturation transfer at 7 T for measurement of ATP metabolism in the liver: reproducibility and initial clinical application in patients with non-alcoholic fatty liver disease

    Saturation transfer (ST) phosphorus MR spectroscopy (31P MRS) enables in vivo insight into energy metabolism and thus could identify liver conditions currently diagnosed only by biopsy. This study assesses the reproducibility of the localized 31P MRS ST in liver at 7 T and tests its potential for noninvasive differentiation of non-alcoholic fatty liver (NAFL) and steatohepatitis (NASH). After the ethics committee approval, reproducibility of the localized 31P MRS ST at 7 T and the biological variation of acquired hepato-metabolic parameters were assessed in healthy volunteers. Subsequently, 16 suspected NAFL/NASH patients underwent MRS measurements and diagnostic liver biopsy. The Pi-to-ATP exchange parameters were compared between the groups by a Mann-Whitney U test and related to the liver fat content estimated by a single-voxel proton (1H) MRS, measured at 3 T. The mean exchange rate constant (k) in healthy volunteers was 0.31 ± 0.03 s-1 with a coefficient of variation of 9.0 %. Significantly lower exchange rates (p -1) when compared to healthy volunteers, and NAFL patients (k = 0.30 ± 0.05 s-1). Significant correlation was found between the k value and the liver fat content (r = 0.824, p 31P MRS ST technique provides a tool for gaining insight into hepatic ATP metabolism and could contribute to the differentiation of NAFL and NASH. (orig.)

  14. Pyrolysis temperature affects phosphorus transformation in biochar: Chemical fractionation and (31)P NMR analysis.

    Xu, Gang; Zhang, You; Shao, Hongbo; Sun, Junna

    2016-11-01

    Phosphorus (P) recycling or reuse by pyrolyzing crop residue has recently elicited increased research interest. However, the effects of feedstock and pyrolysis conditions on P species have not been fully understood. Such knowledge is important in identifying the agronomic and environmental uses of biochar. Residues of three main Chinese agricultural crops and the biochars (produced at 300°C-600°C) derived from these crops were used to determine P transformations during pyrolysis. Hedley sequential fractionation and (31)P NMR analyses were used in the investigation. Our results showed that P transformation in biochar was significantly affected by pyrolysis temperature regardless of feedstock (Wheat straw, maize straw and peanut husk). Pyrolysis treatment transformed water soluble P into a labile (NaHCO3-Pi) or semi-labile pool (NaOH-Pi) and into a stable pool (Dil. HCl P and residual-P). At the same time, organic P was transformed into inorganic P fractions which was identified by the rapid decomposition of organic P detected with solution (31)P NMR. The P transformation during pyrolysis process suggested more stable P was formed at a higher pyrolysis temperature. This result was also evidenced by the presence of less soluble or stable P species, such as such as poly-P, crandallite (CaAl3(OH)5(PO4)2) and Wavellite (Al3(OH)3(PO4)2·5H2O), as detected by solid-state (31)P NMR in biochars formed at a higher pyrolysis temperature. Furthermore, a significant proportion of less soluble pyrophosphate was identified by solution (2%-35%) and solid-state (8%-53%) (31)P NMR, which was also responsible for the stable P forms at higher pyrolysis temperature although their solubility or stability requires further investigation. Results suggested that a relatively lower pyrolysis temperature retains P availability regardless of feedstock during pyrolysis process. PMID:27343937

  15. 31P NMR spectroscopy of tumors in the evaluation of response to therapy

    In this thesis the effects of different kinds of therapy on tumour metabolism were investigated by in vivo 31P NMR spectroscopy. From the first five chapters (laboratory-animal studies) it turns out that after radiotherapy as well as after hyperthermy or chemoterapy changes can be observed in the 31P NMR spectra of tumours. In a number of cases a durable decline occurred in the ratio of the high-energetic adenosinephosphate (ATP) and the low-energeic anorganic phosphate, cuased by the mortification of tumourcells. On the other hand, tumour regression after effective chemotherapy resulted in a growth of the ATP/Pi ratio. In one case a temporary drop occurred which could be related to a temporary decrease in tumour perfusion. In anoter case a temporary drop of the ATP/Pi ratio correlated with resistence against treatment with cis-diaminodichoroplatina. In contrast with the changes in ATP/Pi ratio, the changes, after (chemo)therapy, in tumour pH do not seem to be related with the respons of the tumour. The results of the laboratory-animal experiments indicate that in vivo 31P NMR spectroscopy could be applied in the clinic in order to establish betime the response of tumours on therapy. In ch. 6 initial experiences with clinical NMR spectroscopy of human breast cancer are described. The results indicate that by 31P NMR spectroscopy malignant breast tissues can be discerned from normal breast tissues, following radiotherapy and subsequent tumour regression, in the spectrum of the tumorous region an intense PCr signal developed which appeared to reflect a metabolic change in the tumous itself. 177 refs.; 27 figs.; 6 tabs

  16. Bioenergetic Measurements in Children with Bipolar Disorder: A Pilot 31P Magnetic Resonance Spectroscopy Study

    Sikoglu, Elif M.; J. Eric Jensen; Gordana Vitaliano; Liso Navarro, Ana A; Renshaw, Perry F.; Jean A. Frazier; Moore, Constance M.

    2013-01-01

    Background: Research exploring Bipolar Disorder (BD) phenotypes and mitochondrial dysfunction, particularly in younger subjects, has been insufficient to date. Previous studies have found abnormal cerebral pH levels in adults with BD, which may be directly linked to abnormal mitochondrial activity. To date no such studies have been reported in children with BD. Methods: Phosphorus Magnetic Resonance Spectroscopy (\\(^{31}\\)P MRS) was used to determine pH, phopshocreatine (PCr) and inorganic ph...

  17. In vivo magnetic resonance imaging and 31P spectroscopy of large human brain tumours at 1.5 tesla

    Thomsen, C; Jensen, K E; Achten, E;

    1988-01-01

    31P MR spectroscopy of human brain tumours is one feature of magnetic resonance imaging. Eight patients with large superficial brain tumours and eight healthy volunteers were examined with 31P spectroscopy using an 8 cm surface coil for volume selection. Seven frequencies were resolved in our spe...

  18. Early effects of radiotherapy in small cell lung cancer xenografts monitored by 31P magnetic resonance spectroscopy and biochemical analysis

    Kristjansen, P E; Pedersen, E J; Quistorff, B;

    1990-01-01

    31P magnetic resonance spectroscopy (31P MRS) and biochemical analysis of extracts were applied to study the metabolic response to X-irradiation of small cell lung cancer in nude mice. Two small cell lung cancer xenografts, CPH SCCL 54A and 54B, with different radiosensitivity, although derived...

  19. 31P MAS-NMR of human erythrocytes: independence of cell volume from angular velocity.

    Kuchel, P W; Bubb, W A; Ramadan, S; Chapman, B E; Philp, D J; Coen, M; Gready, J E; Harvey, P J; McLean, A J; Hook, J

    2004-09-01

    31P magic angle spinning NMR (MAS-NMR) spectra were obtained from suspensions of human red blood cells (RBCs) that contained the cell-volume-sensitive probe molecule, dimethyl methylphosphonate (DMMP). A mathematical representation of the spectral-peak shape, including the separation and width-at-half-height in the 31P NMR spectra, as a function of rotor speed, enabled us to explore the extent to which a change in cell volume would be reflected in the spectra if it occurred. We concluded that a fractional volume change in excess of 3% would have been detected by our experiments. Thus, the experiments indicated that the mean cell volume did not change by this amount even at the highest spinning rate of 7 kHz. The mean cell volume and intracellular 31P line-width were independent of the packing density of the cells and of the initial cell volume. The relationship of these conclusions to other non-NMR studies of pressure effects on cells is noted. PMID:15334588

  20. In vivo 31P-NMR spectroscopy of right ventricle in pigs.

    Schwartz, G G; Steinman, S K; Weiner, M W; Matson, G B

    1992-06-01

    The energy metabolism of the right ventricle (RV) in vivo has been largely unexplored. The goal of this study was to develop and implement techniques for in vivo 31P nuclear magnetic resonance (NMR) spectroscopy of the RV free wall. A two-turn, crossover-design elliptical surface coil was constructed to provide high sensitivity across the thin RV wall but minimal sensitivity in the blood-filled RV cavity. In 36 open-chest, anesthetized pigs, 31P spectroscopy of the RV free wall was performed with this coil at a field strength of 2 Tesla. Spectra were obtained from 800 acquisitions in 24 min with an average signal-to-noise ratio of 13.2 for phosphocreatine (PCr). The PCr-to-ATP (PCr/ATP) ratio of porcine RV was 1.42 +/- 0.05 (mean +/- SE), uncorrected for saturation at a repetition time of 1.8 s. With the use of literature values of the time constant of longitudinal relaxation (T1) to correct for partial saturation, the RV PCr/ATP was estimated to lie between 1.7 and 2.3. Decreased RV PCr/ATP was observed during RV ischemia and pressure overload. Thus in vivo 31P spectroscopy of the RV is readily accomplished with an appropriate surface coil and can provide new information about RV energy metabolism. PMID:1621852

  1. 31P nuclear magnetic resonance measurements of intracellular pH in giant barnacle muscle

    The accuracy of intracellular pH (pH/sub i/) measurements by 31P nuclear magnetic resonance (NMR) spectroscopy was examined in single muscle fibers from the giant barnacle, Balanus nubilis. The pH/sub i/ was derived from the chemical shifts of 2-deoxy-D-glucose-6-phosphate and inorganic phosphate. In fibers superfused with sea water at pH 7.7, pH/sub i/ = 7.30 +/- 0.02 at 200C. Experimentally induced pH/sub i/ changes were followed with a time resolution of 3 min. Intracellular alkalinization was induced by exposure to NH3Cl and intracellular acidification followed when NH3 was removed. Then acid extrusion was stimulated by exposure to bicarbonate containing sea water. In single muscle fibers 31P NMR results were in excellent agreement with microelectrode studies over the pH range of 6.5 to 8.0. The initial acid extrusion rate was 1.7 +/- 0.3 mmol x 1-1 x min-1 at pH/sub i/ 6.75. The authors results showed that 31P NMR is a reliable in vivo pH probe

  2. Inhibition of serine proteases by oxygen, sulfur and selenium dialkyl phosphoryl derivatives: Biochemical and 31P NMR studies

    31P NMR spectroscopy was employed to investigate the interaction of chymotrypsin with various organophosphorus inhibitors. The 31P NMR spectrum of diethyl selenophosphoryl chymotrypsin revealed two resonances at approximately 71 ppm and a single resonance at 48 ppm attributed to the covalent and non-covalent enzyme-inhibitor complexes, respectively. The goal of this investigation was to elucidate the basis of the two peaks at ∼71 ppm in the 31P NMR spectrum of diethyl selenophosphosphoryl-α-chymotrypsin. The possibility that the selenium atom in the structure of the organophosphorus inhibitor might have been responsible for the two peaks was addressed by extending the 31P NMR studies to diethyl thiophosphoryl- and diethyl phosphoryl-α-chymotrypsin. The fact that the latter modified enzyme derivatives also yielded 31P NMR spectra that exhibited two resonances assigned to covalent species discounted this possibility. The effect of the alkyl group of the inhibitor on the 31P NMR spectrum of the enzyme-inhibitor complex was further investigated by examining diisopropyl phosphoryl-α-chymotrypsin by 31P NMR spectroscopy

  3. {sup 1}H MR spectroscopy in epilepsy

    Hajek, Milan [MR Unit, Department of Diagnostic and Interventional Radiology, Institute for Clinical and Experimental Medicine, Videnska 1958/9, 140 21 Prague (Czech Republic)], E-mail: miha@medicon.cz; Dezortova, Monika [MR Unit, Department of Diagnostic and Interventional Radiology, Institute for Clinical and Experimental Medicine, Videnska 1958/9, 140 21 Prague (Czech Republic)], E-mail: mode@medicon.cz; Krsek, Pavel [Department of Pediatric Neurology, Charles University, Second Medical School, Motol Hospital, V Uvalu 84, 150 06 Prague 5 (Czech Republic)], E-mail: pavel.krsek@post.cz

    2008-08-15

    The introduction to the application of {sup 1}H MR spectroscopy for clinical and research studies of mesial temporal and extratemporal epilepsies is done. The techniques of single voxel and spectroscopic imaging are discussed and the analysis of {sup 1}H MR spectra together with basic metabolic descriptions is presented.

  4. 1H MR spectroscopy in epilepsy

    The introduction to the application of 1H MR spectroscopy for clinical and research studies of mesial temporal and extratemporal epilepsies is done. The techniques of single voxel and spectroscopic imaging are discussed and the analysis of 1H MR spectra together with basic metabolic descriptions is presented

  5. Study of myocardial metabolism in heterotopically transplanted rat hearts by 31P NMR

    This is a first study which investigated in vivo myocardial metabolism changes associated with acute graft rejection by 31P nuclear magnetic resonance (NMR). The donor hearts were heterotopically transplanted in the cervical portion of the recipient rats. Mean graft survival in the allogeneic transplantation group (Exp. G.) was 9.3 ± 2.6 days (n = 6), while all of the grafts (n = 5) in the syngeneic transplantation group (Cont. G.) have survived more than 21 days (the longest one : > 192) without any rejection episode. Six different kinds of signals were obtained in the spectrum by 31P NMR spectroscopy : phosphomonoester (PME), inorganic phosphate (Pi), phosphocreatine (PCr), as well as ATP-α, -β and -γ. The results obtained here showed : (1) After 24 hours of transplantation, increased Pi/PCr ratios (> 0.5) were observed both in the Exp. G. and in the Cont. G., which suggested the myocardial damage due to transplantation operation procedure. The ratios were gradually decreased and reached to less than 0.5 on the 3rd day after grafting. (2) Thereafter, in the Exp. G. Pi was gradually increased and PCr was gradually decreased because of the acute rejection; the Pi/PCr ratio was elevated beyond 0.5. However, no change of Pi/PCr ratio was observed in the Cont. G. 31P NMR spectroscopy employed in the experimental model of heterotopic heart transplantation at the cervical portion of rats was found to be useful and non-invasive for the study of myocardial metabolism after grafting. (author)

  6. An interstitial miniature antenna for localized in vivo 31P spectroscopy

    Phosphorus spectroscopy can be used to assess response in tumor therapy and to monitor response. Methodical problems of localisation and contamination make it more difficult to interpret and reproduce the spectra. Interstitial and endoluminal spectroscopy antennas placed directly within or close to the tumor could provide help in this problem. We developed an interstitial 31P MRS antenna together with a tuning network which can be used in thermometry catheters for hyperthermia within an internal lumen of 1.1 mm in diameter. A prototype of this type of miniature antenna suitable for use in Siemens MRI scanners at 1.5 T was described spectroscopically with regard to excitation profile, range and SNR. Results: In terms of quality, the excitation profiles of the interstitial antennas in relation to orientation correspond to those of comparable but considerably larger endocavitary antennas and catheter coils for MR imaging and spectroscopy. Maximum sensitivity was achieved by aligning the coil normal perpendicular to the B0 field. Signal losses of up to 50% have to be reckoned with when using other orientations. The maximum range of the interstitial antenna was determined using spectroscopy and was found to be 5 mm, i.e. 9 times coil radius. The sensitivity of the studied type of interstitial antenna allows in vivo 31P spectroscopy to be performed despite the unusually low axial dimension (coil radius r=0.55 mm). The prototype of the described interstitial antenna was used to measure an in vivo spectrum from the back muscle of a rabbit in 10 min. Nevertheless, the detection volume of at least some ml necessary for 31P spectroscopy results mainly from the large antenna length. Conclusion: The sensitivity of the interstitial antenna needs to be further improved in order to assess treatment response in patients. (orig./MG)

  7. Human in-vivo 31P MR spectroscopy of benign and malignant breast tumors

    To assess the potential clinical utility of in-vivo 31P magnetic resonance spectroscopy (MRS) in patients with various malignant and benign breast lesions. Seventeen patients with untreated primary malignant breast lesions (group I), eight patients with untreated benign breast lesions (group II) and seven normal breasts (group III) were included in this study. In-vivo 31P MRS was performed using a 1.5 Tesla MR scanner. Because of the characteristics of the coil, the volume of the tumor had to exceed 12 cc (3x2x2 cm), with a superoinferior diameter at least 3 cm. Mean and standard deviations of each metabolite were calculated and metabolite ratios, such as PME/PCr, PDE/PCr, T-ATP/PCr and PCr/T-ATP were calculated and statistically analyzed. Significant differences in PME were noted between groups I and III (p=0.0213), and between groups II and III (p=0.0213). The metabolite ratios which showed significant differences were PME/PCr (between groups II and III) (p=0.0201), PDE/PCr (between groups I and III, and between groups II and III) (p=0.0172), T-ATP/PCr (between groups II and III) (p=0.0287), and PCr/T-ATP (between groups II and III) (p=0.0287). There were no significant parameters between groups I and II. In-vivo 31P MRS is not helpful for establishing a differential diagnosis between benign and malignant breast lesions, at least with relatively large lesions greater than 3 cm in one or more dimensions

  8. Linear correlation of the barriers to pyramidal inversion of phosphorus with the 31P chemical shifts of acylphosphines

    The dependence of the inversion barriers (ΔG) of phosphorus compounds directly on a parameter of the inversion center, i.e., the chemical shift of the nucleus (delta31 P) were studied. The possibility of such an approach was justified by the correlation both of ΔG, and of delta31 P for phosphorus compounds with one and the same characteristics (the bond angles and electronegativities of the substituent). The acylphosphines (I-IX) were investigated in the range of variation of ΔG, accessible to dynamic NMR and in a fairly wide range of delta31 P

  9. 31P NMR investigations on free and enzyme bound thiamine pyrophosphate

    Pyruvate decarboxylase (PDC) contains thiamine pyrophosphate (TPP) and Mg2+ as cofactors. 31P NMR studies with PDC in the presence of added Mn2+ reveal the pyrophosphate moiety of TPP to be a nonaccessible area for the external Mn2+ and thus proving the Mg-P-complex (taking part in the binding of the coenzyme to the protein) to be a nonaccessible area for the medium. Glyoxylic acid, acting as an inhibitor of PDC by forming a noncleavable bond with the catalytic center of TPP causes a steric immobilization of the coenzyme indicated by a line broadening of the pyrophosphate moiety. 12 refs.; 3 figs

  10. In vivo 31 P NMR and histological investigation of muscle recovery after induced injury

    Muscle damage is a common accompanying exercise both in humans and animals. Although a wide variety of procedures have been used to study exercise-induced injury, it is difficulty to analyse the muscle regeneration with non invasive methods. In this work, a series of experiments was devised to demonstrate the use of in vivo 31 P NMR to allow non invasive and repeatable investigation of the skeletal muscle healing process by following the changes in metabolic activity that take place during muscle repair

  11. 31P NMR for the study of P metabolism and translocation in arbuscular mycorrhizal fungi

    Rasmussen, N.; Lloyd, D.C.; Ratcliffe, R.G.;

    2000-01-01

    biological systems to be studied non-invasively and non-destructively. (3)1P NMR experiments provide information about cytoplasmic and vacuolar pH, based on the pH-dependent chemical shifts of the signals arising from the inorganic P (P-i) located in the two compartments. Similarly, the resonances arising...... spectra of excised AM fungi and mycorrhizal roots contained signals from polyphosphate (PolyP), which were absent in the spectra of nonmycorrhizal roots. This demonstrated that the P-i taken up by the fungus was transformed into PolyP with a short chain length. The spectra of excised AM fungi revealed...

  12. 2D exchange 31P NMR spectroscopy of bacteriophage M13 and tobacco mosaic virus.

    Magusin, P.C.M.M.; Hemminga, M A

    1995-01-01

    Two-dimensional (2D) exchange 31P nuclear magnetic resonance spectroscopy is used to study the slow overall motion of the rod-shaped viruses M13 and tobacco mosaic virus in concentrated gels. Even for short mixing times, observed diagonal spectra differ remarkably from projection spectra and one-dimensional spectra. Our model readily explains this to be a consequence of the T2e anisotropy caused by slow overall rotation of the viruses about their length axis. 2D exchange spectra recorded for ...

  13. Phytic acid degradation by phytase – as viewed by 31P NMR and multivariate curve resolution

    Nielsen, Merete Møller; Viereck, Nanna; Engelsen, Søren Balling

    2007-01-01

    The 31P NMR method is a most direct and useful method to describe the degradation of phytic acid to lower inositol phosphates by the action of the enzyme phytase. The use of chemometric and CARS visualizes and helps in the interpretation of the results. By means of LatentiX it has been possible to visualize the time-dependent hydrolysis of phytic acid and by PCA the complexity of the phytic acid is shown in the score plots. By modeling the spectra in CARS it is possible to identify and quanti...

  14. Symmetry change of 77Se hyperfine components of ESR spectrum of SeO43- radicals in deuterated NH4H2PO4

    D-rate dependence (0 - 70 %) of the 77Se hf line-positions of SeO43- radicals in deuterated NH4H2PO4 is reported. In the paraelectric phase, on cooling, the symmetry of the angular dependence changes from high symmetry to low-symmetry A (which is similar to that for KDP or DKDP), but no remarkable deuteration effect is observed. In the antiferroelectric phase, the angular dependence for ADP still shows the low-symmetry A, while that for DADP (D70 %) shows the low-symmetry B which is compatible with the AFE order (the Nagamiya's model) of the ammonium salts. From this large deuteration effect on the SeO43- it is suggested that the AFE distortion of the PO43- radical in the D salts is larger than that in the H salts. (author)

  15. In vivo 31P-NMR spectroscopy of chronically stimulated canine skeletal muscle

    Chronic stimulation converts skeletal muscle of mixed fiber type to a uniform muscle made up of type I, fatigue-resistant fibers. Here, the bioenergetic correlates of fatigue resistance in conditioned canine latissimus dorsi are assessed with in vivo phosphorus-31 nuclear magnetic resonance (31P-NMR) spectroscopy. After chronic electrical stimulation, five dogs underwent 31P-NMR spectroscopic and isometric tension measurements on conditioned and contralateral control muscle during stimulation for 200, 300, 500, and 800 ms of an 1,100-ms duty cycle. With stimulation, phosphocreatine (PCr) fell proportional to the degree of stimulation in both conditioned and control muscle but fell significantly less in conditioned muscle at all the least intense stimulation period (200 ms). Isometric tension, expressed as a tension time index per gram muscle, was significantly greater in the conditioned muscle at the two longest stimulation periods. The overall small change in PCr and the lack of a plateau in tension observed in the conditioned muscle are similar to that seen in cardiac muscle during increased energy demand. This study indicates that the conditioned muscle's markedly enhanced resistance to fatigue is in part the result of its increased capacity for oxidative phosphorylation

  16. In Vivo 31P Echo-Planar Spectroscopic Imaging of Human Calf Muscle

    Wilhelm, Thomas; Bachert, Peter

    2001-03-01

    Localized phosphorus-31 NMR spectra of human calf muscle in vivo were obtained by means of echo-planar spectroscopic imaging (EPSI) with a 1.5-T whole-body scanner. The technique permits the measurement of two-dimensional 31P SI data at a minimum acquisition time of 2.4 s (8×8 voxels, TR=300 ms). With 9.4 min measurement time (TR=1100 ms, 64 averages) and 25×25×40 mm spatial resolution in vivo the 31P NMR signal-to-noise ratio (S/N) of the phosphocreatine (PCr) resonance was about 45; the multiplets of nucleoside 5‧-triphosphates were resolved. Spectral quality permits quantitative assessment of the PCr signal in a measurement time that is shorter by a factor of 2 or more than the minimum measurement time feasible with chemical-shift imaging. In a functional EPSI study with a time resolution of 20.5 s on the calf muscle of volunteers, spectra showed a 40% decrease of the PCr signal intensity (at rest: S/N≅12) upon exertion of the muscle.

  17. The 31P(3He,d)32S reactions at 25MeV

    The 31P(3He,d)32S reaction was investigated at 25 MeV incident energy. One hundred and eleven levels up to an excitation energy of 12.5 MeV were observed using a split-pole magnetic spectrograph. The experimental angular distributions were analyzed with the distorted-wave Born approximation. The optical model parameters used in the DWBA calculations were obtained from a fit to elastic 3He scattering data taken on 31P at 25 MeV. Gamov functions were used as form factors for the transfered proton in the case of unbound states. Values of the transfered orbital angular momenta l and spectroscopic strengths were obtained for sixty levels, with many odd-parity levels being observed above 9 MeV excitation. Spin and parity assignments were made upon the basis of the l-values obtained from the shapes of the angular distributions and upon comparison with the results of other reactions. Isospin assignments were made by comparison with 32P levels. Except for the lsub(P)=1, T=0 transfers, most of the observed spectroscopic strength is concentrated into a few levels. The existence of a T-mixed doublet of levels, Jsup(π)=1-, is suggested in the 11 MeV region of excitation. The excitation energies and spectroscopic strengths are compared with results of a recent shell-model calculation

  18. Physiologic significance of the phosphorylation potential in isolated perfused rat hearts (31P NMR)

    The authors assessed the metabolic and mechanical effects of changes in coronary perfusion pressure (CPP) and afterload (A) in isolated working apex-ejecting rat hearts perfused with Krebs-Henseleit solution containing an excess of O2 and substrate. Log(phosphorylation potential) or log (ATP)/(ADP)x (Pi), designated (L), and log (PCR)/(Pi), designated (L*), were calculated from HPLC measurements after rapid freeze-clamping. Increasing CPP from 80-140 cm H2O caused an increase in coronary flow(flow), developed pressure(DevP), O2 consumption (VO2), L, L*, and CO. L and L* were directly related to VO2 and CO. Increasing A from 80-140 cm H2O caused an increase in DevP and VO2, but a decrease in L, L*, and CO. L and L* were inversely linearly related to VO2 but were directly linearly related to CO. In both experiments, L and L* are directly related to CO, suggesting that determination of L* (which can be done with 31P NMR spectroscopy) may be a useful non-invasive method for determining cardiac pump function curves. L and L* may be related to the Frank-Starling mechanism. In a separate experiment using 31P NMR spectroscopy of isovolumic (left ventricular balloon) perfused rat hearts, increasing CPP caused a direct linear increase in flow, DevP, and L*, confirming the L* results reported above with CPP experiments using the rapid freeze-clamp technique

  19. Animal manure phosphorus characterization by sequential chemical fractionation, release kinetics and 31P-NMR analysis

    Tales Tiecher

    2014-10-01

    Full Text Available Phosphate release kinetics from manures are of global interest because sustainable plant nutrition with phosphate will be a major concern in the future. Although information on the bioavailability and chemical composition of P present in manure used as fertilizer are important to understand its dynamics in the soil, such studies are still scarce. Therefore, P extraction was evaluated in this study by sequential chemical fractionation, desorption with anion-cation exchange resin and 31P nuclear magnetic resonance (31P-NMR spectroscopy to assess the P forms in three different dry manure types (i.e. poultry, cattle and swine manure. All three methods showed that the P forms in poultry, cattle and swine dry manures are mostly inorganic and highly bioavailable. The estimated P pools showed that organic and recalcitrant P forms were negligible and highly dependent on the Ca:P ratio in manures. The results obtained here showed that the extraction of P with these three different methods allows a better understanding and complete characterization of the P pools present in the manures.

  20. Raman and 31P MAS NMR spectroscopic studies of lead phosphate glasses containing thorium oxide

    (PbO)0.5(P2O5)0.5 glasses in which part of the PbO/ P2O5 was replaced by ThO2 up to 10 mol% have been prepared by conventional melt quench method and characterized by Raman and 31P MAS NMR spectroscopic studies. Raman studies of these samples clearly revealed the existence of PO4 structural units having two non bridging oxygen atoms attached to phosphorus (PO22-). The 31P MAS NMR studies indicated the presence of two types of phosphorus structural units in both PbO -P2O5 and PbO-P2O5-ThO2 glasses, namely Q2 and Q1 (PO4 structural units with 2 and 1 bridging oxygen atoms respectively). Increase in the concentration of ThO2 at the expense of both PbO/P2O5 has been found to result in the increased amount of Q1 structural units of phosphorus, indicating that ThO2 acts as only a network modifier. ThO2 has been found to form the glassy phase with PbO-P2O5 system only up to 10 mol%. (author)

  1. 31P NMR analysis of membrane phospholipid organization in viable, reversibly electropermeabilized Chinese hamster ovary cells

    Chinese hamster ovary (CHO) cells were reversibly permeabilized by submitting them to short, high-intensity, square wave pulses (1.8 kV/cm, 100 μs). The cells remained in a permeable state without loss of viability for several hours at 40C. A new anisotropic peak with respect to control cells was observed on 31P NMR spectroscopic analysis of the phospholipid components. This peak is only present when the cells are permeable, and normal anisotropy is recovered after resealing. Taking into account the fusogenicity of electropermeabilized cells, comparative studies were performed on 5% poly(ethylene glycol) treated cells. The 31P NMR spectra of the phospholipids displayed the same anisotropic peak as in the case of the electropermeabilized cells. In the two cases, this anisotropic peak was located downfield from the main peak associated to the phospholipids when organized in bilayers. The localization of this anisotropic peak is very different from the one of a hexagonal phase. The authors proposed a reorganization of the polar head group region leading to a weakening of the hydration layer to account for these observations. This was also thought to explain the electric field induced fusogenicity of these cells

  2. Nuclear spin decoherence of neutral 31P donors in silicon: Effect of environmental 29Si nuclei

    Petersen, Evan S.; Tyryshkin, A. M.; Morton, J. J. L.; Abe, E.; Tojo, S.; Itoh, K. M.; Thewalt, M. L. W.; Lyon, S. A.

    2016-04-01

    Spectral diffusion arising from 29Si nuclear spin flip-flops, known to be a primary source of electron spin decoherence in silicon, is also predicted to limit the coherence times of neutral donor nuclear spins in silicon. Here, the impact of this mechanism on 31P nuclear spin coherence is measured as a function of 29Si concentration using X -band pulsed electron nuclear double resonance. The 31P nuclear spin echo decays show that decoherence is controlled by 29Si flip-flops resulting in both fast (exponential) and slow (nonexponential) spectral diffusion processes. The decay times span a range from 100 ms in crystals containing 50% 29Si to 3 s in crystals containing 1% 29Si. These nuclear spin echo decay times for neutral donors are orders of magnitude longer than those reported for ionized donors in natural silicon. The electron spin of the neutral donors "protects" the donor nuclear spins by suppressing 29Si flip-flops within a "frozen core," as a result of the detuning of the 29Si spins caused by their hyperfine coupling to the electron spin.

  3. The A31P missense mutation in cardiac myosin binding protein C alters protein structure but does not cause haploinsufficiency.

    van Dijk, Sabine J; Bezold Kooiker, Kristina; Mazzalupo, Stacy; Yang, Yuanzhang; Kostyukova, Alla S; Mustacich, Debbie J; Hoye, Elaine R; Stern, Joshua A; Kittleson, Mark D; Harris, Samantha P

    2016-07-01

    Mutations in MYBPC3, the gene encoding cardiac myosin binding protein C (cMyBP-C), are a major cause of hypertrophic cardiomyopathy (HCM). While most mutations encode premature stop codons, missense mutations causing single amino acid substitutions are also common. Here we investigated effects of a single proline for alanine substitution at amino acid 31 (A31P) in the C0 domain of cMyBP-C, which was identified as a natural cause of HCM in cats. Results using recombinant proteins showed that the mutation disrupted C0 structure, altered sensitivity to trypsin digestion, and reduced recognition by an antibody that preferentially recognizes N-terminal domains of cMyBP-C. Western blots detecting A31P cMyBP-C in myocardium of cats heterozygous for the mutation showed a reduced amount of A31P mutant protein relative to wild-type cMyBP-C, but the total amount of cMyBP-C was not different in myocardium from cats with or without the A31P mutation indicating altered rates of synthesis/degradation of A31P cMyBP-C. Also, the mutant A31P cMyBP-C was properly localized in cardiac sarcomeres. These results indicate that reduced protein expression (haploinsufficiency) cannot account for effects of the A31P cMyBP-C mutation and instead suggest that the A31P mutation causes HCM through a poison polypeptide mechanism that disrupts cMyBP-C or myocyte function. PMID:26777460

  4. Dynamic stereochemistry of erigeroside by measurement of 1H- 1H and 13C- 1H coupling constants

    Tafazzoli, Mohsen; Ghiasi, Mina; Moridi, Mahdi

    2008-07-01

    Erigeroside was extracted from Satureja khuzistanica Jamzad (Marzeh Khuzistani in Persian, family of lamiaceae), and 1H, 13C, 13C{ 1H}, 1H- 1H COSY, HMQC and J-HMBC were obtained to identify this compound and determine a complete set of J-coupling constants ( 1JC-H, 2JC-H, 3JC-H and 3JH-H) values within the exocyclic hydroxymethyl group (CH 2OH) and anomeric center. In parallel, density functional theory (DFT) using B3LYP functional and split-valance 6-311++G** basis set has been used to optimized the structures and conformers of erigeroside. In all calculations solvent effects were considered using a polarized continuum (overlapping spheres) model (PCM). The dependencies of 1J, 2J and 3J involving 1H and 13C on the C 5'-C 6' ( ω), C 6'-O 6' ( θ) and C 1'-O 1' ( φ) torsion angles in erigeroside were computed using DFT method. Complete hyper surfaces for 1JC1',H1', 2JC5',H6'R, 2JC5',H6'S, 2JC6',H5', 3JC4',H6'R, 3JC4',H6'S and 2JH6'R-H5'S as well as 3JH5',H6'R were obtained and used to derive Karplus equations to correlate these couplings to ω, θ and φ. These calculated J-couplings are in agreement with experimental values. These results confirm the reliability of DFT calculated coupling constants in aqueous solution.

  5. On the thermal behaviour of massive and deposited 12-tungstophosphoric heteropolyacid on 31P NMR data

    The influence of heat treatment on heteropolyacid (HPA) H3PW12O40 · nH2O (HPW), both massive and deposited on γ-Al2O3 and SiO2, has been studied by 31P NMR spectra of solid samples and their aqueous extracts. It is found that HPA state is affected by: 1 - chemical interaction with carrier which results in HPA decomposition as early as the stage of impregnation (on γ-Al2O3); 2 - dispersion of the HPA part not bound with carrier which decreases its thermal stability; 3 - hydrolysis in impregnating solution or in aqueous phase of carrier as a result of carrier leaching. At a high humidity of the air non-fixed part transfers reversibly from the solid state to the aqueous phase formed in carrier pores at the expense of capillary condensation of water vapors. 26 refs., 3 figs., 2 tabs

  6. 31P saturation transfer and phosphocreatine imaging in the monkey brain

    31P magnetic resonance imaging with chemical-shift discrimination by selective excitation has been employed to determine the phosphocreatine (PCr) distribution in the brains of three juvenile macaque monkeys. PCr images were also obtained while saturating the resonance of the γ-phosphate of ATP, which allowed the investigation of the chemical exchange between PCr and the γ-phosphate of ATP catalyzed by creatine kinase. Superposition of the PCr images over the proton image of the same monkey brain revealed topological variations in the distribution of PCr and creatine kinase activity. PCr images were also obtained with and without visual stimulation. In two out of four experiments, an apparently localized decrease in PCr concentration was noted in visual cortex upon visual stimulation. This result is interpreted in terms of a possible role for the local ADP concentration in stimulating the accompanying metabolic response

  7. 31P-NMR studies of Mycoplasma gallisepticum cells using a continuous perfusion technique

    31P-NMR studies of Mycoplasma gallisepticum cells have been carried out using a continuous perfusion technique; these are the first such studies with this organism. Using this technique, glucose metabolism was monitored in the intact organisms, and cell extracts were prepared to identify the intermediates. Under glycolytic conditions, high levels of fructose-1,6-diphosphate were observed, indicating that this sugar may play a key role in the regulation of metabolism. The level of phosphoenolpyruvate was low under normal glycolytic conditions, and did not increase during starvation. From the position of the internal inorganic phosphate peak, the intracellular pH was estimated. The cells were found to maintain an intracellular pH of ∼7.1 over an investigated external pH range of 6.6-8.6. (Auth.)

  8. Effects of anoxia on 31P NMR spectra of Phycomyces blakesleeanus during development

    Stanić Marina

    2009-01-01

    Full Text Available The method of 31P NMR spectroscopy was used to investigate the effects of anoxia on Phycomyces blakesleea­nus mycelium during development. The greatest changes were recorded in the PPc, NADH, and α-ATP signals. Decrease of PPc signal intensity is due to chain length reduction and reduction in number of PPn molecules. Smaller decrease of β-ATP compared to α-ATP signal intensity can be attributed to maintenance of ATP concentration at the expense of PPn hydrolysis. Sensitivity to anoxia varies with the growth stage. It is greatest in 32-h and 44-h mycelium, in which PPn is used as an additional energy source, while the smallest effect was noted for 36-h fungi.

  9. Correlations between /sup 31/P NMR spectroscopy and tumor perfusion in murine RIF-1 tumors

    The authors observed /sup 31/P NMR spectra before and after measurement of tumor perfusion by in situ /sup 15/O activation to search for correlations between tumor blood flow and well perfused fraction and the NMR observables. Their findings indicate that: I) /sup 15/O activation does not alter the NMR observables; II) the pH and the ratio of P/sub i/:NTP are inversely correlated (n = 25, p <0.01); III) the well-perfused fraction of the tumor correlates with pH (n = 11, p <0.01), and correlates inversely with the ratio of P/sub i/:NTP (n = 11, p <0.05); and iv) no correlations are observed between the ratio of PCr:NTP or the rate of perfusion and any of the other variables measured. Their results indicate that biological variability between tumors can mask important conclusions even with standard transplantable tumors

  10. 31P-MR spectroscopy of the human liver - spectral hints on hepatic lymphoma infiltration

    Purpose: To evaluate whether phosphorus magnetic resonance spectroscopy (31P-MRS) enables a non-invasive detection of liver involvement in systemic diseases like Hodgkin's lymphoma. Materials and methods: Using a clinical 1.5 Tesla whole-body MR system image-guided localised phosphorus MR spectra from the anatomically defined volumes of interests were measured. A combination of surface coil, adiabatic excitation pulse and modified impage-selected in vivo spectroscopy (ISIS)-sequence was applied. The spectroscopy data were evaluated quantiatively with a time-domain fit programme using non-linear optimisation algorithms to quantify peak areas. After establishment of the examination protocol, 22 healthy volunteers and 13 patients with suspected lymphoma infiltration of the liver were examined. Results: Liver spectra of patients suffering from lymphoma infiltration differed significantly from spectra of persons with normal liver: 1. The peak area ratio of phosphomonoesters (PME) to β-NTP was elevated in all patients with histologically confirmed liver lymphoma. 2. Patients suffering from Hodgkin's disease with specific or unspecific liver infiltration (n=7) could be differentiated from patients without liver involvement. In case of infiltrated liver, the peak area ratio PME to β-NTP was increased, and the pH value was shifted to lower values. Unambiguous differentiation between non-specific (n=3) and specific (n=4) infiltration of the liver was not possible. 3. In patients after cytostatic treatment (n=3), an increase of the peak area ratio of inorganic phosphate to β-NTP was observed. Conclusion: Our preliminary results indicate that 31P-MRS can yield pointers to liver involvement in patients with systemic diseases such as Hodgkin's disease, which may be hardly detected by imaging methods. (orig.)

  11. Physiologic significance of the phosphorylation potential in isolated perfused rat hearts (31-P NMR)

    Watters, T.; Wikman-Coffelt, J.; Wu, S.; Wendland, M.; James, T.; Sievers, R.; Botvinick, E.; Parmley, W.

    1986-03-05

    The authors assessed the metabolic and mechanical effects of changes in coronary perfusion pressure (CPP) and afterload (A) in isolated working apex-ejecting rat hearts perfused with Krebs-Henseleit solution containing an excess of O/sub 2/ and substrate. Log (phosphorylation potential) or log (ATP)/(ADP)x (Pi), designated (L), and log (PCR)/(Pi), designated (L*), were calculated from HPLC measurements after rapid freeze-clamping. Increasing CPP from 80-140 cm H/sub 2/O caused an increase in coronary flow (flow), developed pressure (DevP), O/sub 2/ consumption (VO/sub 2/), L, L*, and CO. L and L* were directly related to VO/sub 2/ and CO. Increasing A from 80-140 cm H/sub 2/O caused an increase in DevP and VO/sub 2/, but a decrease in L, L*, and CO. L and L* were inversely linearly related to VO/sub 2/ but were directly linearly related to CO. In both experiments, L and L* are directly related to CO, suggesting that determination of L* (which can be done with 31-P NMR spectroscopy) may be a useful non-invasive method for determining cardiac pump function curves. L and L* may be related to the Frank-Starling mechanism. In a separate experiment using 31-P NMR spectroscopy of isovolumic (left ventricular balloon) perfused rat hearts, increasing CPP caused a direct linear increase in flow, DevP, and L*, confirming the L* results reported above with CPP experiments using the rapid freeze-clamp technique.

  12. Physiologic significance of the phosphorylation potential in isolated perfused rat hearts (/sup 31/P NMR)

    Watters, T.; Wikman-Coffelt, J.; Wu, S.; Wendland, M.; James, T.; Sievers, R.; Botvinick, E.; Parmley, W.

    1986-03-05

    The authors assessed the metabolic and mechanical effects of changes in coronary perfusion pressure (CPP) and afterload (A) in isolated working apex-ejecting rat hearts perfused with Krebs-Henseleit solution containing an excess of O/sub 2/ and substrate. Log(phosphorylation potential) or log (ATP)/(ADP)x (Pi), designated (L), and log (PCR)/(Pi), designated (L*), were calculated from HPLC measurements after rapid freeze-clamping. Increasing CPP from 80-140 cm H/sub 2/O caused an increase in coronary flow(flow), developed pressure(DevP), O/sub 2/ consumption (VO/sub 2/), L, L*, and CO. L and L* were directly related to VO/sub 2/ and CO. Increasing A from 80-140 cm H/sub 2/O caused an increase in DevP and VO/sub 2/, but a decrease in L, L*, and CO. L and L* were inversely linearly related to VO/sub 2/ but were directly linearly related to CO. In both experiments, L and L* are directly related to CO, suggesting that determination of L* (which can be done with /sup 31/P NMR spectroscopy) may be a useful non-invasive method for determining cardiac pump function curves. L and L* may be related to the Frank-Starling mechanism. In a separate experiment using /sup 31/P NMR spectroscopy of isovolumic (left ventricular balloon) perfused rat hearts, increasing CPP caused a direct linear increase in flow, DevP, and L*, confirming the L* results reported above with CPP experiments using the rapid freeze-clamp technique.

  13. Altered energy metabolism after myocardial infarction assessed by 31P-MR-spectroscopy in humans

    The value of 31P-magnetic resonance spectroscopy (MRS) as a possible tool to distinguish viable from non-viable tissue after myocardial infarction was analysed in humans. Fifteen patients 3 weeks after anterior myocardial infarction were studied with breath-hold cine MRI and 3D-CSI MRS (1.5 T system). 31P-spectra were obtained from infarcted as well as non-infarcted myocardium (voxel size 25 cm3 each). Gold standard for viability was recovery of regional function, as determined by a control MRI 6 months after revascularization. Ten age-matched healthy volunteers served as control group. No significant difference was found between the phosphocreatine to adenosinetriphosphate (PCr/ATP) ratio of volunteers (SD 1.72±0.31) and non-infarcted septal myocardium of patients. Cine MRI demonstrated recovery of regional function in 10 patients, i. e. 10 patients showed viable and 5 non-viable myocardium. In viable myocardium, the PCr/ATP ratio was 1.47±0.38 (non-significant vs volunteers; p>0.05). In the 5 patients with akinetic myocardium, PCr peaks could not be detected. Therefore, calculation of PCr/ATP ratios was not possible. However, a significant reduction of the ATP signal-to-noise ratio (SNR) was observed (2.92±0.73 vs 6.68±0.80; patients vs volunteers; p<0.05). The SNR of ATP of akinetic regions may predict recovery of function after revascularization in patients with myocardial infarction. (orig.)

  14. 31P magnetization transfer measurements of Pi→ATP flux in exercising human muscle

    Savage, David B.; Williams, Guy B.; Porter, David; Carpenter, T. Adrian; Brindle, Kevin M.; Kemp, Graham J.

    2016-01-01

    Fundamental criticisms have been made over the use of 31P magnetic resonance spectroscopy (MRS) magnetization transfer estimates of inorganic phosphate (Pi)→ATP flux (VPi-ATP) in human resting skeletal muscle for assessing mitochondrial function. Although the discrepancy in the magnitude of VPi-ATP is now acknowledged, little is known about its metabolic determinants. Here we use a novel protocol to measure VPi-ATP in human exercising muscle for the first time. Steady-state VPi-ATP was measured at rest and over a range of exercise intensities and compared with suprabasal oxidative ATP synthesis rates estimated from the initial rates of postexercise phosphocreatine resynthesis (VATP). We define a surplus Pi→ATP flux as the difference between VPi-ATP and VATP. The coupled reactions catalyzed by the glycolytic enzymes GAPDH and phosphoglycerate kinase (PGK) have been shown to catalyze measurable exchange between ATP and Pi in some systems and have been suggested to be responsible for this surplus flux. Surplus VPi-ATP did not change between rest and exercise, even though the concentrations of Pi and ADP, which are substrates for GAPDH and PGK, respectively, increased as expected. However, involvement of these enzymes is suggested by correlations between absolute and surplus Pi→ATP flux, both at rest and during exercise, and the intensity of the phosphomonoester peak in the 31P NMR spectrum. This peak includes contributions from sugar phosphates in the glycolytic pathway, and changes in its intensity may indicate changes in downstream glycolytic intermediates, including 3-phosphoglycerate, which has been shown to influence the exchange between ATP and Pi catalyzed by GAPDH and PGK. PMID:26744504

  15. Application of localized {sup 31}P MRS saturation transfer at 7 T for measurement of ATP metabolism in the liver: reproducibility and initial clinical application in patients with non-alcoholic fatty liver disease

    Valkovic, Ladislav [Medical University of Vienna, High Field MR Centre, Department of Biomedical Imaging and Image-guided Therapy, Vienna (Austria); Slovak Academy of Sciences, Department of Imaging Methods, Institute of Measurement Science, Bratislava (Slovakia); Gajdosik, Martin; Chmelik, Marek; Trattnig, Siegfried [Medical University of Vienna, High Field MR Centre, Department of Biomedical Imaging and Image-guided Therapy, Vienna (Austria); Traussnigg, Stefan; Kienbacher, Christian; Trauner, Michael [Medical University of Vienna, Division of Gastroenterology and Hepatology, Department of Internal Medicine III, Vienna (Austria); Wolf, Peter; Krebs, Michael [Medical University of Vienna, Division of Endocrinology and Metabolism, Department of Internal Medicine III, Vienna (Austria); Bogner, Wolfgang [Medical University of Vienna, High Field MR Centre, Department of Biomedical Imaging and Image-guided Therapy, Vienna (Austria); Harvard Medical School, Athinoula A. Martinos Center for Biomedical Imaging, Department of Radiology, Massachusetts General Hospital, Boston, MA (United States); Krssak, Martin [Medical University of Vienna, High Field MR Centre, Department of Biomedical Imaging and Image-guided Therapy, Vienna (Austria); Medical University of Vienna, Division of Endocrinology and Metabolism, Department of Internal Medicine III, Vienna (Austria)

    2014-07-15

    Saturation transfer (ST) phosphorus MR spectroscopy ({sup 31}P MRS) enables in vivo insight into energy metabolism and thus could identify liver conditions currently diagnosed only by biopsy. This study assesses the reproducibility of the localized {sup 31}P MRS ST in liver at 7 T and tests its potential for noninvasive differentiation of non-alcoholic fatty liver (NAFL) and steatohepatitis (NASH). After the ethics committee approval, reproducibility of the localized {sup 31}P MRS ST at 7 T and the biological variation of acquired hepato-metabolic parameters were assessed in healthy volunteers. Subsequently, 16 suspected NAFL/NASH patients underwent MRS measurements and diagnostic liver biopsy. The Pi-to-ATP exchange parameters were compared between the groups by a Mann-Whitney U test and related to the liver fat content estimated by a single-voxel proton ({sup 1}H) MRS, measured at 3 T. The mean exchange rate constant (k) in healthy volunteers was 0.31 ± 0.03 s{sup -1} with a coefficient of variation of 9.0 %. Significantly lower exchange rates (p < 0.01) were found in NASH patients (k = 0.17 ± 0.04 s{sup -1}) when compared to healthy volunteers, and NAFL patients (k = 0.30 ± 0.05 s{sup -1}). Significant correlation was found between the k value and the liver fat content (r = 0.824, p < 0.01). Our data suggest that the {sup 31}P MRS ST technique provides a tool for gaining insight into hepatic ATP metabolism and could contribute to the differentiation of NAFL and NASH. (orig.)

  16. Phosphorus in chronosequence of burnt sugar cane in Brazilian cerrado: humic acid analysis by {sup 31}P NMR; Fosforo em cronossequencia de cana-de-acucar queimada no cerrado goiano: analise de acidos humicos por RMN de {sup 31}P

    Rossi, Celeste Q.; Pereira, Marcos G.; Garcia, Andreas C., E-mail: mgervasiopereira@gmail.com [Universidade Federal Rural do Rio de Janeiro (UFRRJ), Seropedica, RJ (Brazil). Dept. de Solos; Perin, Adriano; Gazolla, Paulo R. [Instituto Federal de Educacao, Ciencia e Tecnologia Goiano, Rio Verde, GO (Brazil); Gonzalez, Antonio P. [Universidade de Coruna, ES (Spain). Faculdad de Ciencias

    2013-10-01

    The aim of this study was to identify, with the use of {sup 31}P NMR spectroscopy, organic P species in humic acids (HA) in samples from Oxisol cultivated in chronosequence with sugar cane, pasture and Cerrado. The main forms of P-type found were orthophosphate, monoester-P (phosphate sugars) and P-diester (orthophosphate). The {sup 31}P NMR technique proved capable of identifying changes in the areas studied as a function of sugar cane burning time. In areas with 1 and 5 years of burnt cane, a decrease in recalcitrant organic P in humic acids indicated the need for use of P-humic substances for plant nutrition (author)

  17. Quantitative analysis of energy metabolism in human muscle using SLOOP {sup 31}P-MR-spectroscopy

    Beer, M.; Koestler, H.; Buchner, S.; Sandstede, J.; Hahn, D. [Wuerzburg Univ. (Germany). Inst. fuer Roentgendiagnostik; Schneider, C.; Toyka, K.V. [Neurologische Klinik und Poliklinik der Univ. Wuerzburg (Germany)

    2002-05-01

    Objective: Energy metabolism is vital for regular muscle function. In humans, in vivo analysis using {sup 31}P-MR-spectroscopy (MRS) is mostly restricted to semiquantitative parameters due to technical demands. We applied spatial localization with optimal pointspread function (SLOOP) for quantification in human skeletal and cardiac muscle. Subjects/Methods: 10 healthy volunteers and 4 patients with myotonic dystrophy type 1 were examined using a 1.5 T system (Magnetom VISION) and chemical shift imaging (CSI) for data collection. Concentrations of PCr, ATP and P{sub i} as well as PCr/ATP ratios were calculated by SLOOP. Results: Concentrations of PCr, ATP and P{sub i} were 29.9{+-}3.4, 7.1{+-}0.9 and 5.7{+-}1.2 [mmol/kg] in normal skeletal muscle, corresponding to previously published studies. Two of the patients with a duration of disease longer than 10 years and a pronounced muscle weakness showed a significant decrease of PCr and ATP in skeletal muscle below 10 and 5 mmol/kg. One of these patients had an additional reduction of PCr in cardiac muscle. (orig.) [German] Ziel: Voraussetzung fuer eine regulaere Muskelfunktion ist ein intakter Energiestoffwechsel. Beim Menschen beschraenkten sich bisherige Untersuchungen mittels der {sup 31}P-MR-Spektroskopie (MRS), welche eine In-Vivo-Analyse erlaubt, jedoch zumeist auf die Analyse semiquantitativer Parameter. Wir verwendeten Spatial Localization with Optimal Pointspread Function (SLOOP), um den Stoffwechsel des Skelettmuskels wie des Herzens zu quantifizieren. Patienten/Methoden: 10 Probanden und 4 Patienten mit myotoner Dystrophie Typ 1 wurden an einem 1.5-T-System (Magnetom VISION) mittels der chemical shift imaging (CSI)-Technik untersucht. Die Berechnung der Konzentrationen von PCr, ATP und P{sub 1} sowie des PCr/ATP Verhaeltnisses erfolgte mittels SLOOP. Ergebnisse: Im Skelettmuskel gesunder Probanden betrugen die Absolutkonzentrationen fuer PCr, ATP und P{sub i} 29,9{+-}3.4, 7,1{+-}0,9 und 5,7{+-}1,2 [mmol

  18. 31P-NMR study of reduction mechanism of 12-molybdophosphoric acid

    Chemical species of unreduced and reduced 12-molybdophosphoric acid and their reaction have been investigated in concentrated aqueous and 50 % water-dioxane solutions using 31P-NMR and polarography. Phosphorus-31 chemical shifts of α- and β-PMo12 in the range of the degree of reduction among 0 and 4 were obtained in 50 % water-dioxane. 31P-NMR study clarified the isomerization and disproportionation behavior of unreduced and reduced PMo12 in concentrated solutions and made it possible to estimate approximate half-life periods for each step. Isomerization of β-PMo12(0) to α-PMo12(o) was immediate in water and rapid in 50 % water-dioxane. The two-electron reduced product of α-PMo12(0) in 50 % water-dioxane was α-PMo12(II) while that in water was a mixture of α-PMo12(0), β-PMo12(II) and β-PMo12(IV). This is attributed to the isomerization of first-formed α-PMo12(II) to β-PMo12(II) which dispreportionates quickly to β-PMo12(IV) and β-PMo12(0), the latter of which is then reduced to β-PMo12(II) or isomerizes to α-PMo12(0) immediately. β-PMo12(IV) was the only stable species in four-electron reduced products of α-PMo12(0) both in water and in 50 % water-dioxane since α-PMo12(IV) gradually isomerized to β-PMo12(IV). Two routes are proposed for the reduction of α-PMo12(0) to β-PMo12(IV) in solutions. Strong reducing agents such as ascorbic acid in a sufficient amount take the following route: α-PMo12(0) → α-PMo12(II) → α-PMo12(IV) → β-PMo12(IV). However, even milder reducing agents incapable of reducing α-PMo12(II) can produce β-PMo12(IV) in water through the other route. (Nogami, K.)

  19. Relation Between Acid and Catalytic Properties of Chlorinated Gamma-Alumina. a 31p Mas Nmr and Ftir Investigation

    Guillaume D.

    1999-07-01

    Full Text Available In this paper, we have studied the effect of chlorine on the surface properties of gamma-alumina, especially on their acid properties. The use of FTIR spectroscopy and 31P MAS NMR of adsorbed trimethylphosphine allows to propose a chlorination mechanism. To correlate the surface properties of these chlorinated gamma-alumina with their catalytic properties, we have used a model reaction, the cracking of n-heptane under reforming conditions. The analysis of the correlation between acid properties determined by 31P MAS NMR and the catalytic results (in terms of activities and selectivities allows to identify which sites are involved in the cracking reaction.

  20. Early results of in-vivo 31P-NMR spectroscopy of the spleen in patients with splenomegaly

    In-vivo 31P-NMR spectroscopy of the spleen was carried out in 15 patients with splenomegaly from various causes (Hodgkin's disease, non-Hodgkin lymphoma, polycythaemia vera, chronic lymphatic leukaemia, chronic myeloid leukaemia). Vome selection was with the ISIS technique, voxel size was between 3x5x5 and 8x6x7 cm3. There was a markedly elevated (PM+Pi)/β-NTP quotient (mean 3.41 with a standard deviation of 0.37) (p31P-NMR spectroscopy for defining splenic involvement in myeloproliferative diseases but further confirmatory studies will be necessary. (orig.)

  1. Lipid Dynamics Studied by Calculation of 31P Solid-State NMR Spectra Using Ensembles from Molecular Dynamics Simulations

    Hansen, Sara Krogh; Vestergaard, Mikkel; Thøgersen, Lea; Schiøtt, Birgit; Nielsen, Niels Christian; Vosegaard, Thomas

    2014-01-01

    We present a method to calculate 31P solid-state NMR spectra based on the dynamic input from extended molecular dynamics (MD) simulations. The dynamic information confered by MD simulations is much more comprehensive than the information provided by traditional NMR dynamics models based on, for...... example, order parameters. Therefore, valuable insight into the dynamics of biomolecules may be achieved by the present method. We have applied this method to study the dynamics of lipid bilayers containing the antimicrobial peptide alamethicin, and we show that the calculated 31P spectra obtained with...

  2. Phosphorus in chronosequence of burnt sugar cane in Brazilian cerrado: humic acid analysis by 31P NMR

    The aim of this study was to identify, with the use of 31P NMR spectroscopy, organic P species in humic acids (HA) in samples from Oxisol cultivated in chronosequence with sugar cane, pasture and Cerrado. The main forms of P-type found were orthophosphate, monoester-P (phosphate sugars) and P-diester (orthophosphate). The 31P NMR technique proved capable of identifying changes in the areas studied as a function of sugar cane burning time. In areas with 1 and 5 years of burnt cane, a decrease in recalcitrant organic P in humic acids indicated the need for use of P-humic substances for plant nutrition (author)

  3. 31P-MR spectroscopy of liver abnormalities with reference to varying pulse recovery times

    The value of 31P-MRS for different types of liver disease and the effect of repetition time (TR) on measurements of relative phosphor metabolite concentrations was studied. Spectroscopy was performed on 26 patients with predominantly focal liver disease and on 14 normals, using a 1.5 Tesla clinical MR system. In all cases, (TR) of 2,400 ms was chosen and in 11 patients and 10 normals additionally shorter (TR) of 600 ms (with T1 weighted spectra) was chosen. The results show that PME/β-ATP and PDE/β-ATP are sensitive indicators of liver disease and differ widely from the findings in normal livers. In patients with liver metastases, the long (TR) of 2,400 ms (16 cases) showed an increase of PME/β-ATP (0.96±0.32) and significant reduction of PDE/β-ATP (1.89±0.47) as compared with normals (PME/β-ATP=0.75±0.26 and PDE/β-ATP=2.27±0.41), for a (TR) of 600 ms, PME/β-ATP (0.87±0.47) and PDE/β-ATP (1.82±0.67) are significantly increased. T1 weighted spectra showed more significant differences in phosphometabolites between patients and normals than density weighted spectra. The spectra in patients showed a significantly reduced signal to noise ratio independent of the (TR). (orig.)

  4. A study of fatigue in rabbit skeletal muscle by in vivo 31P MRS

    Energy metabolism during exercise and recovery process of rabbit skeletal muscle was obserbed by in vivo 31P MRS. The small value of the ratio of the intensities between inorganic phosphate and phosphocreatine at rest indicated that the observed moiety of muscle had high fast-twitch fiber content. More than half of ATP and almost all of phosphocreatine were depleted by electric stimulation at 4Hz. The extreme intracellular pH was 5.9. The recovery from this metabolic state was very slow, and only a small amount of ATP was resynthesized after 40 minutes of recovery. These phenomena show the characteristic features of the energy metabolism in the fatigue of fast-twitch muscle. The metabolic state as indicated by the intensity of phosphocreatine and intracellular pH during exercise was not always parallel to contraction power measured by straingauge. Two inorganic phosphate peaks were observed, which are regarded as the signals from fast-twitch fiber and slow-twitch fiber from their pH values. The ratios of these two peaks were different between 1Hz, 2Hz, and 4Hz electric stimulation. We conclude that we are observing the different recruitment of fiber types at different exercise level in vivo. (author)

  5. Hypoxic stress, tumor cell survival and /sup 31/P-NMR spectrometry

    The authors have studied the /sup 31/P-NMR spectral characteristics of a variety of transplantable tumors in situ. These tumors demonstrate the presence of phosphorylocholine, phosphorylethanolamine; inorganic phosphate; glycerolphosphorylcholine, glycerolphosphorylethanolamine; phosphocreatine; and, nucleoside di- and triphosphates. Sensitivity has been improved by use of a 15 mm id solenoidal coil which allows spectrometry of tumors of -- 300 mg. Two tumor models were used to assess the influence of N/sub 2/ asphyxiation and tumor cell survival. Mice bearing s.c. 16/C mammary adenocarcinoma were N/sub 2/ asphyxiated within the NMR spectrometer and tumors excised after various durations of hypoxia for endpoint dilution analysis. Similar protocols using the RIF-1 tumor and clonogenic assay were also employed. The TD/sub 50/ assay using the 16/C mammary tumor indicated that the tumorigenic cells were most vulnerable during the initial adaptation to anoxia (0-13 min). Further delay in tumor excision following N/sub 2/ asphyxiation or simple tumor excision and incubation at 370C was without effect (2 hrs). Cell yield from either tumor was not influenced by hypoxic stress. Trypan blue dye exclusion was suspect due to a detectable decline of intracellular high energy phosphates

  6. 31P-nuclear magnetic resonance studies of chronic myocardial ischemia in the Yucatan micropig.

    Rath, D P; Bailey, M; Zhang, H; Jiang, Z; Abduljalil, A M; Weisbrode, S; Hamlin, R L; Robitaille, P M

    1995-01-01

    In this work, an x-irradiation/high fat/high cholesterol diet-induced atherogenic model was invoked to examine the effects of severe diffuse atherosclerosis on myocardial metabolism in the in vivo porcine heart. This model was studied using spatially localized 31P-nuclear magnetic resonance (NMR) to monitor pH and the levels of inorganic phosphate, phosphomonoesters, creatine phosphate, and adenosine triphosphate as a function of workload transmurally in control swine and in animals suffering from chronic ischemic heart disease. These preliminary studies revealed that the development of severe atherosclerosis and the accompanying chronically diseased state produce changes in high energy phosphates and that increases in rate pressure products result in demonstrable signs of ischemia in the myocardium which span the entire left ventricular wall. Ischemic changes include a global increase in inorganic phosphate and corresponding decreases in creatine phosphate, ATP, and pH. Importantly, changes in intracellular pH are noted with even the slightest increase in workload suggesting that these diseased hearts display elevated glycolytic activity. By challenging these animals with increased cardiac workload, we directly visualize how the chronically compromised heart responds to severe oxygen challenges in a clinically relevant model of this situation. PMID:7814609

  7. Phases formed upon thermolysis of H3PMo12O40 heteropolyacid by 31P NMR

    (MoO2)(HPO4) (1) and (MoO2)2(P2O7) (2) molybdenyl phosphate 31P NMR spectra are measured, synthesis is performed and a conclusion is made that heteropolyacid (HPA) H3PM12O40 is decomposed under thermolysis in two directions: into MoO3 and 1 at t∼400 deg C (1) and into MoO3 and 2 att ∼500 deg C (2) through PMo12O385 anhydride phase. Conditions of HPA heat treatment, determining the degree of preliminary loss of structural water affect the ratio of directions. Phases 1 and 2 in thermolysis products are highly dispersed, therefore 1 is preserved in them at up to 650-700 deg C while massive 1 is transformed in 2 at up to 400 deg C. Molybdenyl phosphate complexes are observed in mother liquors of 1 synthesis with the ratio P:M ≥1 and [Mo]∼1 mol/l along 95Mo NMR lines with δ=-66 and -103 m.d. 16 refs., 3 figs., 2 tabs

  8. 31P-nuclear magnetic resonance analysis of extracts of vascular smooth muscle

    31P-nuclear magnetic resonance spectroscopy was used to assess phosphate metabolites in perchloric acid extracts of rabbit aorta. In addition to the high energy phosphates, several other phosphorus compounds were detected and quantified. Most notable was the presence of a prominent phosphomonoester compound appearing at a chemical shift of 3.86 delta. This compound constituted 26% of the total extractable tissue phosphorus and is tentatively identified as ribose-5-phosphate, a pentose phosphate pathway intermediate. While ATP and phosphocreatine did not change during glucose and oxygen deprivation or during prolonged muscle contraction, the 3.86delta phosphate decreased significantly. Furthermore, theophylline, an agent that increases intracellular cAMP, also decreased the level of the 3.86 delta phosphate. These results are consistent with the concept that intermediate metabolism sustains high energy phosphate pools in vascular smooth muscle in the steady state under various conditions. The pentose phosphate pathway may play an important role in vascular smooth muscle metabolism. (author)

  9. Analysis of cardiac energy metabolism in valve disease using 31P-MR-spectroscopy

    Patients and methods: 10 healthy volunteers and 10 patients with aortic stenosis (pressure gradients >60 mmHg) were included. For assessment of energy metabolism, 31P-MR spectra were obtained with a double oblique 3D-CSI technique (voxel size 25 cm3). In 5 of 10 patients, follow-up examination was performed 3 months after surgical valve replacement (SVR). Left ventricular (LV) function was analyzed by cine MRI. Results: Before SVR the myocardial phosphocreatine to adenosinetriphosphate (PCr-ATP) ratio was significantly (p=0.0002) reduced to 0.80±0.25 in patients compared to 1.65±0.21 in volunteers. 3 months after SVR, LV mass had significantly (p=0.04) decreased from 238±33 g to 206±47 g. At the same time a significant (p=0.04) increase of the PCr-ATP ratio from 0.80±0.25 to 1.28±0.22 was observed. A slight, but not significant, reduction of the phosphodiester ATP ratio was observed before SVR, with a trend towards normalization after SVR. (orig.)

  10. The structure of phosphate glass biomaterials from neutron diffraction and 31P nuclear magnetic resonance data

    Neutron diffraction and 31P nuclear magnetic resonance spectroscopy were used to probe the structure of phosphate glass biomaterials of general composition (CaO)0.5-x(Na2O)x(P2O5)0.5 (x = 0, 0.1 and 0.5). The results suggest that all three glasses have structures based on chains of Q2 phosphate groups. Clear structural differences are observed between the glasses containing Na2O and CaO. The P-O bonds to bridging and non-bridging oxygens are less well resolved in the neutron data from the samples containing CaO, suggesting a change in the nature of the bonding as the field strength of the cation increases Na+ → Ca2+. In the (CaO)0.5(P2O5)0.5 glass most of the Ca2+ ions are present in isolated CaOx polyhedra whereas in the (Na2O)0.5(P2O5)0.5 glass the NaOx polyhedra share edges leading to a Na-Na correlation. The results of the structural study are related to the properties of the (CaO)0.4(Na2O)0.1(P2O5)0.5 biomaterial

  11. (31)P NMR phospholipid profiling of soybean emulsion recovered from aqueous extraction.

    Yao, Linxing; Jung, Stephanie

    2010-04-28

    The quantity and composition of phospholipids in full-fat soybean flour, flakes, and extruded flakes and in the cream fraction recovered after aqueous extraction (AEP) and enzyme-assisted aqueous extraction (EAEP) of these substrates were studied with (31)P NMR. Extruded flakes had significantly more phosphatidic acid (PA) than flakes and flour prior to aqueous extraction. The PA content of the cream recovered after AEP and EAEP of extruded flakes was similar to that of the starting material, whereas the PA content of the creams from flour and flakes significantly increased. Changes in the PA content could be explained by the action of phospholipase D during the processing step and aqueous extraction. Total phospholipids in the oil recovered from the creams varied from 0.09 to 0.75%, and free oil yield, which is an indicator of cream stability, varied from 6 to 78%. Total phospholipid did not correlate with emulsion stability when it was lower than 0.20%. Inactivation of phospholipase D prior to aqueous extraction of flour resulted in a cream emulsion less stable toward enzymatic demulsification and containing less PA and total phospholipids than untreated flour. The phospholipid distributions in the cream, skim, and insolubles obtained from AEP flour were 7, 51, and 42%, respectively. PMID:20329795

  12. Bioenergetic measurements in children with bipolar disorder: a pilot 31P magnetic resonance spectroscopy study.

    Elif M Sikoglu

    Full Text Available BACKGROUND: Research exploring Bipolar Disorder (BD phenotypes and mitochondrial dysfunction, particularly in younger subjects, has been insufficient to date. Previous studies have found abnormal cerebral pH levels in adults with BD, which may be directly linked to abnormal mitochondrial activity. To date no such studies have been reported in children with BD. METHODS: Phosphorus Magnetic Resonance Spectroscopy ((31P MRS was used to determine pH, phopshocreatine (PCr and inorganic phosphate (Pi levels in 8 subjects with BD and 8 healthy comparison subjects (HCS ages 11 to 20 years old. RESULTS: There was no significant difference in pH between the patients and HCS. However, frontal pH values for patients with BD increased with age, contrary to studies of HCS and the pH values in the frontal lobe correlated negatively with the YMRS values. Global Pi was significantly lower in subjects with BD compared with HCS. There were no significant differences in PCr between the groups. Global PCr-to-Pi ratio (PCr/Pi was significantly higher in subjects with BD compared with HCS. CONCLUSIONS: The change in Pi levels for the patients with BD coupled with the no difference in PCr levels, suggest an altered mitochondrial phosphorylation. However, our findings require further investigation of the underlying mechanisms with the notion that a mitochondrial dysfunction may manifest itself differently in children than that in adults. LIMITATIONS: Further investigations with larger patient populations are necessary to draw further conclusions.

  13. Quantitative analysis of energy metabolism in human muscle using SLOOP 31P-MR-spectroscopy

    Objective: Energy metabolism is vital for regular muscle function. In humans, in vivo analysis using 31P-MR-spectroscopy (MRS) is mostly restricted to semiquantitative parameters due to technical demands. We applied spatial localization with optimal pointspread function (SLOOP) for quantification in human skeletal and cardiac muscle. Subjects/Methods: 10 healthy volunteers and 4 patients with myotonic dystrophy type 1 were examined using a 1.5 T system (Magnetom VISION) and chemical shift imaging (CSI) for data collection. Concentrations of PCr, ATP and Pi as well as PCr/ATP ratios were calculated by SLOOP. Results: Concentrations of PCr, ATP and Pi were 29.9±3.4, 7.1±0.9 and 5.7±1.2 [mmol/kg] in normal skeletal muscle, corresponding to previously published studies. Two of the patients with a duration of disease longer than 10 years and a pronounced muscle weakness showed a significant decrease of PCr and ATP in skeletal muscle below 10 and 5 mmol/kg. One of these patients had an additional reduction of PCr in cardiac muscle. (orig.)

  14. 1H-Tetrazole as Catalyst in Phosphomorpholidate Coupling Reactions : Efficient Synthesis of GDP-Fucose, GDP-Mannose, and UDP-Galactose

    Wittmann, Valentin; Wong, Chi-Huey

    1997-01-01

    An improved procedure is described for the efficient and high-yield (76-91%) synthesis of nucleoside diphosphate sugars from the readily available nucleoside 5'-monophosphomorpholidate and sugar 1-phosphate in the presence of 1H-tetrazole. Comparative kinetic investigations by means of (31)P NMR spectroscopy with different additives (1,2,4-triazole, acetic acid, N-hydroxysuccinimide, 4-(dimethylamino)pyridine hydrochloride, perchloric acid) and mass spectrometric analysis suggest that tetrazo...

  15. Preservation of bilayer structure in human erythrocytes and erythrocyte ghosts after phospholipase treatment : A 31P-NMR study

    Meer, G. van; Kruijff, B. de; Kamp, J.A.F. op den; Deenen, L.L.M. van

    1980-01-01

    1. 1. Fresh human erythrocytes were treated with lytic and non-lytic combinations of phospholipases A2, C and sphingomyelinase. The 31P-NMR spectra of ghosts derived from such erythrocytes show that, in all cases, the residual phospholipids and lysophospholipids remain organized in a bilayer configu

  16. In vivo measurements of T1 relaxation times of 31P-metabolites in human skeletal muscle

    Thomsen, C; Jensen, K E; Henriksen, O

    1989-01-01

    The T1 relaxation times were estimated for 31P-metabolites in human skeletal muscle. Five healthy volunteers were examined in a 1.5 Tesla wholebody imaging system using an inversion recovery pulse sequence. The calculated T1 relaxation times ranged from 5.517 sec for phosphocreatine to 3.603 sec...

  17. INVIVO 31P MAGNETIC-RESONANCE SPECTROSCOPY (MRS) OF TENDER POINTS IN PATIENTS WITH PRIMARY FIBROMYALGIA SYNDROME

    DEBLECOURT, AC; WOLF, RF; VANRIJSWIJK, MH; KAMMAN, RL; KNIPPING, AA; MOOYAART, EL

    1991-01-01

    31P Magnetic Resonance-Spectroscopy was performed at the site of tender points in the trapezius muscle of patients with primary fibromyalgia syndrome. Earlier, in vitro studies have reported changes in the high energy phosphate-metabolism in biopsies taken from tender points of fibromyalgia patients

  18. Intermolecular (119)Sn,(31)P Through-Space Spin-Spin Coupling in a Solid Bivalent Tin Phosphido Complex.

    Arras, Janet; Eichele, Klaus; Maryasin, Boris; Schubert, Hartmut; Ochsenfeld, Christian; Wesemann, Lars

    2016-05-01

    A bivalent tin complex [Sn(NP)2] (NP = [(2-Me2NC6H4)P(C6H5)](-)) was prepared and characterized by X-ray diffraction and solution and solid-state nuclear magnetic resonance (NMR) spectroscopy. In agreement with the X-ray structures of two polymorphs of the molecule, (31)P and (119)Sn CP/MAS NMR spectra revealed one crystallographic phosphorus and tin site with through-bond (1)J((117/119)Sn,(31)P) and through-space (TS)J((117/119)Sn,(31)P) spin-spin couplings. Density functional theory (DFT) calculations of the NMR parameters confirm the experimental data. The observation of through-space (TS)J((117/119)Sn,(31)P) couplings was unexpected, as the distances of the phosphorus atoms of one molecule and the tin atom of the neighboring molecule (>4.6 Å) are outside the sum of the van der Waals radii of the atoms P and Sn (4.32 Å). The intermolecular Sn···P separations are clearly too large for bonding interactions, as supported by a natural bond orbital (NBO) analysis. PMID:27071033

  19. Associative ionization of neon and helium atoms by collisions of excited helium (31p) atoms of thermal energies

    The relative cross-sections of ionizing collisions between He + He and He + Ne atoms, have been studied, the helium being excited in a state (31p) by a laser beam. The results obtained made it possible (a) to reveal in a direct manner the production of molecular ions He2+ and He Ne+ and (b) to determine the relative change in the associative ionizing cross-section in the area (0.035 - 0.17 eV) in the He (31P) + Ne collision, despite the very short life of the He (31P) excited state (1.7 ns). The production of He2+ ions from an He (3 1P) + He collision sets an upper limit to the appearance potential of these ions. The experimental study of the associative ionization in the He (31P) + Ne system made it possible to extend the utilization of the GAMMA(R) self ionization model, already tested for the metastable states, to the radiative states. The GAMMA(R) model seems well suited for the description of collisions of the A excited + B type, where the excitation energy of A is greater than the ionization potential of B

  20. Improved energy kinetics following high protein diet in McArdle's syndrome. A 31P magnetic resonance spectroscopy study

    Jensen, K E; Jakobsen, J; Thomsen, C;

    1990-01-01

    A patient with McArdle's syndrome was examined using bicycle ergometry and 31P NMR spectroscopy during exercise. The patients working capacity was approximately half the expected capacity of controls. Muscle energy kinetics improved significantly during intravenous glucose infusion and after 6...

  1. Chloride dependence of intracellular pH in frog skin: a 31P NMR study

    Single frog skins from Northern Variety Rana pipiens were analyzed by 31P NMR spectroscopy during superfusion alternately with control and experimental Ringer's solutions, permitting each preparation to serve as its own control. The spectral positions of intracellular inorganic phosphate and extracellular methylphosphonate permitted continuous monitoring of intracellular (pH/sub c/) and extracellular (pH0) pH, respectively. Acute and steady state measurements suggested that pH/sub c/ is well regulated at about 7.29 +- 0.05 over an external pH range of about 7.25-7.65. Below this range, pH/sub c/ decreased markedly when the external pH was reduced with nonvolatile acid. In the presence of 2.5 mM HCO3- and 1% CO2, total substitution of external Cl- by gluconate reversibly increased pH/sub c/ by 0.34 +- 0.05 U (mean +- SE). Replacing external Cl- by SO2-4 increased pH/sub c/ by 0.12 +- 0.01 in the presence of external HCO-3, but only by 0.05 +- 0.02 in its absence. SITS (1 mM) at a pH0 of 6.95 +- 0.05 did not significantly alter pH/sub c/, but entirely prevented the steady state alkalinization characteristically induced by gluconate substitution for external Cl-. The results document that: (1) intracellular pH is maintained relatively constant when the external pH is varied over the physiologic range by adding fixed acid or base, and (2) this regulation is (at least in part) a reflection of Cl/HCO3 antiport activity

  2. Electron diffraction and 31P and 27Al NMR studies of aluminium phospate

    Full text: Various forms of aluminium phosphate were crystallised using a variety of fluxes. Selected area electron diffraction showed that preparations of the tridymite form of aluminium phosphate consists of hexagonal sheets of aluminium phosphate stacked in regular random or irregular stacking. The stacking depends on the preparation conditions. Undoped AlPO4 or AlPO4 doped with trivalent cations such as Fe3+ or Cr3+ exhibit a mixture of hexagonal, h, and cubic, c, sequences of layers corresponding to ABA and ABC stacking respectively of successive layers. Doping with 0.1 mole percent of divalent impurities such as Ni2+ or Co2+ with simultaneous doping by Li+ to maintain charge neutrality stabilised pure hexagonal stacking. The 31P and 27Al NMR of samples of AlPO4 with quartz, tridymite, and cristobalite structures gave characteristic peaks that were clearly distinguished. Samples with the quartz and cristobalite structures gave sharp resonances but a sample with the tridymite structure gave a broad resonance if it had random stacking of layers as evidenced by diffraction. However samples prepared with regular stacking gave a resonance that was clearly resolved into two peaks are attributed to hexagonal or cubic stacking sequences of layers respectively. The tridymite form of aluminium phosphate that was undoped or doped with trivalent impurities always showed the two peaks. For the aluminium phosphate doped with divalent impurities the peak indentified as arising from hexagonal stacking of layers predominated with only a weak shoulder from the cubic stacking. The doped aluminium phosphate samples were yellow for Fe3+, blue for Co2+, green for Ni2+, and pink for Cr2+. Further studies using electron paramagnetic resonance and cathodoluminesence are planned to elucidate the nature of these colour centres. Copyright (2002) Australian Society for Electron Microscopy Inc

  3. Gated 31P NMR study of tetanic contraction in rat muscle depleted of phosphocreatine

    Rats were fed a diet containing 1% β-guanidino-propionic acid (GPA) for 6-12 wk to deplete their muscles of phosphocreatine (PCr). Gated 31P nuclear magnetic resonance (NMR) spectra were obtained from the gastrocnemius-plantaris muscle at various time points during either a 1- or 3-s isometric tetanic contraction using a surface coil. The energy cost of a 1-s tetanus in unfatigued control rat muscle was 48.4 μmol ATP x g dry wt-1 x s-1 and was largely supplied by PCr; anaerobic glycogenolysis was negligible. In GPA-fed rats PCr was undetectable after 400 ms. This had no effect on initial force generated per gram, which was not significantly different from controls. Developed tension in a 3-s tetanus in GPA-fed rats could be divided into a peak phase (duration 0.8-0.9 s) and a plateau phase (65% peak tension) in which PCr was undetectable and the [ATP] was < 20% of that in control muscle. Energy from glycogenolysis was sufficient to maintain force generation at this submaximal level. Mean net glycogen utilization per 3-s tetanus was 78% greater than in control muscle. However, the observed decrease in intracellular pH was less than that expected from energy budget calculations, suggesting either increased buffering capacity or modulation of ATP hydrolysis in the muscles of GPA-fed rats. The results demonstrate that the transport role of PCr is not essential in contracting muscle in GPA-fed rats. PCr is probably important in this regard in the larger fibers of control muscle. Although fast-twitch muscles depleted of PCr have nearly twice the glycogen reserves of control muscle, glycogenolysis is limited in its capacity to fill the role of PCr as an energy buffer under conditions of maximum ATP turnover

  4. Multimodal neuroimaging provides a highly consistent picture of energy metabolism, validating 31P MRS for measuring brain ATP synthesis

    Neuroimaging methods have considerably developed over the last decades and offer various noninvasive approaches for measuring cerebral metabolic fluxes connected to energy metabolism, including PET and magnetic resonance spectroscopy (MRS). Among these methods, 31P MRS has the particularity and advantage to directly measure cerebral ATP synthesis without injection of labeled precursor. However, this approach is methodologically challenging, and further validation studies are required to establish 31P MRS as a robust method to measure brain energy synthesis. In the present study, we performed a multimodal imaging study based on the combination of 3 neuroimaging techniques, which allowed us to obtain an integrated picture of brain energy metabolism and, at the same time, to validate the saturation transfer 31P MRS method as a quantitative measurement of brain ATP synthesis. A total of 29 imaging sessions were conducted to measure glucose consumption (CMRglc), TCA cycle flux (VTCA), and the rate of ATP synthesis (VATP) in primate monkeys by using 18F-FDG PET scan, indirect 13C MRS, and saturation transfer 31P MRS, respectively. These 3 complementary measurements were performed within the exact same area of the brain under identical physiological conditions, leading to: CMRglc = 0.27 ± 0.07 μmol.g-1.min-1, VTCA = 0.63 ± 0.12 μmol.g-1.min-1, and VATP = 7.8 ± 2.3 μmol.g-1.min-1. The consistency of these 3 fluxes with literature and, more interestingly, one with each other, demonstrates the robustness of saturation transfer 31P MRS for directly evaluating ATP synthesis in the living brain. (authors)

  5. Influence of the computerized {sup 31}P NMR spectra processing on the tissues pH determination precision; Wplyw obrobki cyfrowej widm {sup 31}P MRJ na dokladnosc pomiaru pH tkanek

    Kupka, T. [Inst. Chemii, Univ. Slaski, Katowice (Poland)]|[Zaklad Ciala Stalego, Polska Akademia Nauk, Zabrze (Poland); Religa, Z.; Zembala, M.; Nozynski, J.; Wojtek, P. [Slaska Akademia Medyczna, Zabrze (Poland); Pasterna, G. [Inst. Fizyki, Univ. Slaski, Katowice (Poland); Makhyanov, N. [Nizhnekamskneftekhym, Nizhnekamsk, Tatarstan (Russian Federation)

    1995-12-31

    The {sup 31}P NMR spectra of different tissues have been measured. To improve the spectra resolution two method of Fourier transformation have been used and namely the CDRE (Convulsion Difference Resolution Enhancement) and LGM (Lorentz-to-Gaussian Multiplication). It was shown that these procedures allow one to improve the quality of measured spectra what results in better precision of the tissues pH determination. 5 refs, 2 figs.

  6. 1H NMR in a-Si

    Carlos, W. E.; Taylor, P. C.

    1982-10-01

    Results of pulsed NMR studies of hydrogen in a-Si: H prepared at several laboratories by glow discharge of silane are presented. The origins of the two 1H NMR lines seen in almost all samples of a-Si: H are discussed. Solid-echo measurements are presented which indicate that these two components are due to spatially isolated groups of protons. We attribute the narrow line to protons slightly clustered in the bulk of the material and the broad line to protons distributed on internal surfaces. The spin-lattice relaxation time shows a minimum at T~30 K which is interpreted as due to relaxation via spin diffusion to a small number of H2 molecules acting as relaxation centers. Annealing results suggest that all the hydrogen molecules are trapped in very similar sites.

  7. Synthesis and biological characterization of new amino-phosphonates for mitochondrial pH determination by 31P NMR spectroscopy

    A series of mitochondria targeted α-amino-phosphonates combining a diethoxy-phosphoryl group and an alkyl chain-connected triphenylphosphonium bromide tail were designed and synthesized, and their pH-sensitive 31P NMR properties and biological activities in vitro and in vivo were evaluated. The results showed a number of these mitoaminophosphonates exhibiting pKa values fitting the mitochondrial pH range, short relaxation, and chemical shift parameters compatible with sensitive 31P NMR detection, and low cytotoxicity on green algae and murine fibroblasts cell cultures. Of these, two selected compounds demonstrated to distribute at NMR detectable levels within the cytosolic and mitochondrial sites following their perfusion to isolated rat livers, with no detrimental effects on cell energetics and aerobic respiration. This study provided a new molecular scaffold for further development of in situ spectroscopic real-time monitoring of mitochondrion/cytosol pH gradients. (authors)

  8. Observations on the cytoplasmic and vacuolar orthophosphate pools in leaf tissues using in vivo 31P-NMR spectroscopy

    A full understanding of the central role of Pi in photosynthesis requires information on the size of the endogenous Pi pools and the extent to which they interact with each other under different physiological conditions. In vivo 31P-NMR spectroscopy has the potential to assist in this objective by the early applications of this technique to leaf tissues were disappointing. Here we report 31P-NMR data from maize and tomato leaf discs that: (i) cast doubt on earlier estimates of the cytoplasmic orthophophate pool size; and (ii) prove that exogenously supplied D-mannose can reduce the cytoplasmic P1level in some circumstances. (author). 21 refs.; 4 figs.; 1 tab

  9. Sequestration of the tributyl phosphate complex of europium nitrate in the clay hectorite. A 31P NMR study

    Application of 31P NMR to distinguish Eu(NO3)3-complexed tributyl phosphate from uncomplexed tributyl phosphate (TBP) facilitates an understanding of the fate of these species in the clay hectorite. Solution 31P NMR studies show dramatic shifts of -156.0 to -172.9 ppm for Eu(NO3)36H2O dissolved in TBP at TBP:Eu ratios 1:1 to 1:2.5. Pure TBP exhibits 31P chemical shift of -0.3 ppm. Mixtures with higher TBP:Eu ratios display lines progressively downfield of -156.0 ppm, reflecting exchange of complexed and free TBP. The Eu(NO3)3-complexed TBP adsorbed into hectorite displays a 31P chemical shift of -180.7 to -193.8 ppm. Clays adsorbed with solutions that are 3.1, 5:1 and 7:1 TBP:Eu display peaks due to complex as well as peaks in the range -4 to -6 ppm attributed to uncomplexed TBP. No evidence of exchange is observed. Spectra of the TBP-adsorbed clay give a TBP line at -0.7 ppm which changes slightly to --5.0 after exchange with Eu(NO3)3. The Eu(NO3)3-exchanged hectorite displays a line at -17.6 ppm after adsorption of TBP. Neither of the latter two samples show indication of complex formation. The hectorite samples exposed to TBP or the complex display (001) d spacings of 17.9-18.4 A compared to 12.3-12.5 A for hectorite which has not been exposed to TBP. 26 refs., 5 figs., 3 tabs

  10. 31P nuclear magnetic resonance studies of effects of some chlorophenols on Escherichia coli and a pentachlorophenol-degrading bacterium.

    Steiert, J G; Thoma, W J; Ugurbil, K; Crawford, R L

    1988-01-01

    A Flavobacterium sp. that mineralizes pentachlorophenol degrades some, but not all, of the other chlorinated phenols. Whole-cell 31P nuclear magnetic resonance was used to compare and observe transmembrane pH gradients and nucleotide pools in the Flavobacterium sp. and Escherichia coli after pentachlorophenol and 3,4,5-trichlorophenol were added to the cell suspensions. The data suggest that those chlorinated phenols which are not degraded by the Flavobacterium sp. may be resistant to degrada...

  11. 31P-NMR studies on membrane phospholipids in microsomes, rat liver slices and intact perfused rat liver

    Kruijff, B. de; Rietveld, A.; Cullis, P.R.

    1980-01-01

    1. 1. The 36.4 and 81 MHz 31P-NMR spectra of isolated rat liver microsomes, rat liver slices and perfused rat liver have been recorded in the 4–40°C temperature range. 2. 2. In isolated microsomes at 37°C the majority of the phospholipids undergo isotropic motion, whereas at 4°C most of the phospho

  12. Energetics of acute pressure overload of the porcine right ventricle. In vivo 31P nuclear magnetic resonance.

    Schwartz, G G; Steinman, S; Garcia, J.; Greyson, C; Massie, B; Weiner, M W

    1992-01-01

    In vivo 31P nuclear magnetic resonance (NMR) spectroscopy of the right ventricular (RV) free wall was employed to determine (a) whether phosphorus energy metabolites vary reciprocally with workload in the RV and (b) the mechanisms that limit RV contractile function in acute pressure overload. In 20 open-chest pigs, phosphocreatine (PCr)/ATP ratio (an index of energy metabolism inversely related to free ADP concentration), myocardial blood flow (microspheres), and segment shortening (sonomicro...

  13. 31P-NMR spectroscopy and histological studies of the response of rat mammary tumours to endocrine therapy.

    Stubbs, M.; Coombes, R C; Griffiths, J R; Maxwell, R J; Rodrigues, L. M.; Gusterson, B. A.

    1990-01-01

    We have shown by 31P-NMR spectroscopy that ovariectomy, in N-methyl-N-nitrosourea induced mammary adenocarcinomas, increases signals from phosphocreatine (PCr) relative to nucleoside triphosphate (NTP) before measurable regression (2 days) and for at least a further 13 days. The present study correlates the NMR changes with histological changes in the regressing tumour. Mammary tumours were examined by NMR before, and 2 and 14 days after, ovariectomy or sham-ovariectomy. Sections were taken f...

  14. 31P NMR studies of intracellular pH and phosphate metabolism during cell division cycle of Saccharomyces cerevisiae.

    Gillies, R.J.; Ugurbil, K; den Hollander, J A; Shulman, R G

    1981-01-01

    We have analyzed changes in intracellular pH and phosphate metabolism during the cell cycle of Saccharomyces cerevisiae (NCYC 239) by using high-resolution 31P NMR spectroscopy. High-density yeast cultures (2 x 10(8) cells per ml) were arrested prior to "start" by sequential glucose deprivation, after which they synchronously replicated DNA and divided after a final glucose feeding. Oxygenation of arrested cultures in the absence of glucose led to increased levels of sugar phosphates and ATP ...

  15. Distinguishing Bicontinuous Lipid Cubic Phases from Isotropic Membrane Morphologies Using 31P Solid-State NMR Spectroscopy

    Yang, Yu; Yao, Hongwei

    2015-01-01

    Nonlamellar lipid membranes are frequently induced by proteins that fuse, bend, and cut membranes. Understanding the mechanism of action of these proteins requires the elucidation of the membrane morphologies that they induce. While hexagonal phases and lamellar phases are readily identified by their characteristic solid-state NMR lineshapes, bicontinuous lipid cubic phases are more difficult to discern, since the static NMR spectra of cubic-phase lipids consist of an isotropic 31P or 2H peak, indistinguishable from the spectra of isotropic membrane morphologies such as micelles and small vesicles. To date, small-angle X-ray scattering is the only method to identify bicontinuous lipid cubic phases. To explore unique NMR signatures of lipid cubic phases, we first describe the orientation distribution of lipid molecules in cubic phases and simulate the static 31P chemical shift lineshapes of oriented cubic-phase membranes in the limit of slow lateral diffusion. We then show that 31P T2 relaxation times differ significantly between isotropic micelles and cubic-phase membranes: the latter exhibit two-orders-of magnitude shorter T2 relaxation times. These differences are explained by the different timescales of lipid lateral diffusion on the cubic-phase surface versus the timescales of micelle tumbling. Using this relaxation NMR approach, we investigated a DOPE membrane containing the transmembrane domain (TMD) of a viral fusion protein. The static 31P spectrum of DOPE shows an isotropic peak, whose T2 relaxation times correspond to that of a cubic phase. Thus, the viral fusion protein TMD induces negative Gaussian curvature, which is an intrinsic characteristic of cubic phases, to the DOPE membrane. This curvature induction has important implications to the mechanism of virus-cell fusion. This study establishes a simple NMR diagnostic probe of lipid cubic phases, which is expected to be useful for studying many protein-induced membrane remodeling phenomena in biology

  16. In vivo mouse myocardial (31)P MRS using three-dimensional image-selected in vivo spectroscopy (3D ISIS): technical considerations and biochemical validations

    Bakermans, A.J.; Abdurrachim, D.; Nierop, B.J. van; Koeman, A.; Kroon, I. van der; Baartscheer, A.; Schumacher, C.A.; Strijkers, G.J.; Houten, S.M.; Zuurbier, C.J.; Nicolay, K.; Prompers, J.J.

    2015-01-01

    (31)P MRS provides a unique non-invasive window into myocardial energy homeostasis. Mouse models of cardiac disease are widely used in preclinical studies, but the application of (31)P MRS in the in vivo mouse heart has been limited. The small-sized, fast-beating mouse heart imposes challenges regar

  17. A comparison of MR elastography and {sup 31}P MR spectroscopy with histological staging of liver fibrosis

    Godfrey, Edmund M. [St James' Hospital, Leeds (United Kingdom); St James' Hospital, Department of Radiology, Leeds (United Kingdom); Patterson, Andrew J.; Priest, Andrew N.; Davies, Susan E.; Joubert, Ilse; Krishnan, Anant S.; Shaw, Ashley S.; Alexander, Graeme J.; Allison, Michael E.; Griffiths, William J.H.; Gimson, Alexander E.S. [Addenbrooke' s Hospital, Cambridge (United Kingdom); Griffin, Nyree [St Thomas' s Hospital, London (United Kingdom); Lomas, David J. [University of Cambridge, Department of Radiology, Cambridge (United Kingdom)

    2012-12-15

    Conventional imaging techniques are insensitive to liver fibrosis. This study assesses the diagnostic accuracy of MR elastography (MRE) stiffness values and the ratio of phosphomonoesters (PME)/phosphodiesters (PDE) measured using {sup 31}P spectroscopy against histological fibrosis staging. The local research ethics committee approved this prospective, blinded study. A total of 77 consecutive patients (55 male, aged 49 {+-} 11.5 years) with a clinical suspicion of liver fibrosis underwent an MR examination with a liver biopsy later the same day. Patients underwent MRE and {sup 31}P spectroscopy on a 1.5 T whole body system. The liver biopsies were staged using an Ishak score for chronic hepatitis or a modified NAS fibrosis score for fatty liver disease. MRE increased with and was positively associated with fibrosis stage (Spearman's rank = 0.622, P < 0.001). PME/PDE was not associated with fibrosis stage (Spearman's rank = -0.041, p = 0.741). Area under receiver operating curves for MRE stiffness values were high (range 0.75-0.97). The diagnostic utility of PME/PDE was no better than chance (range 0.44-0.58). MRE-estimated liver stiffness increases with fibrosis stage and is able to dichotomise fibrosis stage groupings. We did not find a relationship between {sup 31}P MR spectroscopy and fibrosis stage. circle Magnetic resonance elastography (MRE) and MR spectroscopy can both assess the liver. (orig.)

  18. Value of 31P MR spectroscopy in monitoring the early response of hepatocellular carcinoma to transcatheter arterial chemoembolization

    Objective: To evaluate the value of 31P MR spectroscopy in monitoring the early response of hepatocellular carcinoma to chemoembolization. Methods: 31P-MR spectra of HCC obtained before and within 48 h after chemoembolization in 15 HCC patients with 17 lesions. A control group of five adults with normal livers was examined through the same protocol. The median and range of the phosphomonoester (PME)and phosphodiester (PDE) levels in HCCs and in the control subjects were calculated and compared. The median and range of the PME and PDE levels, the ratio of phosphomonoester to nucleoside triphosphate (PME/NPT), and phosphodiester to nucleoside triphosphate (PDE/NPT) in HCC before and after TACE were calculated seperately. For statistical analysis, the two-tailed paired t-test was applied. Alterations of phosphorus metabolism before and after TACE were compared with tumor response evaluated by means of long-term follow-up. Results: Chemoembolization induced decrease of the PME level (P0.05). Conclusions: The ratios of PME/NPT and PDE/NPT of 31P-MRS may provide the monitor of therapeutic early responses of hepatocellular carcinoma to chemoembolization, although yet the larger, more definitive and quantitative studies are needed clinically. (authors)

  19. Effects of nimodipine on EEG and 31P-NMR spectra during and after incomplete forebrain ischemia in the rat

    The effect of nimodipine was studied on EEG power density spectra as well as on 31P-NMR spectra of the brain before, during and after four-vessel occlusion (FVO) in the restrained conscious rat. EEG-spectral analysis: eight rats were submitted to 5 min FVO and four of them received nimodipine (1 mg/kg orally) 75 min before FVO. In the nimodipine-treated rats the post-ischemic overshoot of the EEG power density was significantly lower for the theta, alpha and beta band activity. 31P-NMR spectroscopy: the relative concentrations of phosphocreatine (PCr), ATP and Pi as well as intracellular pH were measured at different intervals after 10 min FVO (n = 10). All values normalised within 15-30 min after restoration of cerebral blood flow without significant differences between nimodipine-treated and control rats. It is concluded that pretreatment with nimodipine has a decreasing effect on the overshoot in EEG power density after transient incomplete forebrain ischemia. This effect was not correlated to significant changes in cerebral 'energy state', as measured by 31P-NMR spectroscopy. (Auth.)

  20. 31P and 13C-NMR studies of the phosphorus and carbon metabolites in the halotolerant alga, Dunaliella salina

    The intracellular phosphorus and carbon metabolites in the halotolerant alga Dunaliella salina adapted to different salinities were monitored in living cells by 31P- and 13C-nuclear magnetic resonance (NMR) spectroscopy. The 13C-NMR studies showed that the composition of the visible intracellular carbon metabolites other than glycerol is not significantly affected by the salinity of the growth medium. The T1 relaxation rates of the 13C-glycerol signals in intact cells were enhanced with increasing salinity of the growth medium, in parallel to the expected increase in the intracellular viscosity due to the increase in intracellular glycerol. The 31P-NMR studies showed that cells adapted to the various salinities contained inorganic phosphate, phosphomonoesters, high energy phosphate compounds, and long chain polyphosphates. In addition, cells grown in media containing up to 1 molar NaCl contained tripolyphosphates. The tripolyphosphate content was also controlled by the availability of inorganic phosphate during cell growth. Phosphate-depleted D. salina contained no detectable tripolyphosphate signal. Excess phosphate, however, did not result in the appearance of tripolyphosphate in 31P-NMR spectra of cells adapted to high (>1.5 molar NaCl) salinities

  1. 31P nuclear magnetic resonance study of the metabolic pools of adenosine triphosphate in cultured bovine adrenal medullary chromaffin cells

    31P NMR was used to resolve and determine the relative quantity and mobility of ATP in the cytosolic and vesicular compartments of isolated adrenomedullary chromaffin cells. The cells were cultured on microcarrier beads and superfused with an oxygenated medium-thereby permitting dense suspensions of viable cells to be maintained in the NMR probe for extended time periods. Under these conditions, distinct 31P signals could be seen for ATP within the vesicular and the cytosolic pools. Comparison of the integrated areas of the β-phosphate resonances from the two ATP pools indicated 77% of the endogenous ATP was in the vesicular pool. From this observation and the assumption that the concentration of ATP in the vesicle is 87.5 mM, the concentration of ATP calculated to be in the cytoplasmic pool was ∼ 4 mM. The pH in the vesicle determined from the chemical shift of the γ-phosphate resonance of vesicular ATP was 5.84 ± 0.17, slightly higher than the intragranular pH measured in hypoxic cells. Spin-lattice relaxation times of ATP 31P resonances in the vesicular pool were from 12 to 14 times shorter than the ATP resonances in the cytosol, corresponding to a decrease in molecular mobility due to incorporation of ATP within a catecholamine-storage complex

  2. Analysis of monoglycerides, diglycerides, sterols, and free fatty acids in coconut (Cocos nucifera L.) oil by 31P NMR spectroscopy.

    Dayrit, Fabian M; Buenafe, Olivia Erin M; Chainani, Edward T; de Vera, Ian Mitchelle S

    2008-07-23

    Phosphorus-31 nuclear magnetic resonance spectroscopy ( (31)P NMR) was used to differentiate virgin coconut oil (VCO) from refined, bleached, deodorized coconut oil (RCO). Monoglycerides (MGs), diglycerides (DGs), sterols, and free fatty acids (FFAs) in VCO and RCO were converted into dioxaphospholane derivatives and analyzed by (31)P NMR. On the average, 1-MG was found to be higher in VCO (0.027%) than RCO (0.019%). 2-MG was not detected in any of the samples down to a detection limit of 0.014%. On the average, total DGs were lower in VCO (1.55%) than RCO (4.10%). When plotted in terms of the ratio [1,2-DG/total DGs] versus total DGs, VCO and RCO samples grouped separately. Total sterols were higher in VCO (0.096%) compared with RCO (0.032%), and the FFA content was 8 times higher in VCO than RCO (0.127% vs 0.015%). FFA determination by (31)P NMR and titration gave comparable results. Principal components analysis shows that the 1,2-DG, 1,3-DG, and FFAs are the most important parameters for differentiating VCO from RCO. PMID:18576656

  3. Follow-up by 31P NMR spectroscopy of the energy metabolism of malignant tumor in rats during treatment

    The energy metabolism of tumors in rats was investigated by in vivo 31P-NMR spectroscopy. The effects of radiotherapy, chemotherapy or radiotherapy combined with 5-fluoro-uracil (5-FU) chemotherapy were evaluated by observing the changes of these spectra in chemically induced subcutaneous fibrosarcoma in rats. Two milligrams of DMBA in solution in olive oil were administered subcutaneously in the flank of 20 Wister rats and 17 fibrosarcoma occurred. 31P NMR spectra were recorded with a Brueker Medspec 30/47 spectrometer using a surface coil positioned over the tumor. Significant changes in the spectra were not observed during tumor growth. Radiotherapy and 5-FU chemotherapy alone did not induce major changes in the 31P spectra. But the situation was complete different for animals receiving the therapeutic combination. A clear increase in the ratio of inorganic phosphate to total phosphorus signal was observed 48 h after the first irradiation session. The pH shifted concurrently to the acidic range. No effect on tumor regression was observed in the rats from the chemotherapy group, while regression less than 50% in rats treated by irradiation only, and at least 80% in the combined group. (author). 30 refs.; 4 figs

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

    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.

  5. Fractioning of sodium polyphosphate and characterization by {sup 31}P NMR: a experience to physical-chemistry lessons; Fracionamento de polifosfato de sodio e caracterizacao por RMN de 31P: um experimento para aulas de Fisico-Quimica

    Lima, Emilia Celma de Oliveira; Alcantara, Glaucia Braz Alcantara; Damasceno, Fernando Cruvinel, E-mail: elima@quimica.ufg.b [Universidade Federal de Goias (UFG), Goiania, GO (Brazil). Inst. de Quimica; Moita Neto, Jose Machado [Universidade Federal do Piaui (UFPI), Teresina, PI (Brazil). Dept. de Quimica; Galembeck, Fernando [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Inst. de Quimica

    2010-07-01

    This text describes an experiment on fractional precipitation of a polymer together with determination of average degree of polymerization by NMR. Commercial sodium polyphosphate was fractionated by precipitation from aqueous solution by adding increasing amounts of acetone. The polydisperse salt and nine fractions obtained from it were analyzed by {sup 31}P nuclear magnetic resonance and the degree of polymerization of the salts and of the fractions were calculated. Long-chain sodium polyphosphate was also synthesized and analyzed. This experiment was tested in a PChem lab course but it can be used also to illustrate topics of inorganic polymers and analytical chemistry. (author)

  6. 13C and 31P NMR [Nuclear Magnetic Resonance] studies of prostate tumor metabolism

    The current research on prostate cancer by NMR spectroscopy and microscopy will most significantly contribute to tumor diagnosis and characterization only if sound biochemical models of tumor metabolism are established and tested. Prior searches focused on universal markers of malignancy, have to date, revealed no universal markers by any method. It is unlikely that NMRS will succeed where other methods have failed, however, NMR spectroscopy does provide a non-invasive means to analyze multiple compounds simultaneously in vivo. In order to fully evaluate the ability of NMRS to differentiate non-malignant from malignant tissues it is necessary to determine sufficient multiple parameters from specific, well-diagnosed, histological tumor types that, in comparison to normal tissue and non-neoplastic, non-normal pathologies from which the given neoplasm must be differentiated, one has enough degrees of freedom to make a mathematically and statistically significant determination. Confounding factors may consist of tumor heterogeneity arising from regional variations in differentiation, ischemia, necrosis, hemorrhage, inflammation and the presence of intermingled normal tissue. One related aspect of our work is the development of {13C}-1H metabolic imaging of 13C for metabolic characterization, with enhanced spatial localization (46). This should markedly extend the range of potential clinical NMR uses because the spatial variation in prostate metabolism may prove to be just as important in tumor diagnoses as bulk (volume-averaged) properties themselves. It is our hope that NMRS and spectroscopic imaging will reveal a sound correlation between prostate metabolism and tumor properties that will be clinically straightforward and useful for diagnosis

  7. Enhanced Uptake of Ifosfamide into GH3 Prolactinomas with Hypercapnic Hyperoxic Gases Monitored In Vivo by 31P MRS

    Loreta M. Rodrigues

    2002-01-01

    Full Text Available Previously, 31P magnetic resonance spectroscopy (MRS has been used to detect ifosfamide (IF in vivo and to show that breathing carbogen (5% CO2/95% O2 enhances the uptake and increases the efficacy of IF in rat GH3 prolactinomas [Rodrigues LM, Maxwell RJ, McSheehy PMJ, Pinkerton CR, Robinson SP, Stubbs M, and Griffiths JR (1997. In vivo detection of ifosfamide by 31P MRS in rat tumours; increased uptake and cytotoxicity induced by carbogen breathing in GH3 prolactinomas. Br J Cancer 75, 62-68]. We now show that other hypercapnic and/or hyperoxic (5% CO2 in air, 2.5% CO2 in O2 gas mixtures also increase the uptake of IF into tumors, measured by 31P MRS. All gases caused an increased uptake (Cmax of IF compared to air breathing, with carbogen inducing the largest increase (85% (P<.02 compared to 46% with 2.5% CO2 in O2 (P<.004 and 48% with 5% CO2 in air (P<.004. The Tmax (time of maximum concentration in tumor posintravenous injection of IF was significantly (P<.04 later in the cohort that breathed 5% CO2 in air. The increased uptake of IF with carbogen breathing was selective to tumor tissue and there were no significant increases in any of the normal tissues studied, suggesting that any host tissue toxicity would be minimal. Carbogen breathing by patients causes breathlessness. There was no significant difference in IF uptake between breathing carbogen and 2.5% CO2 in O2 and, therefore, the ability of 2.5% CO2 in O2 to also increase IF uptake may be clinically useful as it causes less patient discomfort.

  8. Intracellular pH of perfused single frog skin: combined 19F- and 31P-NMR analysis.

    Civan, M M; Lin, L E; Peterson-Yantorno, K; Taylor, J; Deutsch, C

    1984-11-01

    Intracellular pH (pHc) has been determined in frog skin by applying two different methods of pH measurement, 19F and 31P nuclear magnetic resonance (NMR) analysis, to the same tissues. Results from both NMR approaches confirm an observation by Lin, Shporer, and Civan [Am. J. Physiol. 248 (Cell Physiol. 17): 1985] that acidification of the extracellular medium reverses the sign of the pH gradient present under baseline conditions. The fluorinated probe, alpha-(difluoromethyl)-alanine methyl ester, was introduced into the epithelial cells by preincubating skins for 4.7-10.4 h at room temperature in Ringer solutions containing 1 mM ester. The free amino acid was subsequently released by intracellular esterase activity, thus providing a high enough probe concentration for NMR analysis to be practicable. From measurements of short-circuit current and transepithelial resistance under base-line and experimental conditions and the appearance of phosphocreatine (PCr) in the 31P spectrum of preloaded tissues, the fluorinated probe appears to be nontoxic to frog skin. Measurement of the chemical shift of methylphosphonate relative to PCr permitted calculation of extracellular pH. Estimation of the intracellular pH was performed both by measurement of the chemical shift of inorganic phosphate (Pi) relative to PCr and by measurement of the central peak spacing of the 19F spectrum. From four direct comparisons of the two techniques in two experiments, the difference in the estimated pH was only 0.03 +/- 0.07 pH units, supporting the concept that 31P-NMR analysis is a valid method of measuring pH in this tissue. PMID:6496729

  9. Energy metabolism variation in experimental cerebral ischemia in mongolian gerbils examined by using in vivo 31P-NMR

    The mongolian gerbil is a characteristic animal in which cerebral ischemia is similar to that of the human being in that it can be induced by the ligation of the unilateral caortid artery. Howerver, although ischemia is induced in only 40 to 60 percent of the examined gerbils, there is no appropriate method to assess the development of ischemia in the living state. Recently, it has become possible to investigate the energy metabolism in sequence in a living animal by using the in vivo 31P-NMR method. In this study, the energy metabolism in the brain of living gerbils was investigated by measuring the in vivo 31P-NMR with the surface coil method, and consequently, variations in the development of ischemia in this model was detected. A unilateral carotid artery was ligated in 33 gerbils. Ishemic changes in 31P-NMR spectra, which consisted of a decrease in the peaks of ATP and phosphocreatine (PCr), and a concommitant increase in inorganic phosphate (Pi) associated with a decline of tissue pH, were observed on the ligated-side hemisphere in 9 of the 33 gerbils. The time required for developing these ischemic change varied from immediately after ligation to several hours after ligation. In two cases, the changes in the spectrum were transient and recovered spontaneously within 1 hour. In other gerbils, the recovery of energy metabolism was observed when circulation was restored to the ischemic brain. No ischemic changes in the spectrum were observed in 18 of the 33 gerbils. In all cases, no ischemic changes were observed in spectra obtained from the opposite-side hemisphere. However, the ischemic changes appeared immediately after ligation in all gerbils in which the bilateral carotid artery was ligated. Thus, it was apparent that in this model, there was a wide variation not only in the uncertainty of developing ischemia, but also in the time course of developing the ischemic change. (J.P.N.)

  10. Exertional muscle pain in familial Mediterranean fever patients evaluated by MRI and 31P magnetic resonance spectroscopy

    Aim: To evaluate the effect of physical activity on the structural, morphological, and metabolic characteristics of the gastrocnemius muscle in familial Mediterranean fever (FMF) patients, utilizing quantitative 31P magnetic resonance spectroscopy (MRS), in order to elucidate the mechanism of their exertional leg pain. Materials and methods: Eleven FMF patients suffering from exertional leg pain (eight male, three female; mean age 33 years) and six healthy individuals (three male, three female; mean age 39 years) constituted the control group. All of the participants underwent magnetic resonance imaging (MRI) and non-selective 31P MRS (3 T) of the leg muscles before and after graded exercise on a treadmill. Phosphocreatine (PCr):inorganic phosphate (Pi), PCr:adenosine triphosphate (ATP) ratios and the intracellular pH of the leg muscles were measured using 31P MRS. Results: For both groups, normal muscle mass with no signal alterations was observed on the MRI images after exercise. The normal range of pre- and post- exercise MRS muscle parameters was observed in both groups. However, the intracellular pH post-exercise, was significantly higher (less acidic) in the FMF group compared to the control group [pH (FMF) = 7.03 ± 0.02; pH (control) 7.00 ± 0.02; p < 0.0006]. Conclusions: The finding of a less prominent, post-exercise acidification of the gastrocnemius muscle in this FMF patient group suggests a forme fruste of glycogenosis. This preliminary observation should be further investigated in a future, larger-scale study

  11. Phosphatidylinositol-specific phospholipase C from Bacillus cereus combines intrinsic phosphotransferase and cyclic phosphodiesterase activities: A 31P NMR study

    The inositol phosphate products formed during the cleavage of phosphatidylinositol by phosphatidylinositol-specific phospholipase C from Bacillus cereus were analyzed by 31P NMR. 31P NMR spectroscopy can distinguish between the inositol phosphate species and phosphatidylinositol. Chemical shift values (with reference to phosphoric acid) observed are -0.41, 3.62, 4.45, and 16.30 ppm for phosphatidylinositol, myo-inositol 1-monophosphate, myo-inositol 2-monophosphate, and myo-inositol 1,2-cyclic monophosphate, respectively. It is shown that under a variety of experimental conditions this phospholipase C cleaves phosphatidylinositol via an intramolecular phosphotransfer reaction producing diacylglycerol and D-myo-inositol 1,2-cyclic monophosphate. The authors also report the new and unexpected observation that the phosphatidylinositol-specific phospholipase C from B. cereus is able to hydrolyze the inositol cyclic phosphate to form D-myo-inositol 1-monophosphate. The enzyme, therefore, possesses phosphotransferase and cyclic phosphodiesterase activities. The second reaction requires thousandfold higher enzyme concentrations to be observed by 31P NMR. This reaction was shown to be regiospecific in that only the 1-phosphate was produced and stereospecific in that only D-myo-inositol 1,2-cyclic monophosphate was hydrolyzed. Inhibition with a monoclonal antibody specific for the B.cereus phospholipase C showed that the cyclic phosphodiesterase activity is intrinsic to the bacterial enzyme. They propose a two-step mechanism for the phosphatidyl-inositol-specific phospholipase C from B. cereus involving sequential phosphotransferase and cyclic phosphodiesterase activities. This mechanism bears a resemblance to the well-known two-step mechanism of pancreatic ribonuclease, RNase A

  12. Study of macroergic compounds in red blood cells of pregnant anemic women using a method of 31 P-NMR

    The analysis of the intensities of ATP and ADP signals in spectra of 31 P-NMR has shown that the ATP level in RBC during anemia in pregnant women is reduced, while the rate of a decrease in the ATP/ADP ratio following washing RBC from plasma is higher as compared with control. When measuring chemical shifts of 2,3-DPH, we have found that the value of the intracellular pH during anemia in RBC is lower in RBC washed from plasma as compared with control. The results are accounted for by a more intensive operation of enzymes of the glycolytic path

  13. 31P-NMR studies on membrane phospholipids in microsomes, rat liver slices and intact perfused rat liver

    de Kruijff, B.; Rietveld, A.; Cullis, P.R.

    1980-01-01

    1. 1. The 36.4 and 81 MHz 31P-NMR spectra of isolated rat liver microsomes, rat liver slices and perfused rat liver have been recorded in the 4–40°C temperature range. 2. 2. In isolated microsomes at 37°C the majority of the phospholipids undergo isotropic motion, whereas at 4°C most of the phospholipids give rise to typical ‘bilayer’ spectra. 3. 3. Isolated hydrated rat liver microsomal phosphatidylethanolamine is organised in the hexagonal HII phase above 7°C. 4. 4. The Mn2+ permeability of...

  14. 31P NMR saturation transfer study of the creatine kinase reaction in human skeletal muscle at rest and during exercise.

    Goudemant, Jean-François; Francaux, Marc; Mottet, I.; Demeure, R.; Sibomana, M.; Sturbois, Xavier

    1997-01-01

    The creatine kinase reaction has been studied by 31P NMR in exercising human calf muscle. Quantitative analysis of high energy phosphates and saturation transfer study of the creatine kinase flux in the direction of ATP synthesis (Vfor) were performed at rest and during exercise. As expected, exercise induced a [PCr] decrease (from 28.5 +/- 0.9 to 21.9 +/- 1.5 mM, P < 0.01) matched by a Pi increase (from 4.5 +/- 0.2 to 8.9 +/- 1.8 mM, P = 0.06). pHi and [ATP] remained unchanged. Vfor did not ...

  15. In vivo 31P nuclear magnetic resonance saturation transfer measurements of phosphate exchange reactions in the yeast Saccharomyces cerevisiae

    31P saturation transfer techniques have been used to measure phosphate kinetics in the yeast Saccharomyces cerevisiae. The phosphate comsumption rate observed in acetate grown mid-log cells was combined with measurements of O2 consumption to yield P/O ratios of 2.2 and 2.9, for cells respiring on glucose and ethanol, respectively. However, no phosphate consumption activity was observed in saturation transfer experiments on anaerobic glucose fed cells. The phosphate consumption rates measured by saturation transfer in cells respiring on glucose and ethanol was attributed to the unidirectional rates of mitochondrial ATP synthesis. (Auth.)

  16. 31P-NMR分析湿地沉积物有机磷的方法优化%Optimizing the Method for 31 P-NMR Analysis of Organic Phosphorus f rom Wetland Sediments

    陆瑾; 王海文; 郝红; 高博; 贾建丽

    2013-01-01

    Solution 31 P-Nuclear Magnetic Resonance (NMR) is an analysis technology which has been an effective means for the analysis of environmental organic phosphorus .However ,the method is rarely applied in the study of wetlands so that the corre-sponding researches about wetland sediment sample preparation method also very deficient .The present study was aimed to find the most suitable sample preparation method for 31 P-NMR analysis of the artificial wetland sediments ,using different extractant (NaOH or 0.25 mol · L -1 NaOH+0.05 mol · L -1 EDTA as main extractant ,and 1 M HCl as pre-extractant or not) ,sample to extractant ratio (1∶8 or 1∶10) ,centrifugation conditions and scans time and so on .The results showed that the best 31 P-NMR spectrum could be obtained with freeze-ried ,ground and sieved sediments ,1 M HCl as pre-extractant for 16 h ,NaOH+0.05 mol · L -1 EDTA as main extractant for 16 h ,extraction ratio of 1∶8 ,and low temperature and high-speed centrifugation (4 ℃ ,10 000 r · min-1 for 30min) for avoiding hydrolysis of certain components .Besides ,choosing much longer NMR scan time ,as 14~16 h (scans about 25 000 times) ,could get more complete spectral signals spectrum .And finally ,four kinds of P-compounds (orthophosphate ,orthophosphate monoesters ,orthophosphate diesters and pyrophosphate ) were detected in the NMR spec-trum .But neither polyphosphate nor phosphonates was not found in all these experiments ,which need further study .Compared with the traditional chemical analysis method ,31 P-NMR method of sample preparation is relatively simple .Then it is less de-structive with components distinguished completely .Using 31 P-NMR technology ,the cognition of wetland phosphorus cycle ,es-pecially organophosphate ,will be expected to get new breakthrough .%近年来,31P-NMR(nuclearmagneticresonance)已成为研究环境有机磷的有力武器,然而此方法在湿地学研究中的应用却很少,关于湿地沉积物样品制

  17. Contribution to the study of the 31P, 1H spin spin coupling constant N. M. R. in three co-ordinated phosphorus compounds. Influence of the bond orientation and of the nature of the substituent around the phosphorus atom

    In order to investigate the influence of the configuration at the phosphorus atom and the influence of the substituents attached to the phosphorus atom on the JPH spin spin coupling constant, we have performed the NMR spectrum analysis of some three coordinated organo-phosphorus compounds. The studied coupling constants are 3JPH through P-O-C-H and P-C-C-H fragments and 2JPH through P-C-H fragment. The results clearly show that on the NMR time scale, in all the studied compounds (1,3,2-dioxaphospholanes, 1,3,2-dioxaphosphorinanes, 3-phospha-cyclopentene and 4-phosphorinanone) there is no inversion of the bonds around phosphorous. This conclusion held also for secondary phosphines. For a given geometry of the bonds joining the P and H atoms, and a given disposition of the bonds around the phosphorus atom, there is only a little influence of the nature of the substituents on the JPH spin coupling constants. The geometrical dependence of the 3JPH cannot be explained by a 'Karplus law'. There is an influence of the bond disposition around phosphorus. In the case of the 2JP-C-H, one can plot a curve 2JP-C-H = f(α) (0≤ α ≤ 180), α denote the dihedral angle of the two plane defined the first one by the P, C and H atoms, and the second one by the P-C bond together with the three-fold axis of the bond around phosphorus assuming a regular pyramidal arrangement. The function 2JP-C-H = f(α) has two maxima, one for α = 0 degrees and the other for α = 180 degrees, and also a minimum for α = 110 degrees. (author)

  18. 慢性乙型肝炎患者31P MRS与血清肝功能相关性研究%Relationship of in vivo 31P MR spectroscopy to serum transaminase in chronic hepatitis B

    崔恩铭; 谭理连; 李志铭; 汪银玉; 林凡; 刘克; 黄勇

    2007-01-01

    目的:探讨慢性乙型肝炎患者肝脏31P MRS波谱及代谢生化信息特点,以及与肝功能变化之间的相关性及临床价值.方法:按2000年西安会议全国病毒性肝炎防治方案标准,将26例慢性乙型肝炎患者分为轻、中、重及肝功能正常肝炎组,并选择20例健康志愿者作对照,分别行常规MR扫描及31P MRS成像,观察31P MRS波谱及代谢生化信息特点,并分析各指标与肝功能生化指标(ATL、AST)之间的相关性.结果:对照组的%PME及PME/PDE分别为9.32+2.74,0.31±0.06,肝功能正常肝炎组分别为9.5±4.2,0.32±0.14,轻度组分别为10.97±1,0.38±0.08,中度组分别为12.59±3.18,0.45±0.13,重度组分别为15.49±4.7,0.53±0.14.肝功能正常的肝炎患者各31P MRS指标与对照组无统计学差异,而对照组与重度组、轻度组与重度组之间的%PME,以及对照组与中度组、对照组与重度组、轻度组与重度组之间的PME/PDE有统计学差异,其中PME/PDE与ALT呈正相关(P=0.037),而与AST无相关性(P=0.075).结论:肝脏31P MRS能无创的、直接的检测肝代谢过程的生化信息及能量状况,能提示慢性乙型肝炎患者有肝功能损害程度,对慢性乙型肝炎患者的肝功能检测及监测具有重要价值.

  19. Defective mitochondrial function in vivo in skeletal muscle in adults with Down's syndrome: a 31P-MRS study.

    Alexander C Phillips

    Full Text Available Down's syndrome (DS is a developmental disorder associated with intellectual disability (ID. We have previously shown that people with DS engage in very low levels of exercise compared to people with ID not due to DS. Many aspects of the DS phenotype, such as dementia, low activity levels and poor muscle tone, are shared with disorders of mitochondrial origin, and mitochondrial dysfunction has been demonstrated in cultured DS tissue. We undertook a phosphorus magnetic resonance spectroscopy ((31P-MRS study in the quadriceps muscle of 14 people with DS and 11 non-DS ID controls to investigate the post-exercise resynthesis kinetics of phosphocreatine (PCr, which relies on mitochondrial respiratory function and yields a measure of muscle mitochondrial function in vivo. We found that the PCr recovery rate constant was significantly decreased in adults with DS compared to non-DS ID controls (1.7 ± 0.1 min(-1 vs 2.1 ± 0.1 min(-1 respectively who were matched for physical activity levels, indicating that muscle mitochondrial function in vivo is impaired in DS. This is the first study to investigate mitochondrial function in vivo in DS using (31P-MRS. Our study is consistent with previous in vitro studies, supporting a theory of a global mitochondrial defect in DS.

  20. Localized Semi-LASER Dynamic 31P Magnetic Resonance Spectroscopy of the Soleus During and Following Exercise at 7 T

    Fiedler, Georg B; Schmid, Albrecht I; Goluch, Sigrun; Schewzow, Kiril; Laistler, Elmar; Mirzahosseini, Arash; Niess, Fabian; Unger, Ewald; Wolzt, Michael; Moser, Ewald

    2015-01-01

    Object This study demonstrates the applicability of semi-LASER localized dynamic $^{31}$P MRS to deeper lying areas of the exercising human soleus muscle (SOL). The effect of accurate localization and high temporal resolution on data specificity is investigated. Materials and Methods To achieve high signal-to-noise ratio (SNR) at a temporal resolution of 6 s, a custom-built calf coil array was used at 7T. The kinetics of phosphocreatine (PCr) and intracellular pH were quantified separately in SOL and gastrocnemius medialis (GM) muscle of 9 volunteers, during rest, plantar flexion exercise and recovery. Results The average SNR of PCr at rest was 64$\\pm$15 in SOL (83$\\pm$12 in GM). End exercise PCr depletion in SOL (19$\\pm$9%) was far lower than in GM (74$\\pm$14%). pH in SOL increased rapidly and, in contrast to GM, remained elevated until the end of exercise. Conclusion $^{31}$P MRS in single-shots every 6 s localized in the deeper lying SOL enabled quantification of PCr recovery times at low depletions and of...

  1. Analysis of the bond-valence method for calculating (29) Si and (31) P magnetic shielding in covalent network solids.

    Holmes, Sean T; Alkan, Fahri; Iuliucci, Robbie J; Mueller, Karl T; Dybowski, Cecil

    2016-07-01

    (29) Si and (31) P magnetic-shielding tensors in covalent network solids have been evaluated using periodic and cluster-based calculations. The cluster-based computational methodology employs pseudoatoms to reduce the net charge (resulting from missing co-ordination on the terminal atoms) through valence modification of terminal atoms using bond-valence theory (VMTA/BV). The magnetic-shielding tensors computed with the VMTA/BV method are compared to magnetic-shielding tensors determined with the periodic GIPAW approach. The cluster-based all-electron calculations agree with experiment better than the GIPAW calculations, particularly for predicting absolute magnetic shielding and for predicting chemical shifts. The performance of the DFT functionals CA-PZ, PW91, PBE, rPBE, PBEsol, WC, and PBE0 are assessed for the prediction of (29) Si and (31) P magnetic-shielding constants. Calculations using the hybrid functional PBE0, in combination with the VMTA/BV approach, result in excellent agreement with experiment. © 2016 Wiley Periodicals, Inc. PMID:27117609

  2. The intact muscle lipid composition of bulls: an investigation by MALDI-TOF MS and 31P NMR.

    Dannenberger, Dirk; Süss, Rosmarie; Teuber, Kristin; Fuchs, Beate; Nuernberg, Karin; Schiller, Jürgen

    2010-02-01

    The analysis of beef lipids is normally based on chromatographic techniques and/or gas chromatography in combination with mass spectrometry (GC/MS). Modern techniques of soft-ionization MS were so far scarcely used to investigate the intact lipids in muscle tissues of beef. The objective of the study was to investigate whether matrix-assisted laser desorption and ionization time-of-flight (MALDI-TOF) mass spectrometry and (31)P nuclear magnetic resonance (NMR) spectroscopy are useful tools to study the intact lipid composition of beef. For the MALDI-TOF MS and (31)P NMR investigations muscle samples were selected from a feeding experiment with German Simmental bulls fed different diets. Beside the triacylglycerols (TAGs), phosphatidylethanolamine (PE), phosphatidylcholine (PC) and phosphatidylinositol (PI) species the MALDI-TOF mass spectra of total muscle lipids gave also intense signals of cardiolipin (CL) species. The application of different matrix compounds, 2,5-dihydroxybenzoic acid (DHB) and 9-aminoacridine (9-AA), leads to completely different mass spectra: 9-AA is particularly useful for the detection of (polar) phospholipids, whereas apolar lipids, such as cholesterol and triacylglycerols, are exclusively detected if DHB is used. Finally, the quality of the negative ion mass spectra is much higher if 9-AA is used. PMID:19900429

  3. In vivo 31P-NMR studies on energy metabolism and the effect of methotrexate in a murine implanted osteosarcoma

    The energy metabolism of Dunn osteosarcoma subcutaneously implanted in C3H/He mice was studied in vivo by a 31P-NMR spectrometer with surface-coils. The spectra of Dunn osteosarcoma showed peaks of sugarphosphate, inorganic phosphate, phosphocreatine, phosphomonoester, and ATPs. In the early stage of the tumor growth phosphocreatine and ATP showed large signal intensities and the tissue pH was 7.23 ± 0.08. Following the tumor growth phosphocreatine and ATP decreased and the tissue pH fell to 6.82 ± 0.08. Immediately after a small dose of MTX (2 mg/kg) was administered, an increase of inorganic phosphate and a decrease of phosphocreatine were temporarily observed when MTX concentrations of the tumor tissues were maximum. High energy metabolites were apparently consumed with the active transport of MTX. After twelve hours of a high dose of MTX (500 mg/kg) was administered, disappearance of phosphocreatine and ATP with an increase of inorganic phosphate was observed previous to the histological change. In vivo 31P-NMR spectroscopy may be useful in the evaluation of chemotherapy. (author)

  4. Non-invasive determination of metabolite concentrations in human transplanted kidney in vivo by 31P MR spectroscopy

    To investigate concentrations of phosphorus-containing metabolites in human transplanted kidney in vivo by quantitative 31P MR spectroscopy (MRS) using surface coils and to compare the obtained values with previous data. Material and Methods: In 5 patients with well-functioning transplanted kidneys, 31P spectra were obtained with the three-dimensional localization image-selected in vivo spectroscopy technique applying a protocol for quantitative spectroscopy using surface coils. Relaxation corrected signal intensities determined by time domain fitting were used to derive absolute molar concentrations for phosphate-containing metabolites. Results: Little or no phosphocreatine in all spectra verified the absence of muscle contamination, confirming proper volume localization. The mean concentrations in the transplanted kidneys were as follows: ATP 1.60±0.26 mmol/l, PDE 2.14±0.91 mmol/l, Pi 0.66±0.25 mmol/l, PME 2.32±0.50 mmol/l. These values are consistent with previously reported values determined by other techniques. Conclusion: The non-invasive determination of absolute metabolite concentrations in human kidney using MRS supplements the use of signal intensity ratios to detect pathologic changes in the energy metabolism of transplanted kidneys

  5. 31P nuclear magnetic resonance study of intracellular phosphate pools and polyphosphate metabolism in Heterosigma akashiwo (Hada) Hada (raphidophyceae)

    The effects of starvation and subsequent addition of phosphate-containing medium on the phosphate metabolic intermediates were studied by 31P-NMR spectroscopy of perchloric acid extracts and intact cells of Heterosigma akashiwo (Hada) Hada. When orthophosphate in the medium was completely depleted the medium was enriched with orthophosphate (4.5 μM). In the phosphate starved condition, the P cell quota was 76 fmol x cell-1 and the major components of phosphate intermediates were phosphodiester, sugar phosphate and orthophosphate (P/sub i/). After addition of P/sub i/, rapid uptake of P/sub i/ was observed and the P cell quota increased to 108 fmol x cell-1 in 2 h, 134 fmol x cell-1 in 5 h and 222 fmol x cell-1 in 1 day after addition of phosphate. The 31P-NMR spectrum indicated that a major portion of P was stored as polyphosphate, in which the average chain length of polyphosphate increased from 10 to 20 phosphate residues in one day after addition of P/sub i/

  6. Genotype-phenotype correlation between the cardiac myosin binding protein C mutation A31P and hypertrophic cardiomyopathy in a cohort of Maine Coon cats

    Granström, S; Godiksen, M T N; Christiansen, M;

    2015-01-01

    OBJECTIVES: A missense mutation (A31P) in the cardiac myosin binding protein C gene has been associated with hypertrophic cardiomyopathy (HCM) in Maine Coon cats. The aim of this study was to investigate the effect of A31P on development of HCM, myocardial diastolic dysfunction detected by color...... tissue Doppler imaging and occurrence of cardiac death during longitudinal follow-up in a cohort of Maine Coon cats. ANIMALS: The original cohort comprised 282 cats (158 of wild-type genotype, 99 heterozygous for A31P and 25 homozygous for A31P). METHODS: Prospective longitudinal study including...... echocardiography and registration of survival. RESULTS: The median age at the initial examination was 1.7 years (range, 0.8-9.2 years) and 6.4% (18/282) of the cats were diagnosed with HCM. One hundred sixty-five cats were eligible for echocardiographic re-examination, and during an average follow-up period of 2...

  7. Conformation and dynamics of melittin bound to magnetically oriented lipid bilayers by solid-state (31)P and (13)C NMR spectroscopy.

    Naito, A.; T. Nagao; Norisada, K; Mizuno, T; Tuzi, S.; Saitô, H.

    2000-01-01

    The conformation and dynamics of melittin bound to the dimyristoylphosphatidylcholine (DMPC) bilayer and the magnetic orientation in the lipid bilayer systems were investigated by solid-state (31)P and (13)C NMR spectroscopy. Using (31)P NMR, it was found that melittin-lipid bilayers form magnetically oriented elongated vesicles with the long axis parallel to the magnetic field above the liquid crystalline-gel phase transition temperature (T(m) = 24 degrees C). The conformation, orientation, ...

  8. Effects of hypo- und hyperthyroidism on skeletal muscle metabolism. A sup 31 P magnetic resonance spectroscopy study. Einfluss von Hyper- und Hypothyreose auf den Energiestoffwechsel der Skelettmuskulatur. Eine Untersuchung mit sup 31 P-Kernspinspektroskopie

    Moka, D.; Theissen, P.; Linden, A.; Waters, W.; Schicha, H. (Koeln Univ. (Germany, F.R.). Klinik und Poliklinik fuer Nuklearmedizin)

    1991-06-01

    {sup 31}P magnetic resonance spectroscopy allows non-invasive evaluation of phosphorus metabolism in man. The purpose of the present study was to assess the influence of hyper- and hypothyroidism on the metabolism of resting human skeletal muscle. The present data show that quantitative measurement of phosphate metabolism by NMR is possible as also demonstrated by other studies. Using a quantitative evaluation method with an external standard, significant differences in the levels of phosphocreatine, adenosintriphosphate, and phosphodiesters were found. In hypothyroid patients a TSH-dependent increase in phosphodiesters and a decrease in adenosintriphosphate and phosphocreatine was observed. In hyperthyroidism a similar decrease in adenosintriphosphate but a considerably higher decrease in phosphocreatine occurred. In the light of the results of other studies of muscle matabolism, these changes appear to be non-specific so that further studies are required to assess the clinical value of such measurements. (orig.).

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

    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 ...

  10. Development of 31P nuclear magnetic resonance methods for the study of phosphate metabolisms in E. coli and B. subtilis

    31P NMR experiments were performed on escherichia coli and Bacillus subtilis at various temperatures under aerobic and anaerobic conditions. The total soluble intracellular phosphate concentration was estimated to be 2 x 10-17 mole/cell, while intracellular orthophosphate concentration was around 1 x 10-17 mole/cell. Addition of glucose resulted in a general decrease in intracellular pH and was accompanied by the formation of sugar monophosphates. The concentrations of soluble intracellular phosphates, both inorganic and organic phosphates, were estimated by integration versus methylene diphosphonic acid (MDPA) standard. Although intracellular and extracellular orthophosphate could be observed, these appear to exchange rapidly on the NMR time scale. (Author)

  11. In vivo 31 P NMR Spectroscopy for the study of P Pools and their Dynamics in Arbuscular Mycorrhizal Fungi

    Viereck, Nanna

    The main objective of the studies described in the present P1i.D. thesis was to investigate the phospbate (P) metabolism of arbuscular mycorrhizal (AM) fungi by in viv0 31P nuclear magnetic resonance (NMR) spectroscopy. P is an essential nutrient for all organisms. It is required in relatively...... of AM fungi used included Scutellospora caloJpora, G. mosseae and Gigaspora rosea. The cucumber plants were grown in a central mesh-bag, which prevents root penetration but allow free passage of AM fungal hyphae. Tbe extraradical mycelium grew into sand surrounding the mesh-bag and could be collected...... from the sand, while root matenal could be collected from the mesh-bag. A circulation system was constructed for oxygenating the excised hyphae or roots while in the NMR tube. Both the efficiency of P, uptake and the turn-over of P metabolites by excised hyphae were investigated in order to clarify the...

  12. Simultaneous 31P-NMR spectroscopy and EMG in exercising and recovering human skeletal muscle: a correlation study

    Vestergaard-Poulsen, P; Thomsen, C; Sinkjaer, T;

    1995-01-01

    of the muscle. Simultaneous 31P-nuclear magnetic resonance spectroscopy and surface electromyography were performed during sustained static exercise and recovery in healthy volunteers and a patient with McArdle's disease. A clear dissociation between the median power frequency of the surface...... electromyogram and pH was seen in the healthy volunteers during recovery and during exercise in the patient with McArdle's disease. The results indicate that proton or lactate accumulation is not primarily responsible for the spectral changes of the surface electromyogram as previously suggested. The motor unit...... myoelectrical activity seen after exercise is not caused by an incomplete recovery of phosphorous metabolism, pH, or lactate but could probably be an impairment of the excitation-contraction coupling....

  13. Determination of basicity of neutral organic phosphorus extractants in nonpolar solvents by the 31P NMR method

    The variant of the NMR method application is developed for quantitative description of acidic-basic properties of neutral organic phosphorus extractants, R3P--O (NPE), in non-polar organic solvents. For the NPE basicity determination the dependence of the chemical shift value in NMR31P spectra of 0.1 M NPE solutions in the dodecane on sulfuric acid acitivity in aqueous phase at 0-12 M acidity is studied. The linear equation relating NPE basicity and electronic structure of these compounds expressed through the sum: of Kabachnik reaction constants is derived. Linear dependences between the NPE basicity value in dodecane and NPE basicity in nitromethane as well as enthalpies of complexes formation with charge transport with standard acid-iodine in heptane, enthalpies of hydrogen complexes formation with phenol and water have been found

  14. 31P NMR measurements of the ADP concentration in yeast cells genetically modified to express creatine kinase

    Rabbit muscle creatine kinase has been introduced into the yeast Saccharomyces cerevisiae by transforming cells with a multicopy plasmid containing the coding sequence for the enzyme under the control of the yeast phosphoglycerate kinase promoter. The transformed cells showed creating kinase activities similar to those found in mammalian heart muscle. 31P NMR measurements of the near-equilibrium concentrations of phosphocreatine and cellular pH together with measurements of the total extractable concentrations of phosphocreatine and creatine allowed calculation of the free ADP/ATP ratio in the cell. The calculated ratio of approximately 2 was considerably higher than the ratio of between 0.06 and 0.1 measured directly in cell extracts

  15. 31P-NMR analysis of congestive heart failure in the SHHF/Mcc-facp rat heart.

    Michael O'Donnell, J; Narayan, P; Bailey, M Q; Abduljalil, A M; Altschuld, R A; McCune, S A; Robitaille, P M

    1998-02-01

    31P-NMR was used to monitor myocardial bioenergetics in compensated and failing SHHF/MCC-fa(cp) (SHF) rat hearts. The SHHF/Mcc-fa(cp) (spontaneous hypertension and heart failure) rat is a relatively new genetic model in which all individuals spontaneously develop congestive heart failure, most during the second year of life. Failing SHF rat hearts displayed a pronounced decrease in resting PCr:ATP ratios (Ppressure products (RRP, mmHg X beats/min) from 44.5+/-1.4 to 66.6+/-3. 4 K with dobutamine infusion, whereas hearts in end-stage failure were able to increase their RPP from baseline values of 27+/-4 K to only 37+/-7 K. The data indicate that a pronounced decline in PCr and total creatine signals the transition from compensatory hypertrophy to decompensation and failure in the SHF rat model of hypertensive cardiomyopathy. PMID:9515000

  16. 13C/31P NMR studies on the role of glucose transport/phosphorylation in human glycogen supercompensation.

    Price, T B; Laurent, D; Petersen, K F

    2003-05-01

    This study measured muscle glycogen during a 7-day carbohydrate loading protocol. Twenty healthy subjects (12 male, 8 female) performed 1 hr treadmill/toe-raise exercise immediately before a 3-day low carbohydrate (LoCHO) diet (20 % carbohydrate, 60 % fat, 20 % protein). On day 3 they repeated the exercise and began a 4-day high carbohydrate (HiCHO) diet (90 % carbohydrate, 2 % fat, 8 % protein). The order of administration of the diet was reversed in a subpopulation (n = 3). Interleaved natural abundance 13C/ 31P NMR spectra were obtained before and immediately after exercise, and each day during the controlled diets in order to determine concentrations of glycogen (GLY), glucose-6-phosphate (G6P), and muscle pH. Following exercise, muscle GLY and pH were reduced (p supercompensation. PMID:12784164

  17. 31P NMR study of magnetic phase transitions of MnP single crystal under 2 GPa pressure

    Fan, GuoZhi; Zhao, Bo; Wu, Wei; Zheng, Ping; Luo, JianLin

    2016-05-01

    Superconductivity on the border of the long-range magnetic order has been discovered in MnP under high pressures. In order to investigate the nature of the magnetic properties adjacent to the superconducting state, we performed zero-field 31P NMR for MnP single crystal under ambient and hydrostatic pressure of 2 GPa, respectively. Radio frequency power level was used to determine whether NMR signal originates from a helical state or not. When 2 GPa pressure was applied, the signal from helical state exists even above 160 K, while that from the ferromagnetic phase was not observed. Our NMR results indicate that the magnetic phase which is adjacent to the superconducting state is in a helical magnetic structure.

  18. Effects of chloramphenicol on brain energy metabolism using 31P spectroscopy: influences on sleep-wake states in rat.

    Chahboune, Halima; Mahdjoub, Rachid; Desgoutte, Pierre; Rousset, Colette; Briguet, André; Cespuglio, Raymond

    2008-08-01

    Effects of chloramphenicol (antibiotic inhibiting complex-1 of respiratory chain) and thioamphenicol (TAP, a structural analog of CAP inactive on complex-1) were examined on cerebral energy metabolites and sleep-wake cycle architecture in rat. In the first group, animals were chronically equipped with a cranial surface resonator and (31)P spectroscopic measurements were performed using a 2 T magnetic resonance spectrometer (operating frequency 34.46 MHz). CAP administration (400 mg/kg, tail vein, light period) induced deficits in phosphocreatine (-30%, p electrodes for EEG and electromyogram recordings. CAP administered intraperitoneally at light-onset reduced rapid-eye movement (REM) sleep (-60% in the first 6 h of light period, p EEG were, respectively, increased and decreased (p EEG. Overall, these data indicate that REM sleep occurrence is linked to an aerobic production of ATP. PMID:18507739

  19. A two-compartment phantom for VOI profile measurements in small-bore 31P MR spectroscopy

    Vikhoff, Babro; Stubgaard, Max; Stensgaard, Anders;

    1998-01-01

    A two-compartment gel phantom for VOI profile measurements in volume-selective 31P spectroscopy in small-bore units is presented. The phantom is cylindrical with two compartments divided by a very thin (30 microm) polyethene film. This thin film permits measurements with a minimum of susceptibility...... influences from the partition wall. The phantom was used for evaluation of the volume selection method ISIS (image-selected in vivo spectroscopy). The position of the phantom was fixed in the magnet during the measurements, while the volume of interest (VOI) was moved stepwise over the border. The signal...... from the two compartments was measured for each position and the data were evaluated following differentiation. We have found this phantom suitable for VOI profile measurements of ISIS in small-bore systems. The phantom forms a useful complement to recommended phantoms for small bore-spectroscopy...

  20. A two-compartment phantom for VOI profile measurements in small-bore 31P MR spectroscopy

    A two-compartment gel phantom for VOI profile measurements in volume-selective 31P spectroscopy in small-bore units is presented. The phantom is cylindrical with two compartments divided by a very thin (30 μm) polyethene film. This thin film permits measurements with a minimum of susceptibility influences from the partition wall. The phantom was used for evaluation of the volume selection method ISIS (image-selected in vivo spectroscopy). The position of the phantom was fixed in the magnet during the measurements, while the volume of interest (VOI) was moved stepwise over the border. The signal from the two compartments was measured for each position and the data were evaluated following differentiation. We have found this phantom suitable for VOI profile measurements of ISIS in small-bore systems. The phantom forms a useful complement to recommended phantoms for small bore-spectroscopy. (author)

  1. Characterization of phosphorus forms in lake macrophytes and algae by solution (31)P nuclear magnetic resonance spectroscopy.

    Feng, Weiying; Zhu, Yuanrong; Wu, Fengchang; Meng, Wei; Giesy, John P; He, Zhongqi; Song, Lirong; Fan, Mingle

    2016-04-01

    Debris from aquatic macrophytes and algae are important recycling sources of phosphorus (P), which can result in continuing blooms of algae by recycling bioavailable P in the eutrophic lakes. However, knowledge of forms of P in aquatic macrophytes and algae and their contribution to internal loads of P in lakes is limited. Without such knowledge, it is difficult to develop appropriate strategies to remediate and or restore aquatic ecosystems that have become eutrophic. Therefore, in this work, P was extracted from six types of aquatic macrophytes and algae collected from Tai Lake of China and characterized by use of solution (31)P-nuclear magnetic resonance (NMR) spectroscopy. When extracted by 0.5 M NaOH-25 mM EDTA, extraction recovery of total P(TP) and organic P(Po) exceeded 90 %. Concentrations of Po in algae and aquatic macrophytes were 5552 mg kg(-1) and 1005 mg kg(-1) and accounted for 56.0 and 47.2 % of TP, respectively. When Po, including condensed P, was characterized by solution (31)P-NMR Po in algae included orthophosphate monoesters (79.8 %), pyrophosphate (18.2 %), and orthophosphate diester (2.0 %), and Po in aquatic macrophytes included orthophosphate monoesters (90.3 %), pyrophosphate (4.2 %), and orthophosphate diester (5.5 %). Additionally, orthophosphate monoesters in algal debris mainly included β-glycerophosphate (44.1 %), α-glycerophosphate (13.5 %), and glucose 6-phosphate (13.5 %). Orthophosphate monoesters in aquatic macrophytes mainly included β-glycerophosphate (27.9 %), α-glycerophosphate (24.6 %), and adenosine 5' monophosphate (8.2 %). Results derived from this study will be useful in better understanding nutrient cycling, relevant eutrophication processes, and pollution control for freshwater lakes. PMID:26681323

  2. Reproducibility of Creatine Kinase Reaction Kinetics in Human Heart: A 31P Time Dependent Saturation Transfer Spectroscopy

    Bashir, Adil; Gropler, Robert

    2014-01-01

    Creatine Kinase (CK) is essential for buffering and rapid regeneration of adenosine triphosphate (ATP) in heart tissue. Herein we demonstrate a 31P magnetic resonance spectroscopy (MRS) protocol to quantify CK reaction kinetics in human myocardium at 3T. Furthermore we sought to quantify the test–retest reliability of the measured metabolic parameters. The method localizes 31P signal from heart using modified 1D image selected in vivo spectroscopy (ISIS) and a time dependent saturation transfer (TDST) approach was used to measure CK reaction parameters. Fifteen healthy volunteers (22 measurements total) were tested. The CK reaction rate constant (kf) was 0.32 ± 0.05 sec−1 and coefficient of variation (CV) = 15.62%. Intrinsic T1 for phosphocreatine (PCr) was 7.36 ± 1.79 sec with CV = 24.32%. These values are consistent those previously reported. PCr/ATP ratio was equal to 1.94 ± 0.15 with CV = 7.73%, which is within the range of healthy subjects. The reproducibility of the technique was tested in 7 subjects and inferred parameters such as kf and T1 exhibited good reliability (intraclass correlation coefficient (ICC) = 0.90 and 0.79 for kf and T1 respectively). The reproducibility data provided in this study will enable calculation of power and sample sizes required for clinical and research studies. The technique will allow for the examination of cardiac energy metabolism in clinical and research studies providing insight in the relationship between energy deficit and functional deficiency in heart. PMID:24706347

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

    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.

  4. Tumour oxygenation assessed by polarographic needle electrodes and bioenergetic status measured by 31P magnetic resonance spectroscopy im human soft tissue tumours

    The purpose of this study was to evaluate the feasibility of polarographic oxygen electrode measurements and phosphorus magnetic resonance spectroscopy (31P-MRS) in extravisceral soft tissue tumours, designated to receive preoperative radiotherapy. Pretreatment tumour oxygenation was determined in 41 cases and 31P-MRS was amenable to lesions in 34 patients. Biopsies were characterized histopathologically as 25 primary soft tissue sarcomas (STS), 2 recurrent STS, 9 benign and 5 other malignancies. Evaluation of phosphorus (31P) spectra was possible in 11 cases. The oxygenation status of normal tissue was higher than that of tumours, whereas no difference was found between oxygenation status of benign lesions and that of STS. There was substantial variation between tumours in the median pO2 and the bioenergetic status (β-NTP/Pi). No correlation was found between tumour pO2 and volume (n=25). Moreover, there was no correlation between β-NTP/Pi and the median tumour pO2, the fraction of pO2 values ≤2.5 mm Hg or tumour volume (n=10), respectively. In conclusion, oxygen electrode assessment was found to be a clinically applicable and feasible technique for measuring tumour oxygenation status, whereas the success of 31P-MRS in human neoplasms was limited by a very poor resolution in the phosphorus signal that allowed analysis of 31P spectra in 11 tumours out of 34 cases. (orig.)

  5. Evaluation of recombinant CXCL8(3-73)K11R/G31P in muscle fibrosis and Trichinella larvae encapsulation in a murine model of trichinellosis.

    Yan, Wenhui; Li, Fang; Qin, Yuanhua; Ren, Yixin; Zheng, Lili; Dai, Xiaodong; Mao, Weifeng; Cui, Yu

    2016-06-01

    Trichinella spiralis (T. spiralis) larvae in raw or inadequately cooked meat can cause chronic infections in a wide range of hosts including humans. During the development inside the skeletal muscles, T. spiralis larvae infect muscle cells accompanying with the infiltration of host inflammatory cells, eventually create a new type of cell known as nurse cell developing a surrounding vascular network to support the larvae development. Controlling of host inflammatory responses and angiogenesis influences both the nurse cell differentiation and the parasite larvae development. CXCL8 is a chemokine that acts on G-protein coupled receptors, of which activation contributes to fibrosis and angiogenesis. CXCL8(3-73)K11R/G31P (G31P) has been reported as a CXCL8 analogue. The aim of this study is to investigate the effect of G31P in inflammatory responses and the development of T. spiralis larvae in muscle tissues of mice infected with T. spiralis. The level of inflammatory factors and the morphology of T. spiralis larvae in infected tissues were investigated through ELISA and electron-microscopy analysis. G31P up-regulated IFN-γ and down-regulated CXCL8 level, and impaired the encapsulation of T. spiralis larvae in vivo. The results showed that G31P influenced the development of T. spiralis larvae in muscle tissues. PMID:27089392

  6. Real time response of brain phosphocreatine to a 4S workload determined by 31P fMRS

    Full text: Phosphocreatine (PCr) is suggested to play a major role in buffering ATP in the brain and, as such, upon induction of mental work, PCr is initially the major source of high-energy phosphate bonds. We have developed a real-time functional magnetic resonance spectroscopy (fMRS) protocol using the 31P nucleus which enables us to measure levels of high-energy phosphate compounds (ATP and PCr), brain pH and inorganic phosphate in response to an intense mental workload (4s of 8Hz flashing chequerboard stimulation). Using this paradigm we have obtained data with 0.5 s time resolution. This improves upon previous published time resolution of 3.5 s. The new paradigm shows that PCr levels decrease immediately following stimulus onset with levels recovering rapidly following stimulus cessation. This recovery results in an overshoot of resting levels before rebounding slightly and recovering to back resting levels ∼ 16s after cessation of stimulus. In this respect, the timecourse of PCr consumption and resupply mirrors those of glucose and oxygen under conditions of transient oxygen and glucose debt. During the same period cerebral pH increases linearly from resting levels. This is consistent with continual sequestration of H+ by ADP, reflecting synthesis of ATP. This suggests that the energy debt resulting from the workload is ongoing for some time following cessation of stimulus. Copyright (2002) Australian Neuroscience Society

  7. Physiological effects of the form of nitrogen on corn root tips: a 31P nuclear magnetic resonance study

    Physiological effects of different N forms (NO−3, NH+4, or a combination of both) on corn (Zea mays L.) root tips and leaves were studied by following 31P signals with a nuclear magnetic resonance spectrometer. With root tips, both cytoplasmic and vacuolar pH could be measured, whereas with leaves, only vacuolar pH could be determined. The N treatments did not affect the cytoplasmic pH of corn root tips in contrast to proposals of previous workers. Leaf vacuolar pH was higher and root tip vacuolar pH lower with NO−3 than with NH+4. Under anaerobic conditions, cytoplasmic pH was reduced because of lactic acid fermentation. Nitrate, an electron acceptor, delayed the acidification of the cytoplasm compartment because it represents an alternative way to reoxidize NADH. In conclusion, for the conditions of these experiments, the pH of the cytoplasm of corn root tips was not modified by the form of N absorbed; however, the pH of this compartment was affected by the form of N presented during development anaerobiosi. (author)

  8. Characterization of the phosphoserine of pepsinogen using /sup 31/P nuclear magnetic resonance: corroboration of X-ray crystallographic results

    Williams, S.P.; Bridger, W.A.; James, M.N.G.

    1986-10-21

    The endogenous phosphoserine residue in porcine pepsinogen has been titrated with use of phosphorus-31 nuclear magnetic resonance (/sup 31/P NMR). It has an observed pK/sub a/sub 2// of 6.7 and a narrow line width (approx. =10 Hz). The phosphate can be readily removed by an acid phosphatase from potato; however, it is resistant to hydrolysis by several alkaline phosphatases. The X-ray crystal structure of porcine pepsinogen at 1.8-A resolution shows a rather weak and diffuse region of electron density in the vicinity of the phosphorylated serine residue. This suggests considerable dynamic mobility or conformational disorder of the phosphate. In order to define more fully this behavior the NMR data have been used to corroborate these crystallographic results. All these physical data are consistent with a highly mobile phosphoserine residue on the surface of the zymogen and freely exposed to solvent. In addition, certain properties of this phosphoserine moiety on pepsinogen are similar to those of one of the phosphorylated residues of ovalbumin. The possible significance of this is discussed.

  9. Characterization of the phosphoserine of pepsinogen using 31P nuclear magnetic resonance: corroboration of X-ray crystallographic results

    The endogenous phosphoserine residue in porcine pepsinogen has been titrated with use of phosphorus-31 nuclear magnetic resonance (31P NMR). It has an observed pK/sub a2/ of 6.7 and a narrow line width (≅10 Hz). The phosphate can be readily removed by an acid phosphatase from potato; however, it is resistant to hydrolysis by several alkaline phosphatases. The X-ray crystal structure of porcine pepsinogen at 1.8-A resolution shows a rather weak and diffuse region of electron density in the vicinity of the phosphorylated serine residue. This suggests considerable dynamic mobility or conformational disorder of the phosphate. In order to define more fully this behavior the NMR data have been used to corroborate these crystallographic results. All these physical data are consistent with a highly mobile phosphoserine residue on the surface of the zymogen and freely exposed to solvent. In addition, certain properties of this phosphoserine moiety on pepsinogen are similar to those of one of the phosphorylated residues of ovalbumin. The possible significance of this is discussed

  10. Spectroscopic quantification of soil phosphorus forms by {sup 31}P-NMR after nine years of organic or mineral fertilization

    Gatiboni, Luciano Colpo, E-mail: gatiboni@cav.udesc.br [Universidade Estadual de Santa Catarina (UDESC), Lages, SC (Brazil); Brunetto, Gustavo; Rheinheimer, Danilo dos Santos; Kaminski, Joao; Flores, Alex Fabiani Claro; Lima, Maria Angelica Silveira; Girotto, Eduardo; Copetti, Andre Carlos Cruz, E-mail: danilo.rheinheimer@pq.cnpq.br, E-mail: joao.kaminski@gmail.com, E-mail: acflores@quimica.ufsm.br, E-mail: masl32003@gmail.com, E-mail: girottosolos@gmail.com, E-mail: andrecopetti@yahoo.com.br [Universidade Federal de Santa Maria (UFSM), RS (Brazil); Pandolfo, Carla Maria; Veiga, Milton, E-mail: pandolfo@epagri.sc.gov.br, E-mail: milveiga@epagri.sc.gov.br [Empresa de Pesquisa Agropecuaria e Extensao Rural de Santa Catarina (EPAGRI), Campos Novos, SC (Brazil)

    2013-05-15

    Long-standing applications of mineral fertilizers or types of organic wastes such as manure can cause phosphorus (P) accumulation and changes in the accumulated P forms in the soil. The objective of this research was to evaluate the forms of P accumulated in soils treated with mineral fertilizer or different types of manure in a long-term experiment. Soil was sampled from the 0-5 cm layer of plots fertilized with five different nutrient sources for nine years: 1) control without fertilizer; 2) mineral fertilizer at recommended rates for local conditions; 3) 5 t ha{sup -1} year{sup -1} of moist poultry litter; 4) 60 m{sup 3} ha{sup -1} year{sup -1} of liquid cattle manure and 5) 40 m{sup 3} ha{sup -1} year{sup -1} of liquid swine manure. The {sup 31}P-NMR spectra of soil extracts detected the following P compounds: orthophosphate, pyrophosphate, inositol phosphate, glycerophosphate, and DNA. The use of organic or mineral fertilizer over nine years did not change the soil P forms but influenced their concentration. Fertilization with mineral or organic fertilizers stimulated P accumulation in inorganic forms. Highest inositol phosphate levels were observed after fertilization with any kind of manure and highest organic P concentration in glycerophosphate form in after mineral or no fertilization. (author)

  11. 1H-1H correlations across N-H···N hydrogen bonds in nucleic acids

    In 2HJNN-COSY experiments, which correlate protons with donor/acceptor nitrogens across Nd···HNa bonds, the receptor nitrogen needs to be assigned in order to unambiguously identify the hydrogen bond. For many situations this is a non-trivial task which is further complicated by poor dispersion of (Na,Nd) resonances. To address these problems, we present pulse sequences to obtain direct, internucleotide correlations between protons in uniformly 13C/15N labeled nucleic acids containing Nd···HNa hydrogen bonds. Specifically, the pulse sequence H2(N1N3)H3 correlates H2(A,ω1):H3(U,ω2) protons across Watson-Crick A-U and mismatched G·A base pairs, the sequences H5(N3N1)H1/H6(N3N1)H1 correlate H5(C,ω1)/H6(C,ω1):H1(G,ω2) protons across Watson-Crick G-C base pairs, and the H2(N2N7)H8 sequence correlates NH2(G,A,C;ω1):H8(G,A;ω2) protons across G·G, A·A, sheared G·A and other mismatch pairs. These 1H-1H connectivities circumvent the need for independent assignment of the donor/acceptor nitrogen and related degeneracy issues associated with poorly dispersed nitrogen resonances. The methodology is demonstrated on uniformly 13C/15N labeled samples of (a) an RNA regulatory element involving the HIV-1 TAR RNA fragment, (b) a multi-stranded DNA architecture involving a G·(C-A) triad-containing G-quadruplex and (c) a peptide-RNA complex involving an evolved peptide bound to the HIV-1 Rev response element (RRE) RNA fragment

  12. In vivo measurement of intracellular pH in human brain during different tensions of carbon dioxide in arterial blood. A 31P-NMR study

    Jensen, K E; Thomsen, C; Henriksen, O

    1988-01-01

    The effect of changes in carbon dioxide tension in arterial blood upon intracellular pH in brain tissue was studied in seven healthy volunteers, aged 22-45 years. The pH changes were monitored by use of 31P nuclear magnetic resonance spectroscopy, performed on a whole-body 1.5 Tesla Siemens imaging...

  13. Spin-lattice relaxation time of inorganic phosphate in human tumor xenografts measured in vivo by 31P-magnetic resonance spectroscopy. Influence of oxygen tension

    Previous 31P-magnetic resonance spectroscopy (31P-MRS) studies have suggested that the spin-lattice relaxation time (T1) of the inorganic phosphate (Pi) resonance is shorter in well-oxygenated than in poorly oxygenated tumors. Amelanotic human melanoma xenografts were therefore subjected to 31P-MRS to investigate whether the T1 of the Pi resonance might be a useful parameter for assessment of tumor oxygenation status. It was searched for possible correlations between the T1 of the Pi resonance and oxygen tension or parameters closely related to oxygen tension, including 31P-MRS tumor energy status and blood supply per viable tumor cell. Oxygen tension, tumor energy status, and blood supply per viable tumor cell decreased with increasing tumor volume. In contrast to previous suggestions, the T1 of the Pi resonance decreased with increasing tumor volume and decreasing oxygen tension, tumor energy status, and blood supply per viable tumor cell, possibly because the tumors developed necrotic regions concomitantly with the decrease in oxygenation status, resulting in increased concentrations of freely dissolved para-magnetic ions in the tissue. Consequently, the T1 of the Pi resonance can probably not be utilized to estimate the oxygenation status of tumors, at least not in tumors with necrotic regions. (orig.)

  14. Brief Report: Approaches to [Superscript 31]P-MRS in Awake, Non-Sedated Children with and without Autism Spectrum Disorder

    Erickson, Laura C.; Scott-Van Zeeland, Ashley A.; Hamilton, Gavin; Lincoln, Alan; Golomb, Beatrice A.

    2012-01-01

    We piloted a suite of approaches aimed to facilitate a successful series of up to four brain and muscle [superscript 31]Phosphorus-Magnetic Resonance Spectroscopy ([superscript 31]P-MRS) scans performed in one session in 12 "awake", non-sedated subjects (ages 6-18), 6 with autism spectrum disorders (ASD) and 6 controls. We targeted advanced…

  15. Metabolic changes of masseter muscle in experimental unilateral bite-raised rat determined by {sup 31}P-MRS

    Nishide, Naoto [Kyoto Prefectural Univ. of Medicine (Japan)

    1997-05-01

    Occlusal interference is known to alter the functional activity of masticatory muscle, but no alteration of the energy metabolism of masticatory muscle which has gone occlusal interference has been reported. The purpose of this study was to investigate the energy metabolism in rat masseter muscle during masticatory movements following unilateral bite-raising. A bite-raising splint (1 mm) was fixed on the unilateral upper molar of experimental rats, and after 2, 4 and 6 weeks, the rats were anesthetized and masticatory movements were induced by electrical stimulation applied to the masseter muscle (with a biting force of 40 g, a frequency of 5 Hz and a stimulation time of 32 min). {sup 31}P Magnetic Resonance Spectroscopy of the masseter muscle were recorded during a sequence of rest, stimulation and recovery periods, and the resonance signal area ratio of PCr and Pi ((PCr)/(PCr + Pi)) and the muscle pH were determined. After 4 and 6 weeks following the bite-raising, the masseter of the bite-raised side showed a decrease in the (PCr)/(PCr + Pi) ratio compared with a control group during stimulation (p<0.05). Neither the bite-raised side masseter at 2 weeks and the contralateral side at 4 weeks showed any differences compared with the control. The muscle pH during stimulation was similar in both the control and the bite-raised groups of rats. These findings suggest that the occlusal alteration induced by unilateral bite-raising reduces the masseter energy level during mastication. (author)

  16. Metabolic changes of masseter muscle in experimental unilateral bite-raised rat determined by 31P-MRS

    Occlusal interference is known to alter the functional activity of masticatory muscle, but no alteration of the energy metabolism of masticatory muscle which has gone occlusal interference has been reported. The purpose of this study was to investigate the energy metabolism in rat masseter muscle during masticatory movements following unilateral bite-raising. A bite-raising splint (1 mm) was fixed on the unilateral upper molar of experimental rats, and after 2, 4 and 6 weeks, the rats were anesthetized and masticatory movements were induced by electrical stimulation applied to the masseter muscle (with a biting force of 40 g, a frequency of 5 Hz and a stimulation time of 32 min). 31P Magnetic Resonance Spectroscopy of the masseter muscle were recorded during a sequence of rest, stimulation and recovery periods, and the resonance signal area ratio of PCr and Pi ((PCr)/(PCr + Pi)) and the muscle pH were determined. After 4 and 6 weeks following the bite-raising, the masseter of the bite-raised side showed a decrease in the (PCr)/(PCr + Pi) ratio compared with a control group during stimulation (p<0.05). Neither the bite-raised side masseter at 2 weeks and the contralateral side at 4 weeks showed any differences compared with the control. The muscle pH during stimulation was similar in both the control and the bite-raised groups of rats. These findings suggest that the occlusal alteration induced by unilateral bite-raising reduces the masseter energy level during mastication. (author)

  17. Partial trisomy 2q due to a maternal balanced translocation t(2;22) (q31;p12)

    Steinberg, L.S.; Bleiman, M.; Punnett, H.H. [St. Christopher`s Hospital for Children, Philadelphia, PA (United States)] [and others

    1994-09-01

    Features consistent among reported patients with 2q duplications due to familial translocations or de novo duplications include pre- and postnatal growth failure, ocular defects such as congenital glaucoma, cardiac defects, micrognathia, urogenital defects, renal defects, connective tissue laxity, neurologic defects, and dermatologic abnormalities. Genotype/phenotype correlations of patients with trisomy 2q due to familial translocations are complicated by the presence of the deletions of the other chromosome involved. We have had the opportunity to observe `pure` trisomy 2q31-qter resulting from adjacent-1 segregation from 46,XX,t(2;22)(q31;p12) in a carrier mother with apparent loss of the 22 NOR region. He was the 2453 gm product of a gestation complicated by gestational diabetes to a 29-year-old G1 P0 mother and a 30-year-old father. At birth, he was noted to have hypotonia, micrognathia, microphthalmia, left cryptorchidism, hypospadias, bilateral clinodactyly of the fifth digits, mild hyperextensibility of the joints, dry skin disorder, and bilateral hydronephrosis by ultrasound. He was treated for hypoglycemia in the nursery and had a vesicostomy at two months for vesicoureteral reflux. A hearing test at two months found moderate hearing loss in the right ear and mild to moderate hearing loss in the left ear. At 3 months he had surgery for a PDA and bilateral glaucoma and was treated for periods of hypothermia and type IV renal tubular acidosis. This patient and others with unbalanced translocations involving the NOR region of an acrocentric chromosome allow for genotype/phenotype correlation of the `pure` trisomic region.

  18. 31P nuclear magnetic resonance studies of the association of basic proteins with multilayers of diacyl phosphatidylserine.

    Smith, R; Cornell, B A; Keniry, M A; Separovic, F

    1983-08-10

    Lysozyme, cytochrome c, poly(L-lysine), myelin basic protein and ribonuclease were used to form multilayer dispersions containing about 50% protein (by weight) with bovine brain diacyl phosphatidylserine (PS). 31P nuclear magnetic resonance shift anisotropies, spin-spin (T2) and spin-lattice (T1) relaxation times for the lipid headgroup phosphorus were measured at 36.44 MHz. At pH 7.5, lysozyme, cytochrome c, poly(L-lysine) and ribonuclease were shown to increase the chemical shift anisotropy of PS by between 12-20%. Myelin basic protein altered the shape of the phosphate resonance, suggesting the presence of two lipid components, one of which had a modified headgroup conformation. The presence of cytochrome c led to the formation of a narrow spike at the isotropic shift position of the spectrum. Of the various proteins or peptides we have studied, only poly(L-lysine) and cytochrome c had any effect on the T1 of PS (1050 ms). Both caused a 20-30% decrease in T1 of the lamellar-phase phosphate peak. The narrow peak in the presence of cytochrome c had a very short T1 of 156 ms. The possibility is considered that the cytochrome Fe3+ contributes to the phosphate relaxation in this case. The effect of all proteins on the T2 of the phosphorus resonance was to cause an increase from the value for pure PS (1.6 ms) to between 2 and 5 ms. The results obtained with proteins are compared with the effects of small ions and intrinsic membrane proteins on the order and motion of the headgroups of lipids in bilayers. PMID:6191774

  19. Analysis of intracranial cystic disease on 1H MR spectroscopy

    Objective: To analyze the features of intracrayze the features of intracranial cystic diseases on 1H MRS, and to evaluate the applicable value of 1H MRS. Methods: Fifty-two patients were examinated by single voxel 1H MRS, included I-II graded astrocytomas (n=8), glioblastomas (n=9), metastasis (n=13), brain abscesses (n=10), epidermoids (n=4), anachnoid cysts (n=5), brain Cysticerciasis (n=3). Results: (1) There was only Lac in I-II graded astrocytomas. But in glioblastomas, as were as all showed Lac, 4 cases showed low Cho and NAA and 2 cases Lip. (2) In 13 metastasis patients, 7 cases only presented Lac, 6 cases showed Cho, 3 cases showed low NAA and 6 ones Lip. (3) In brain abscesses, all showed Lac, 9 cases displayed AA, 6 cases showed Ace, 5 cases appeared Suc and Ala, 2 eases had Lip. (4) Four eases of epidermoid showed Lac, one showed Lip. In 4 arachnoid cysts, 2 cases had low Lac, one showed Lip. Three cases of cysticercosis showed Lac, Ace, Suc, Ala and no AA, Cho, NAA. Conclusion: Lac is the most common resonance peak on 1H MRS in intracranial cystic diseases and for no diagnostic specificity. AA combined Ace, Suc, and Ala are highly specificity for brain abscess. Ace, Suc and Ala appearance cues the the possible existence of cysticercosis. 1H MRS is helpful for the qualitative diagnosis of intracranial disease. (authors)

  20. Analysis of cardiac energy metabolism in valve disease using {sup 31}P-MR-spectroscopy; Untersuchungen des kardialen Energiestoffwechsels bei Herzvitien mit der {sup 31}P-MR-Spektroskopie

    Beer, M.; Viehrig, M.; Seyfarth, T.; Sandstede, J.; Lipke, C.; Pabst, T.; Kenn, W.; Hahn, D. [Wuerzburg Univ. (Germany). Inst. fuer Roentgendiagnostik; Harre, K.; Horn, M.; Neubauer, S. [Wuerzburg Univ. (Germany). Medizinische Klinik; Landschuetz, W.; Kienlin, M. von [Wuerzburg Univ. (Germany). Physikalisches Inst. 5

    2000-02-01

    Patients and methods: 10 healthy volunteers and 10 patients with aortic stenosis (pressure gradients >60 mmHg) were included. For assessment of energy metabolism, {sup 31}P-MR spectra were obtained with a double oblique 3D-CSI technique (voxel size 25 cm{sup 3}). In 5 of 10 patients, follow-up examination was performed 3 months after surgical valve replacement (SVR). Left ventricular (LV) function was analyzed by cine MRI. Results: Before SVR the myocardial phosphocreatine to adenosinetriphosphate (PCr-ATP) ratio was significantly (p=0.0002) reduced to 0.80{+-}0.25 in patients compared to 1.65{+-}0.21 in volunteers. 3 months after SVR, LV mass had significantly (p=0.04) decreased from 238{+-}33 g to 206{+-}47 g. At the same time a significant (p=0.04) increase of the PCr-ATP ratio from 0.80{+-}0.25 to 1.28{+-}0.22 was observed. A slight, but not significant, reduction of the phosphodiester ATP ratio was observed before SVR, with a trend towards normalization after SVR. (orig.) [German] Patienten und Methode: 10 gesunde Probanden und 10 Patienten mit Aortenklappenstenose (Druckgradient >60 mmHg) wurden untersucht. Zur Erfassung des kardialen Energiestoffwechsels wurde eine doppelt angulierbare 3D-CSI-Technik verwendet (Voxelgroesse 25 ccm). 3 Monate nach Aortenklappenersatz (AKE) erfolgte bei 5 Patienten eine Nachkontrolle. Bei den Patienten wurden zusaetzlich linksventrikulaere (LV) Funktionsparameter mittels cine-MRI-Technik analysiert. Ergebnisse: Vor Klappenersatz war bei den Patienten das Phosphokreatin-Adenosintriphosphat (PCr-ATP)-Verhaeltnis mit 0,80{+-}0,25 signifikant im Vergleich zu Gesunden (1,65{+-}0,21; p=0,0002) erniedrigt. 3 Monate nach AKE konnte eine signifikante (p=0,04) Verringerung der LV-Masse von 238{+-}33 g auf 206{+-}47 g nachgewiesen werden. Die LV-Ejektionsfraktion aenderte sich jedoch nicht wesentlich (von 61{+-}11% auf 65{+-}7%; p=0,22). Zur selben Zeit zeigte sich ein signifikanter (p=0,04) Anstieg des PCr-ATP-Verhaeltnis von 0

  1. Hyperfine interactions in MnAs studied by perturbed angular correlations of $\\gamma$-rays using the probe $^{77}$Br $\\rightarrow ^{77}$Se and first principles calculations for MnAs and other Mn pnictides

    Gonçalves, J N; Correia, J G; Lopes, A M L

    2011-01-01

    The MnAs compound shows a first-order transition at T$_{c}$≈ 42$^{\\circ}$C, and a second-order transition at T$_{t}$ ≈120$^{\\circ}$C. The first-order transition, with structural (hexagonal-orthorhombic), magnetic (FM-PM) and electrical conductivity changes, is associated to magnetocaloric, magnetoelastic, and magnetoresistance effects. We report a study in a large temperature range from −196$^{\\circ}$C up to 140$^{\\circ}$C, using the $\\gamma\\!-\\!\\gamma$ perturbed angular correlations method with the radioactive probe $^{77}$Br→$^{77}$Se, produced at the ISOLDE-CERN facility. The electric field gradients and magnetic hyperfine fields are determined across the first- and second-order phase transitions encompassing the pure and mixed phase regimes in cooling and heating cycles. The temperature irreversibility of the 1st order phase transition is seen locally, at the nanoscopic scale sensitivity of the hyperfine field, by its hysteresis, detailing and complementing information obtained with macroscopic me...

  2. 脑胶质瘤的1H MRS

    杨桂芬; 田伟

    2005-01-01

    活体质子磁共振波谱(proton magnetic resonance spectroscopy,1H MRS)由于能够无创性检测肿瘤组织及正常表观组织代谢物的变化,目前在胶质瘤的分级、诊断、范围确定及鉴别诊断中有积极的应用价值。本文主要介绍1H MRS在胶质瘤中的研究现状。

  3. Localized double-quantum-filtered 1H NMR spectroscopy

    Thomas, M. A.; Hetherington, H. P.; Meyerhoff, D. J.; Twieg, D. B.

    The image-guided in vivo spectroscopic (ISIS) pulse sequence has been combined with a double-quantum-filter scheme in order to obtain localized and water-suppressed 1H NMR spectra of J-coupled metabolites. The coherence-transfer efficiency associated with the DQ filter for AX and A 3X spin systems is described. Phantom results of carnosine, alanine, and ethanol in aqueous solution are presented. For comparison, the 1H NMR spectrum of alanine in aqueous solution with the binomial (1331, 2662) spin-echo sequence is also shown.

  4. Optical absorption, 31P NMR, and photoluminescence spectroscopy study of copper and tin co-doped barium–phosphate glasses

    The optical and structural properties of 50P2O5:50BaO glasses prepared by melting have been investigated for additive concentrations of 10 and 1 mol% of CuO and SnO dopants. Absorption and photoluminescence spectroscopies were employed in the optical characterization, whereas structural properties were assessed by 31P nuclear magnetic resonance (NMR) spectroscopy. Residual Cu2+ was detectable by absorption spectroscopy for the highest concentration of CuO and SnO. More prominently, the optical data suggests contributions from both twofold-coordinated Sn centers and Cu+ ions to light absorption and emission in the glasses. The luminescence depends strongly on excitation wavelength for the highest concentration of dopants where a blue–white emission is observed under short-wavelength excitation (e.g., 260 nm) largely due to tin, while an orange luminescence is exhibited for longer excitation wavelengths (e.g., 360 nm) essentially due to Cu+ ions. On the other hand, dissimilar luminescent properties were observed in connection to Cu+ ions for the lowest concentration studied, as the copper ions were preferentially excited in a narrower range at shorter wavelengths near tin centers absorption. The structural analyses revealed the glass matrix to be composed essentially of Q2 (two bridging oxygens) and Q1 (one bridging oxygen) phosphate tetrahedra. A slight increase in the Q1/Q2 ratio reflected upon SnO doping alone suggests a major incorporation of tin into the glass network via P–O–Sn bonds, compatible with the 2-coordinated state attributed to the luminescent Sn centers. However, a significant increase in the Q1/Q2 ratio was indicated with the incorporation of copper at the highest concentration, consistent with a key role of the metal ions as network modifiers. Thus, the change in Cu+ optical properties concurs with different distributions of local environments around the ions induced by variation in metal ion concentration. Luminescence decay curve

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

    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...

  6. 1H NMR spectroscopy-based interventional metabolic phenotyping

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

    2010-01-01

    1H NMR spectroscopy-based metabolic phenotyping was used to identify biomarkers in the plasma of patients with rheumatoid arthritis (RA). Forty-seven patients with RA (23 with active disease at baseline and 24 in remission) and 51 healthy subjects were evaluated during a one-year follow-up with...

  7. Main: 1H1Y [RPSD[Archive

    Full Text Available 1H1Y イネ Rice Oryza sativa L. D-Ribulose-5-Phosphate ... 3-Epimerase Oryza Sativa Molecule: D-Ribul ... ose-5-Phosphate ... 3-Epimerase; Chain: A, B; Engineered: Yes Isomeras ... e 5.1.3.1 (D-Ribulose-5-Phosphate ... 3-Epimerase) S.Jelakovic, G.E.Schulz S.Jelakovic, ...

  8. Main: 1H1Z [RPSD[Archive

    Full Text Available 1H1Z イネ Rice Oryza sativa L. D-Ribulose-5-Phosphate ... 3-Epimerase Oryza Sativa Molecule: D-Ribul ... ose-5-Phosphate ... 3-Epimerase; Chain: A, B; Engineered: Yes Isomeras ... e 5.1.3.1 (D-Ribulose-5-Phosphate ... 3-Epimerase) S.Jelakovic, G.E.Schulz S.Jelakovic, ...

  9. Liver Metabolite Concentrations Measured with 1H MR Spectroscopy

    Ouwerkerk, Ronald; PETTIGREW, RODERIC I.; Gharib, Ahmed M.

    2012-01-01

    In vivo measurement of liver choline concentrations in healthy humans is feasible, and even measurement of glycogen can be achieved in some patients at 3.0 T with point-resolved 1H MR spectroscopy by using navigator-guided synchronization to respiratory motion and state-of-the-art B0 field shimming techniques.

  10. Applications of 1H-NMR to Biodiesel Research

    Biodiesel is an alternative diesel fuel derived from vegetable oils, animal fats, or used cooking oils. It is produced by reacting these materials with an alcohol in the presence of a catalyst to give the corresponding mono-alkyl esters. 1H-NMR is a routine analytical method that has been used for...

  11. A compilation of information on the {sup 31}P(p,{alpha}){sup 28}Si reaction and properties of excited levels in the compound nucleus {sup 32}S

    Miller, R.E.; Smith, D.L. [Argonne National Lab., IL (United States). Technology Development Div.

    1997-11-01

    This report documents a survey of the literature, and provides a compilation of data contained therein, for the {sup 31}P(p,{alpha}){sup 28}Si reaction. Attention is paid here to resonance states in the compound-nuclear system {sup 32}S formed by {sup 31}P + p, with emphasis on the alpha-particle decay channels, {sup 28}Si + {alpha} which populate specific levels in {sup 28}Si. The energy region near the proton separation energy for {sup 32}S is especially important in this context for applications in nuclear astrophysics. Properties of the excited states in {sup 28}Si are also considered. Summaries of all the located references are provided and numerical data contained in them are compiled in EXFOR format where applicable.

  12. 31P NMR study of the stoichiometry and stability of several mercury(II) halides with a phosphorus ylide in different solvents

    Sabounchei, Seyyed Javad; Pourshahbaz, Mahbubeh; Hasan Zebarjadian, Mohammad; Keypour, Hassan; Bordbar, Maryam

    2013-02-01

    31P NMR measurements were employed to monitor the stoichiometry and stability of complexes between HgCl2, HgBr2 and HgI2 with 4-methylbenzoylmethylenetriphenylphosphorane (L) in acetonitrile (AN), dimethylsulfoxide (DMSO), dimethylformamide (DMF) and tetrahydrofuran (THF) solvents of varying composition. In all cases studied, the variation of 31P chemical shift with the [M]/[L] mole ratio indicated the formation of 1:1 complexes. The formation constants of the resulting complexes were evaluated from computer fitting of the mole ratio data to an equation that relates the observed chemical shifts to the formation constant. In all solvents used, the stabilities of the resulting 1:1 complexes varied in the order HgCl2 > HgBr2 > HgI2.

  13. Maintenance of high-energy brain phosphorous compounds during insulin-induced hypoglycemia in men. 31P nuclear magnetic resonance spectroscopy study

    Hilsted, Jannik; Jensen, K E; Thomsen, C;

    1988-01-01

    31P nuclear magnetic resonance (NMR) spectroscopy allows noninvasive studies of cerebral energy-rich phosphorous compounds in humans. In an attempt to characterize the relationship between peripheral blood glucose concentrations and whole-brain phosphate metabolism during insulin...... constant during the experiment. These results show that the integrated brain profile of energy-rich phosphorous compounds is unaffected by experimental insulin-induced hypoglycemia in humans....

  14. Study of semi-conductor spectrometers for high counting rates. Application to the study of the reaction 31P (p, α0): Ep < 2 MeV

    The study of nuclear reactions involving particles of low charge (E 31P shows which are the factors limiting the resolving power. In the second part we examine the various types of spectrometer which can be used in the case of a high count-rate. We have built an apparatus which can be used for carrying out spectrometry on particles produced by nuclear reactions, for a total, count-rate of 105 counts/sec. (author)

  15. Evidence for fast oscillations in the He(31P) total emission cross section in He+-Ne low-energy collisions

    High energy resolution measurements of the He(31P) total emission cross section in He+-Ne low centre-of-mass energy (30 eV-2000 eV) collisions show a very complex structure. The emission cross section reveals fast and low-amplitude oscillations superimposed on slow, high-amplitude oscillations. The latter can be interpreted with the Rosenthal model, but the former constitute a new and original feature, the origin of which is not clear. (author)

  16. 31P magnetic resonance spectroscopy to measure in vivo cardiac energetics in normal myocardium and hypertrophic cardiomyopathy: Experiences at 3 T

    Background: 31P magnetic resonance spectroscopy (MRS) allows measurement of in vivo high-energy phosphate kinetics in the myocardium. While traditionally 31P cardiac spectroscopy is performed at 1.5 T, cardiac MRS at higher field strength can theoretically increase signal to noise ratio (SNR) and spectral resolution therefore improving sensitivity and specificity of the cardiac spectra. The reproducibility and feasibility of performing cardiac spectroscopy at 3 T is presented here in this study in healthy volunteers and patients with hypertrophic cardiomyopathy. Methods: Cardiac spectroscopy was performed using a Phillips 3T Achieva scanner in 37 healthy volunteers and 26 patients with hypertrophic cardiomyopathy (HCM) to test the feasibility of the protocol. To test the reproducibility a single volunteer was scanned eight times on separate occasions. A single voxel 31P MRS was performed using Image Selected In vivo Spectroscopy (ISIS) volume localization. Results: The mean phosphocreatine/adenosine triphosphate (PCr/ATP) ratio of the eight measurements performed on one individual was 2.11 ± 0.25. Bland Altman plots showed a variance of 12% in the measurement of PCr/ATP ratios. The PCr/ATP ratio was significantly reduced in HCM patients compared to controls, 1.42 ± 0.51 and 2.11 ± 0.57, respectively, P 31P MRS at 3 T is a reliable method of measuring in vivo high-energy phosphate kinetics in the myocardium for clinical studies and diagnostics. Based on our data an impairment of cardiac energetic state in patients with hypertrophic cardiomyopathy is indisputable.

  17. Assessment of preparation methods for organic phosphorus analysis in phosphorus-polluted Fe/Al-rich Haihe river sediments using solution 31P-NMR.

    Wenqiang Zhang

    Full Text Available Fe/Al-rich river sediments that were highly polluted with phosphorus (P were used in tests to determine the optimum preparation techniques for measuring organic P (Po using solution (31P nuclear magnetic resonance spectroscopy ((31P-NMR. The optimum pre-treatment, extraction time, sediment to solution ratio and sodium hydroxide-ethylenediaminetetraacetic acid (NaOH-EDTA extractant solution composition were determined. The total P and Po recovery rates were higher from freeze- and air-dried samples than from fresh samples. An extraction time of 16 h was adequate for extracting Po, and a shorter or longer extraction time led to lower recoveries of total P and Po, or led to the degradation of Po. An ideal P recovery rate and good-quality NMR spectra were obtained at a sediment:solution ratio of 1:10, showing that this ratio is ideal for extracting Po. An extractant solution of 0.25 M NaOH and 50 mM EDTA was found to be more appropriate than either NaOH on its own, or a more concentrated NaOH-EDTA mixture for (31P-NMR analysis, as this combination minimized interference from paramagnetic ions and was appropriate for the detected range of Po concentrations. The most appropriate preparation method for Po analysis, therefore, was to extract the freeze-dried and ground sediment sample with a 0.25 M NaOH and 50 mM EDTA solution at a sediment:solution ratio of 1:10, for 16 h, by shaking. As lyophilization of the NaOH-EDTA extracts proved to be an optimal pre-concentration method for Po analysis in the river sediment, the extract was lyophilized as soon as possible, and analyzed by (31P-NMR.

  18. Application of pulsed-gradient 31P NMR on frog muscle to measure the diffusion rates of phosphorus compounds in cells

    Pulsed-gradient 31P NMR was used to measure the diffusion rates of phosphorus compounds in aqueous solution and in living muscles. The diffusion rates of creatine phosphate and inorganic phosphate in intact frog muscle cells were reduced by a factor of approx. 2 from those in aqueous solution, which suggests that the apparent intracellular viscosity is approx. 2 times larger than in aqueous solution

  19. Silencing of the glycerophosphocholine phosphodiesterase GDPD5 alters the phospholipid metabolite profile in a breast cancer model in vivo as monitored by 31P Magnetic Resonance Spectroscopy

    Wijnen, J.P.; Jiang, L.; Greenwood, T.R.; Cheng, M; Döpkens, M.; Cao, M.D.; Bhujwalla, Z M; Krishnamachary, B; Klomp, D. W. J.; Glunde, K.

    2014-01-01

    Abnormal choline phospholipid metabolism is an emerging hallmark of cancer, which is implicated in carcinogenesis and tumor progression. The malignant metabolic phenotype is characterized by high levels of phosphocholine (PC) and relatively low levels of glycerophosphocholine (GPC) in aggressive breast cancer cells. Phosphorus Magnetic Resonance Spectroscopy (31P MRS) is able to noninvasively detect these water-soluble metabolites of choline as well as ethanolamine phospholipid metabolism. He...

  20. [31P-NMR analysis of high energy phosphorous compounds (ATP and phosphocreatine) in the living rat brain--effects of halothane anesthesia and a hypoxic condition].

    Yuasa, T; Miyatake, T; Kuwabara, T; Umeda, M; Eguchi, K

    1983-11-01

    31phosphorus nuclear magnetic resonance (31P-NMR) measurements have provided new and valuable insights for studying the metabolism of living systems. The aim of this paper is to introduce a technique of application of 31P-NMR measurements using a surface coil method, and to discuss the effects of halothane anesthesia and hypoxic hypoxia on the energetic metabolism of intact rat brains. All measurements were made using a JEOL FX 270 spectrometer with a super conducting magnet of 54-mm bore diameter. The magnetic field intensity of this machine is 6.3 tesla, and the resonance frequency used for 31P was 109.14 MHz. We remodelled an ordinary probe to take a live rat, and the animals were made to inhale anesthetic halothane or mixture of oxygen and nitrogen at various concentrations controlled by a flow regulator. The best conditions for measurements with our surface coil method were determined in this study as follows: (1) 90 degrees pulse width and selectivity, Fig. 1 shows signal selectivity in depthwise direction changed with 90 degrees pulse width, which was set to 20 microseconds. (2) Sensitivity and resolution; To obtain a spectrum of 31P-NMR from a rat brain 500 accumulations of free induction decays were considered suitable for both time and space resolution. Fig. 2 shows variations of signal intensity with pulse repetition time, which was set to 2 sec. It took about 17 min for averaging to get a spectrogram. (3) Quantitative accuracy and qualification; As shown in Fig. 3, a linear relationship was found between the signal intensity of beta-phosphate of ATP and the concentration of ATP solutions, thus proving the quantitative accuracy of our systems.(ABSTRACT TRUNCATED AT 250 WORDS) PMID:6661335

  1. 31P magnetic resonance spectroscopy of the Sherpa heart: a phosphocreatine/adenosine triphosphate signature of metabolic defense against hypobaric hypoxia.

    Hochachka, P W; Clark, C M; Holden, J E; Stanley, C; Ugurbil, K; Menon, R S

    1996-01-01

    Of all humans thus far studied, Sherpas are considered by many high-altitude biomedical scientists as most exquisitely adapted for life under continuous hypobaric hypoxia. However, little is known about how the heart is protected in hypoxia. Hypoxia defense mechanisms in the Sherpa heart were explored by in vivo, noninvasive 31P magnetic resonance spectroscopy. Six Sherpas were examined under two experimental conditions [normoxic (21% FiO2) and hypoxic (11% FiO2) and in two adaptational state...

  2. Value of dynamic 31p magnetic resonance spectroscopy technique in in vivo assessment of the skeletal muscle mitochondrial function in type 2 diabetes

    WU Fei-yun; TU Hui-juan; QIN Bin; CHEN Ting; XU Hua-feng; QI Jing; WANG De-hang

    2012-01-01

    Background Phosphorous magnetic resonance spectroscopy (31p-MRS) has been successfully applied to study intracellular membrane compounds and high-energy phosphate metabolism.This study aimed to evaluate the capability of dynamic 31p-MRS for assessing energy metabolism and mitochondrial function in skeletal muscle from type 2 diabetic patients.Methods Dynamic 31p-MRS was performed on 22 patients with type 2 diabetes and 26 healthy volunteers.Spectra were acquired from quadriceps muscle while subjects were in a state of rest,at exercise and during recovery.The peak areas of inorganic phosphate (Pi),phosphocreatine (PCr),and adenosine triphosphate (ATP) were measured.The concentration of adenosine diphosphate (ADP) and the intracellular pH value were calculated from the biochemistry reaction equilibrium.The time constant and recovery rates of Pi,PCr,and ADP were analyzed using exponential curve fitting.Results As compared to healthy controls,type 2 diabetes patients had significantly lower skeletal muscle concentrations of Pi,PCr and β-ATP,and higher levels of ADP and Pi/PCr.During exercise,diabetics experienced a significant Pi peak increase and PCr peak decrease,and once the exercise was completed both Pi and PCr peaks returned to resting levels.Quantitatively,the mean recovery rates of Pi and PCr in diabetes patients were (10.74±1.26) mmol/s and (4.74±2.36) mmol/s,respectively,which was significantly higher than in controls.Conclusions Non-invasive quantitative 31P-MRS is able to detect energy metabolism inefficiency and mitochondrial function impairment in skeletal muscle of type 2 diabetics.

  3. Treatment of glycogenosys type V (McArdle disease) with creatine and ketogenic diet with clinical scores and with 31P-MRS on working leg muscle

    Vorgerd, M; Zange, J

    2007-01-01

    McArdle’s disease is caused by genetic defects of the musclespecific isozyme of glycogen phosphorylase, which block ATP formation from glycogen in skeletal muscle. Creatine supplementation and ketogenic diet have been tested as potential supplements for muscle energy metabolism which may improve muscle symptomatic. Outcome measures were clinical scores describing muscle symptomatic and parameters derived from 31P-MRS examinations on working muscle. In two placebo controlled cross-over studies...

  4. Different early effect of irradiation in brain and small cell lung cancer examined by in vivo 31P-magnetic resonance spectroscopy

    Kristjansen, P E; Pedersen, A G; Quistorff, B;

    1992-01-01

    Early effects of irradiation were evaluated by non-invasive in vivo 31P-magnetic resonance spectroscopy (31P-MRS) of two small cell lung cancer (SCLC) tumor lines CPH SCCL 54A and 54B, in nude mice. The tumors were originally derived from the same patient and have similar morphology and growth...... characteristics, but a different radiosensitivity. The 54A tumors are twice as radiosensitive as the 54B's. In the present study the tumors were treated with 2.5, 10, and 40 Gy. For comparison, nude mice were given cranial irradiation at the same three doses, and the effect was evaluated by in vivo 31P-MRS. No...... effect was observed in brain at any dose level. In contrast, 40 Gy induced a statistically significant reduction in ATP/Pi ratio during the 12-h post-irradiation period. This effect was more pronounced in 54A than in 54B. Some reduction was observed following 10 Gy, whereas 2.5 Gy induced no changes in...

  5. 31P magnetic resonance spectroscopy study of influences of cranial irradiation on cerebral energy metabolism in children with acute lymphoblastic leukemia

    The effect of cranial irradiation on the cerebrum was studied. Energy metabolism in the brain was assessed before and after cranial irradiation using 31P magnetic resonance spectroscopy (31P-MRS). The subjects were 3 pediatric patients with initial acute lymphotic leukemia (ALL), who underwent induction chemotherapy and central nervous system (CNS) prophylaxis according to the ALL high risk 911 protocol of Children's Cancer and Leukemia Study Group. The patients underwent 31P-MRS within one week before and after prophylactic CNS irradiation with a total dose of 18 Gy (i.e., 0.5 Gy in two fractions, 1.0 Gy in two fractions, and 1.5 Gy in 10 fractions - 4 times a week in 3-4 weeks). All 3 patients showed a decrease in phosphocreatine and ATP levels, which are indicators of energy metabolism, and also in the intracellular pH level in the brain tissue. Cranial irradiation was thus suggested to induce hypoxia in the brain tissue. (S.Y.)

  6. Reproducibility and influencing factors of 31P MR spectroscopy in rabbit liver with two-dimensional chemical shift imaging

    .05). Conclusions: The relative quantification of hepatic β-ATP may be most reliable among the phosphorus metabolites for rabbit liver because of its good reproducibility and small CV. The quantification of phosphorus metabolites by 31P MRS with 2D CSI in rabbit liver is affected by many factors. (authors)

  7. 5-Pentyl-4-phenylsulfonyl-1H-pyrazol-3-ol

    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.

  8. 2-Methyl-1H-benzimidazol-3-ium hydrogen phthalate

    YuanQi Yu; Haidong He; Kai Tong; Shouwen Jin; Feng Lin

    2011-01-01

    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.

  9. Laundering and Deinking Applications of 1H NMR Imaging

    Tutunjian, P. N.; Borchardt, J. K.; Prieto, N. E.; Raney, K. H.; Ferris, J. A.

    One-dimensional 1H NMR imaging techniques are used to visualize oil removal from fabrics and paper fibers immersed in aqueous solutions of nonionic detergents. The method provides a unique approach to the study of oil-removal kinetics in nonionic detergent systems where traditional optical techniques fail due to solution turbidity. The only requirement of the NMR experiment is the use of deuterated water in order to selectively image the hydrocarbon phase. Preliminary applications to laundering and paper deinking are discussed.

  10. Hochfeld 1H-NMR-Mikroskopie zur biophysikalischen Grundlagenforschung

    Haddad, Daniel

    2005-01-01

    Dank der mit modernen NMR-Spektrometern (Kernspintomographen) routinemäßig realisierbaren isotropen räumlichen Auflösungen von wenigen Mikrometern, ergeben sich für die 1H NMR-Mikroskopie zahlreiche neue Anwendungsgebiete. Allerdings sind die Möglichkeiten und Grenzen der NMR-Mikroskopie bezüglich ihrer praktischen Anwendbarkeit bisher nur wenig untersucht worden. Die vorliegende Arbeit ist im Bereich der biophysikalischen Grundlagenforschung angesiedelt und soll die praktische Anwendbarkeit ...

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

    Zhang, Rongchun; Nishiyama, Yusuke; Ramamoorthy, Ayyalusamy

    2015-10-01

    A proton-detected 3D 1H/13C/1H chemical shift correlation experiment is proposed for the assignment of chemical shift resonances, identification of 13C-1H connectivities, and proximities of 13C-1H and 1H-1H nuclei under ultrafast magic-angle-spinning (ultrafast-MAS) conditions. Ultrafast-MAS is used to suppress all anisotropic interactions including 1H-1H 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) 1H/1H and 2D 13C/1H (F2/F3) chemical shift correlation spectra extracted from the 3D spectrum enable the identification of 1H-1H proximity and 13C-1H connectivity. In addition, the 2D (F1/F2) 1H/13C chemical shift correlation spectrum, incorporated with proton magnetization exchange via the fp-RFDR recoupling of 1H-1H dipolar couplings, enables the measurement of proximities between 13C and even the remote non-carbon-bonded protons. The 3D experiment also gives three-spin proximities of 1H-1H-13C chains. Experimental results obtained from powder samples of L-alanine and L-histidine ṡ H2O ṡ HCl demonstrate the efficiency of the 3D experiment.

  12. Proton-detected 3D 14N/14N/1H isotropic shift correlation experiment mediated through 1H-1H RFDR mixing on a natural abundant sample under ultrafast MAS

    Pandey, Manoj Kumar; Nishiyama, Yusuke

    2015-09-01

    In this contribution, we have demonstrated a proton detection-based approach on a natural abundant powdered L-Histidine HCl-H2O sample at ultrafast magic angle spinning (MAS) to accomplish 14N/14N correlation from a 3D 14N/14N/1H isotropic shift correlation experiment mediated through 1H finite-pulse radio frequency-driven recoupling (fp-RFDR). Herein the heteronuclear magnetization transfer between 14N and 1H has been achieved by HMQC experiment, whereas 14N/14N correlation is attained through enhanced 1H-1H spin diffusion process due to 1H-1H dipolar recoupling during the RFDR mixing. While the use of ultrafast MAS (90 kHz) provides sensitivity enhancement through increased 1H transverse relaxation time (T2), the use of micro-coil probe which can withstand strong 14N radio frequency (RF) fields further improves the sensitivity per unit sample volume.

  13. Changes in energy metabolism in the quadriceps femoris after a single bout of acute exhaustive swimming in rats: a 31p-magnetic resonance spectroscopy study

    Sun Yingwei; Pan Shinong; Chen Zhian; Zhao Heng; Ma Ying; Zheng Liqiang; Li Qi

    2014-01-01

    Background Little is known about the value of 31P-magnetic resonance spectroscopy (31P-MRS) in in vivo assessment of exhaustive exercise-induced injury in skeletal muscle.We aimed to evaluate the value of a 31P-MRS study using the quadriceps femoris after a single bout of acute exhaustive swimming in rats,and the correlation between 31P-MRS and histological changes.Methods Sixty male Sprague-Dawley rats were randomly assigned to control,half-exhaustive,and exhaustive exercise groups.31P-MRS of the quadriceps femoris of the right lower limb was performed immediately after swimming exercise to detect Pi,PCr,and β-ATP.The Pi/PCr,Pi/β-ATP,PCr/β-ATP,and PCr/(PCr+Pi) were calculated and pH measured.Areas under the receiver operating characteristic curve (AUCs) were calculated to evaluate the diagnostic potential of 31P-MRS in identifying and distinguishing the three groups.HE staining,electron microscopy and desmin immunostaining after imaging of the muscle were used as a reference standard.The correlation between 31P-MRS and the mean absorbance (A value) of desmin staining were analyzed with the Pearson correlation test.Results Pi,PCr,Pi/PCr,and PCr/(PCr+Pi) showed statistically significant intergroup differences (P<0.05).AUCs of Pi,PCr,Pi/PCr,and PCr/(PCr+Pi) were 0.905,0.848,0.930,and 0.930 for the control and half-exhaustive groups,while sensitivity and specificity were 90%/85%,95%/55%,95%/80%,and 90%/85%,respectively.The AUCs of Pi,PCr,Pi/PCr and PCr/(PCr+Pi) were 0.995,0.980,1.000,and 1.000 for the control and exhaustive groups,while sensitivity and specificity were 95%/90%,100%/90%,100%/95%,and 100%/95%,respectively.The AUCs of Pi,PCr,Pi/PCr,and PCr/(PCr+Pi) were 0.735,0.865,0.903,and 0.903 for the half-exhaustive and exhaustive groups,while sensitivity and specificity were 80%/60%,90%/75%,95%/65%,and 95%/70%,respectively.In the half-exhaustive group,some muscle fibers exhibited edema in HE staining,and the

  14. Dynamic 1H NMR Studies of Schiff Base Derivatives

    Köylü, M. Z.; Ekinci, A.; Böyükata, M.; Temel, H.

    2016-01-01

    The spin-lattice relaxation time T 1 and the spin-spin relaxation time T 2 of two Schiff base derivatives, N,N'-ethylenebis(salicylidene)-1,2-diaminoethane (H2L1) and N,N'-ethylenebis (salicylidene)-1,3-diaminopropane (H2L2), in DMSO-d6 solvent were studied as a function of temperature in the range of 20-50°C using a Bruker Avance 400.132 MHz 1H NMR spectrometer. Based on the activation energy ( E a) and correlation time (τc), we believe that the Schiff base derivatives perform a molecular tumbling motion.

  15. Localization of epileptogenic focus by 1H MR spectroscopy

    In fourteen patients suffering from pharmacoresistant epilepsy with partial complex seizures, 1H MR spectra from the left and right hippocampus were assessed. From the ratios NAA/Cr, NAA/Cho and NAA/(Cr+Cho) the asymmetry coefficient was calculated which characterizes the reduced NAA (N-acetyl aspartate) concentration in the assumed epileptogenic focus. An agreement between MRS and the EEG findings was found in 10 out of 14 cases, i.e. in 71%. MR spectroscopy is therefore another non-invasive diagnostic method suitable for the assessment of lateralization of an epileptic focus before epileptosurgery. (author) 2 tabs., 3 figs., 30 refs

  16. 2-Methyl-1H-benzimidazol-3-ium hydrogen phthalate

    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.

  17. 1H MR spectroscopy characteristics of cerebral alveolar echinococcosis

    Objective: To investigate the characteristics of proton magnetic resonance spectroscopy (1H MRS) in patients with cerebral alveolar echinococcosis (CAE). Methods: Thirteen patients with 33 lesions proven to be CAE histologically and clinically were examined by conventional MRI and 2D multi-voxel spectroscopy with a 3.0 T double gradient superconductivity magnetic resonance scanner. Concentrations of the metabolites containing N-acetyl-aspartic-acid (NAA), Choline (Cho), Creatine (Cr), lipids and lactic acid (Lip + Lac), myo-Inositol (mI) were detected and the value of Cho/Cr, NAA/Cr, (Lip + Lac)/Cr, mI/Cr were calculated. The values of Cho/Cr, NAA/Cr, (Lip + Lac)/Cr, mI/Cr were compared between the lesions and the contralateral normal brain parenchyma. Statistical analysis was performed using the Wilcoxon signed-rank test. Results: CAE 1H MRS in the lesions was characterized by the decrease of Cho, NAA to varying degrees, and a visible lipid with or without lactate peak. Compared with the control group, the ratio of NAA/Cr was decreased markedly, whereas Cho/Cr, mI/Cr increased mildly and (Lip + Lac)/Cr increased markedly in the lesions. The medians and interquartile ranges of Cho/Cr, NAA/Cr, (Lip + Lac)/Cr and mI/Cr in the lesions were: 1.88 (1.24-2.23), 1.32 (1.07-1.58), 32.96 (24.59-47.30) and 0.91 (0.67-1.08), respectively. The medians and interquartile ranges of Cho/Cr, NAA/Cr, (Lip + Lac)/Cr and mI/Cr of control group were 0.84 (0.704-0.98), 2.00 (1.80-2.18), 0.90 (0.74-0.99) and 0.26 (0.18-0.31), respectively. There were statistically significant differences of the measures between the lesions and the control regions (Z=-5.932, -6.086, -6.946, -6.984, P<0.01). Conclusions: Multi-voxel 1H MRS can reflect pathological characteristics of CAE. 1H MRS provides metabolic information for diagnosis of CAE and may be a supplement to conventional magnetic resonance examination. (authors)

  18. Enhanced spectral resolution in RNA HCP spectra for measurement of 3JC2'P and 3JC4'P couplings and 31P chemical shift changes upon weak alignment

    The 'out-and-back' 3D HCP experiment, using gradient- and sensitivity-enhanced detection, provides a convenient method for assignment of the 31P NMR spectra and accurate measurement of the 31P chemical shifts of ribonucleic acids. The 13C resolution in such spectra can be doubled, at the cost of a 50% reduction in sensitivity, by combining 13C evolution during the 13C-31P de- and rephasing periods. The multiple connectivities observable for a given 31P, including correlations to the intranucleotide C5'H2 and C4'H groups, and the C2'H, C3'H and C4'H groups of the preceding nucleotide, permit independent measurements of the 31P shift. The 13C spectrum of these groups is typically crowded for an RNA molecule in isotropic solution and overlap becomes more problematic in media used to achieve partial alignment. However, many of these correlations are resolvable in the combined-evolution HCP spectrum. The difference in 31P chemical shift between isotropic solution and a medium containing liquid crystalline Pf1 provides information on the orientation of phosphate groups. The intensities measured in the 3D HCP spectrum, obtained for an isotropic sample, yield values for the 3JC2'P and 3JC4'P couplings, thereby providing important restraints for the backbone torsion angles ε and β. The experiments are illustrated for a uniformly 13C-enriched, 24-residue stem-loop RNA sequence, and results for the helical stem region show close agreement between observed Δδ(31P) values and those predicted for a model A-form RNA helix when using a uniform 31P CSA tensor. This confirms that Δδ(31P) values can be used directly as restraints in refining nucleic acid structures

  19. Early Detection of Myocardial Bioenergetic Deficits: A 9.4 Tesla Complete Non Invasive 31P MR Spectroscopy Study in Mice with Muscular Dystrophy.

    Weina Cui

    Full Text Available Duchenne muscular dystrophy (DMD is the most common fatal form of muscular dystrophy characterized by striated muscle wasting and dysfunction. Patients with DMD have a very high incidence of heart failure, which is increasingly the cause of death in DMD patients. We hypothesize that in the in vivo system, the dystrophic cardiac muscle displays bioenergetic deficits prior to any functional or structural deficits. To address this we developed a complete non invasive 31P magnetic resonance spectroscopy (31P MRS approach to measure myocardial bioenergetics in the heart in vivo.Six control and nine mdx mice at 5 months of age were used for the study. A standard 3D -Image Selected In vivo Spectroscopy (3D-ISIS sequence was used to provide complete gradient controlled three-dimensional localization for heart 31P MRS. These studies demonstrated dystrophic hearts have a significant reduction in PCr/ATP ratio compare to normal (1.59±0.13 vs 2.37±0.25, p<0.05.Our present study provides the direct evidence of significant cardiac bioenergetic deficits in the in vivo dystrophic mouse. These data suggest that energetic defects precede the development of significant hemodynamic or structural changes. The methods provide a clinically relevant approach to use myocardial energetics as an early marker of disease in the dystrophic heart. The new method in detecting the in vivo bioenergetics abnormality as an early non-invasive marker of emerging dystrophic cardiomyopathy is critical in management of patients with DMD, and optimized therapies aimed at slowing or reversing the cardiomyopathy.

  20. Changes of high-energy phosphorous compounds in skeletal muscle during glucose-induced thermogenesis in man. A 31P MR spectroscopy study

    Thomsen, C; Jensen, Karl Erik; Astrup, A;

    1989-01-01

    By the use of invasive techniques, skeletal muscle has been shown to contribute to thermogenesis induced by glucose in humans. In an attempt to study this phenomenon by a non-invasive method, this study investigated intracellular high-energy phosphorous compounds in calf muscle by 31P MR......H remained unchanged after the glucose administration. No changes were seen in the control experiments. The processes responsible for the decreased energy state of the skeletal muscle cell may be an obligatory conversion of glucose to glycogen. Also, facultative processes, such as sodium/potassium pumping...

  1. Interference effect involving doubly excited states [1s2p](3,1P)3p2 (J=1) in 1s photoionization of neon

    Within the framework of multiconfiguration Dirac-Fock (MCDF) method, the interference between photoionization and photoexcitation autoionization involving the doubly excited states [1s2p](3,1P)3p2 (J=1) of neon have been studied theoretically. The present results indicate the fine structure of the interference spectra in experiment and show the dominant contribution to the total profile resulting from some individual resonances. Reasonable agreement is found between the present calculations and other available theoretical and experimental results. In addition, some interesting trends of variation of Fano parameters q and ρ2 have also been pointed out. (author)

  2. Hydrophobization of epoxy nanocomposite surface with 1H,1H,2H,2H-perfluorooctyltrichlorosilane for superhydrophobic properties

    Psarski, Maciej; Marczak, Jacek; Celichowski, Grzegorz; Sobieraj, Grzegorz; Gumowski, Konrad; Zhou, Feng; Liu, Weimin

    2012-10-01

    Nature inspires the design of synthetic materials with superhydrophobic properties, which can be used for applications ranging from self-cleaning surfaces to microfluidic devices. Their water repellent properties are due to hierarchical (micrometer- and nanometre-scale) surface morphological structures, either made of hydrophobic substances or hydrophobized by appropriate surface treatment. In this work, the efficiency of two surface treatment procedures, with a hydrophobic fluoropolymer, synthesized and deposited from 1H,1H,2H,2H-perfluorooctyltrichlorosilane (PFOTS) is investigated. The procedures involved reactions from the gas and liquid phases of the PFOTS/hexane solutions. The hierarchical structure is created in an epoxy nanocomposite surface, by filling the resin with alumina nanoparticles and micron-sized glass beads and subsequent sandblasting with corundum microparticles. The chemical structure of the deposited fluoropolymer was examined using XPS spectroscopy. The topography of the modified surfaces was characterized using scanning electron microscopy (SEM), and atomic force microscopy (AFM). The hydrophobic properties of the modified surfaces were investigated by water contact and sliding angles measurements. The surfaces exhibited water contact angles of above 150° for both modification procedures, however only the gas phase modification provided the non-sticking behaviour of water droplets (sliding angle of 3°). The discrepancy is attributed to extra surface roughness provided by the latter procedure.

  3. Radio observations of the CMa OB1 H II regions

    A sensitive 100 x 150 13-cm map made of the CMa OB1 H II regions' radio emission shows a strong similarity to Hα emission photographs. Sharpless 296 is shown to consist of a prominent central and western arc completed by a weaker southern loop, and with a faint northern bar. The emission is thermal, superimposed over a predominantly non-thermal background. The H142α recombination line has been detected at eight positions in S296, and in S292 and S297. The average electron temperature in S296 is 6900 +- 1300 K. The UV fluxes from the CMa OB1 stars account for the observed emission measures of the H II regions. The H142α 1sr velocities indicate that the ionized material is in contact with the molecular clouds. (author)

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

    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.

  5. A study of 1H-MR spectroscopy in the prefrontal cortex and amygdala of heroine abusers

    Objective: To explore the characteristic findings of 1H-MR spectroscopy (1H-MRS) in the prefrontal cortex and amygdala of patients with heroine dependence (HD), and the relationship to total cumulative dose of inhaled heroine. Methods: Fourteen male HD patients and 12 healthy controls (HC) underwent 1H-MRS at the prefrontal cortex and amygdala regions. The total cumulative in haled heroin dose was (852±341) g in HD. Ratios of N-acetylaspartate/creatine(NAA/Cr) and choline/creatine (Cho/Cr) were respectively measured in the prefrontal cortex and bilateral amygdale regions. The student's t test and the linear correlation were employed for statistical analysis. Results: Compared to HC group, HD patients had a significant lower ratio of NAA/Cr in the prefrontal cortex (1.44±0.46 vs 1.50±0.75, t=1.77, P< 0.05), left amygdala region (1.32±0.08 vs 1.42±0.08, t=3.41, P<0.05), and right amygdala region (1.34±0.09 vs 1.44±0.10, t=2.63, P<0.05), the HD patients had a significant increased ratio of Cho/Cr in the prefrontal cortex (0.92±0.06 vs 0.86±0.08, t=2.31, P<0.05), left amygdala region (1.20±0.12 vs 1.07±0.04, t=3.60, P<0.05) and right amygdala region(1.26±0.15 vs 1.12±0.11, t=2.60, P<0.05). There was a negative linear correlation between the total cumulative inhaled heroine dose and the ratio of NAA/Cr in the prefrontal cortex (r=-0.9159, P<0.01), left amygdala region( r= -0.8756, P<0.01), and right amygdala region (r=-0.9399, P<0.01) respectively. Conclusions: The study indicates that neuronal damage and glial proliferation may occur in the prefrontal cortex and amygdala region, which suggests the abnormalities of executive function and emotion in patients with HD. A relationship exists between the heroin-induced metabolic abnormality and the total cumulative dose of inhaled heroine. (authors)

  6. 31P NMR characterization and efficiency of new types of water-insoluble phosphate fertilizers to supply plant-available phosphorus in diverse soil types.

    Erro, Javier; Baigorri, Roberto; Yvin, Jean-Claude; Garcia-Mina, Jose M

    2011-03-01

    Hydroponic plant experiments demonstrated the efficiency of a type of humic acid-based water-insoluble phosphate fertilizers, named rhizosphere controlled fertilizers (RCF), to supply available phosphorus (P) to different plant species. This effect was well correlated to the root release of specific organic acids. In this context, the aims of this study are (i) to study the chemical nature of RCF using solid-state (31)P NMR and (ii) to evaluate the real efficiency of RCF matrix as a source of P for wheat plants cultivated in an alkaline and acid soil in comparison with traditional water-soluble (simple superphosphate, SSP) and water-insoluble (dicalcium phosphate, DCP) P fertilizers. The (31)P NMR study revealed the formation of multimetal (double and triple, MgZn and/or MgZnCa) phosphates associated with chelating groups of the humic acid through the formation of metal bridges. With regard to P fertilizer efficiency, the results obtained show that the RCF matrix produced higher plant yields than SSP in both types of soil, with DCP and the water-insoluble fraction from the RCF matrix (WI) exhibiting the best results in the alkaline soil. By contrast, in the acid soil, DCP showed very low efficiency, WI performed on a par with SSP, and RCF exhibited the highest efficiency, thus suggesting a protector effect of humic acid from soil fixation. PMID:21254775

  7. 31P-MR-spectroscopy of the skeletal muscles under load: demonstration of normal energy metabolism compared to different neuromuscular diseases

    Purpose: 31P-MR spectroscopy of skeletal muscle under ecercise was used to obtain the range of normal variation and comparison was made for different neuromascular diseases. Methods: 41 examinations of 24 volunteers and 41 investigations in 35 patients were performed on 1.5 T MR systems (Gyroscan S15 und S15/ACSII, Philips). Localised 31P-MR spectra of the calf muscle were obtained in time series with a resolution of 12 s. Results: Two types of muscle energy metabolism were identified from the pattern of spectroscopic time course in volunteers: While the first group was characterised by a remarkable decline to lower pH values during exercise, the second group showed only small pH shifts (minimum pH: 6.48±0.13 vs 6.87±0.07, p-6) although comparable workload conditions were maintained. The pH-values correlated well with blood lactate analysis. Patients with metabolic disorders and chronic fatigue syndrome (CFS) showed decreased resting values of PCr/(PCr+Pi) and increased pH levels during exercise. PCr recovery was significantly delayed (0.31 vs 0.65 min-1, pi), altered pH time courses, and decreased PCr recovery seem to be helpful indicators for diagnosis of metabolic muscle disorders. (orig./MG)

  8. On the use of (31)P NMR for the quantification of hydrosoluble phosphorus-containing compounds in coral host tissues and cultured zooxanthellae.

    Godinot, Claire; Gaysinski, Marc; Thomas, Olivier P; Ferrier-Pagès, Christine; Grover, Renaud

    2016-01-01

    (31)P Nuclear Magnetic Resonance (NMR) was assessed to investigate the phosphorus-containing compounds present in the tissues of the scleractinian coral Stylophora pistillata as well as of cultured zooxanthellae (CZ). Results showed that phosphorus-containing compounds observed in CZ were mainly phosphate and phosphate esters. Phosphate accounted for 19 ± 2% of the total phosphorus compounds observed in CZ maintained under low P-levels (0.02 μM). Adding 5 mM of dissolved inorganic phosphorus (KH2PO4) to the CZ culture medium led to a 3.1-fold increase in intracellular phosphate, while adding 5 mM of dissolved organic phosphorus led to a reduction in the concentration of phosphorus compounds, including a 2.5-fold intracellular phosphate decrease. In sharp contrast to zooxanthellae, the host mainly contained phosphonates, and to a lesser extent, phosphate esters and phosphate. Two-months of host starvation decreased the phosphate content by 2.4 fold, while bleaching of fed corals did not modify this content. Based on (31)P NMR analyses, this study highlights the importance of phosphonates in the composition of coral host tissues, and illustrates the impact of phosphorus availability on the phosphorus composition of host tissues and CZ, both through feeding of the host and inorganic phosphorus enrichment of the CZ. PMID:26902733

  9. A high-energy X-ray diffraction, 31P and 11B solid-state NMR study of the structure of aged sodium borophosphate glasses

    The structure of aged melt-quenched sodium borophosphate glasses of composition (P2O5)40(B2O3)x(Na2O)60-x (with x in the range 10-40) has been studied by high-energy X-ray diffraction (HEXRD), 31P and 11B magic angle spinning (MAS) NMR. Similar to the fresh samples, both P-O-P and P-O-B linkages are found to be present in these glasses. All three techniques show that the cross-linking between borate and phosphate units increases with boron oxide content. Distinctively upon aging, the glass is found to hydrolyze causing the network to degrade. At the same time, crystalline phases are now also observed. XRD and DTA show that the samples have a higher tendency towards crystallization with increasing boron oxide content upon exposed to moisture. 31P and 11B MAS NMR results are in agreement with these findings. TGA data show that samples with higher boron oxide content take up more moisture upon aging, suggesting that crystallization may be associated with glass hydrolysis. HEXRD results also suggest that sodium ions are preferentially associated with borate units with increasing boron oxide content

  10. Trimethylphosphine-Assisted Surface Fingerprinting of Metal Oxide Nanoparticle by (31)P Solid-State NMR: A Zinc Oxide Case Study.

    Peng, Yung-Kang; Ye, Lin; Qu, Jin; Zhang, Li; Fu, Yingyi; Teixeira, Ivo F; McPherson, Ian James; He, Heyong; Tsang, Shik Chi Edman

    2016-02-24

    Nano metal oxides are becoming widely used in industrial, commercial and personal products (semiconductors, optics, solar cells, catalysts, paints, cosmetics, sun-cream lotions, etc.). However, the relationship of surface features (exposed planes, defects and chemical functionalities) with physiochemical properties is not well studied primarily due to lack of a simple technique for their characterization. In this study, solid state (31)P MAS NMR is used to map surfaces on various ZnO samples with the assistance of trimethylphosphine (TMP) as a chemical probe. As similar to XRD giving structural information on a crystal, it is demonstrated that this new surface-fingerprint technique not only provides qualitative (chemical shift) but also quantitative (peak intensity) information on the concentration and distribution of cations and anions, oxygen vacancies and hydroxyl groups on various facets from a single deconvoluted (31)P NMR spectrum. On the basis of this technique, a new mechanism for photocatalytic •OH radical generation from direct surface-OH oxidation is revealed, which has important implications regarding the safety of using nano oxides in personal care products. PMID:26812527

  11. Bioenergetics of the calf muscle in Friedreich ataxia patients measured by 31P-MRS before and after treatment with recombinant human erythropoietin.

    Wolfgang Nachbauer

    Full Text Available Friedreich ataxia (FRDA is caused by a GAA repeat expansion in the FXN gene leading to reduced expression of the mitochondrial protein frataxin. Recombinant human erythropoietin (rhuEPO is suggested to increase frataxin levels, alter mitochondrial function and improve clinical scores in FRDA patients. Aim of the present pilot study was to investigate mitochondrial metabolism of skeletal muscle tissue in FRDA patients and examine effects of rhuEPO administration by phosphorus 31 magnetic resonance spectroscopy (31P MRS. Seven genetically confirmed FRDA patients underwent 31P MRS of the calf muscles using a rest-exercise-recovery protocol before and after receiving 3000 IU of rhuEPO for eight weeks. FRDA patients showed more rapid phosphocreatine (PCr depletion and increased accumulation of inorganic phosphate (Pi during incremental exercise as compared to controls. After maximal exhaustive exercise prolonged regeneration of PCR and slowed decline in Pi can be seen in FRDA. PCr regeneration as hallmark of mitochondrial ATP production revealed correlation to activity of complex II/III of the respiratory chain and to demographic values. PCr and Pi kinetics were not influenced by rhuEPO administration. Our results confirm mitochondrial dysfunction and exercise intolerance due to impaired oxidative phosphorylation in skeletal muscle tissue of FRDA patients. MRS did not show improved mitochondrial bioenergetics after eight weeks of rhuEPO exposition in skeletal muscle tissue of FRDA patients.EU Clinical Trials Register2008-000040-13.

  12. Comparison of the clinical state and its changes in patients with Duchenne and Becker muscular dystrophy with results of in vivo 31P magnetic resonance spectroscopy

    A total of 14 boys with the Duchenne and Becker forms of muscular dystrophy (DMD, BMD) were examined using 31P magnetic resonance (MR) spectroscopy; 12 boys were examined repeatedly. The results were correlated with clinical findings (including those of genetic tests) and with data obtained from examinations of an age-matched control group. Evaluation of results using principal component analysis revealed maximum variability in the following ratios: phosphocreatine/inorganic phosphate (PCr/Pi), phosphocreatine/phosphodiesters (PCr/PDe) and phosphocreatine/phosphomonoesters (PCr/PMe). A decrease in PCr/Pi correlates with weakness of the hip girdle and of the lower part of the shoulder girdle in DMD/BMD patients. The values of all ratios in the group of patients with the DMD phenotype differ significantly from results obtained in the group with the BMD phenotype. Continuous follow-up of patients using 31P MR spectroscopy revealed a marked decrease in PCr/Pi in DMD/BMD patients at an age that could be expected in subjects with a typical clinical course of DMD/BMD. An attempt to manage a concomitant disease with prednisone and carnitene was followed by an increase in PCr/Pi in 3 cases. A rise in the PCr/Pi ratio signalled clinical improvement in the patients. A decrease in PCr/Pi was found after controlled physical training, a finding consistent with data obtained from clinical observations describing an adverse effect of physical stress on the dystrophic process. (orig.)

  13. On the use of 31P NMR for the quantification of hydrosoluble phosphorus-containing compounds in coral host tissues and cultured zooxanthellae

    Godinot, Claire; Gaysinski, Marc; Thomas, Olivier P.; Ferrier-Pagès, Christine; Grover, Renaud

    2016-02-01

    31P Nuclear Magnetic Resonance (NMR) was assessed to investigate the phosphorus-containing compounds present in the tissues of the scleractinian coral Stylophora pistillata as well as of cultured zooxanthellae (CZ). Results showed that phosphorus-containing compounds observed in CZ were mainly phosphate and phosphate esters. Phosphate accounted for 19 ± 2% of the total phosphorus compounds observed in CZ maintained under low P-levels (0.02 μM). Adding 5 mM of dissolved inorganic phosphorus (KH2PO4) to the CZ culture medium led to a 3.1-fold increase in intracellular phosphate, while adding 5 mM of dissolved organic phosphorus led to a reduction in the concentration of phosphorus compounds, including a 2.5-fold intracellular phosphate decrease. In sharp contrast to zooxanthellae, the host mainly contained phosphonates, and to a lesser extent, phosphate esters and phosphate. Two-months of host starvation decreased the phosphate content by 2.4 fold, while bleaching of fed corals did not modify this content. Based on 31P NMR analyses, this study highlights the importance of phosphonates in the composition of coral host tissues, and illustrates the impact of phosphorus availability on the phosphorus composition of host tissues and CZ, both through feeding of the host and inorganic phosphorus enrichment of the CZ.

  14. Post mortem energy metabolism and meat quality of porcine M. longissimus dorsi as influenced by stunning method - A (31)P NMR spectroscopic study.

    Bertram, Hanne Christine; Stødkilde-Jørgensen, Hans; Karlsson, Anders Hans; Andersen, Henrik Jørgen

    2002-09-01

    Post mortem changes in phosphorus metabolites and pH were studied in M. longissimus dorsi from pigs (n=10) stunned either by CO(2) (n=3), electrical (n=2), captive bolt pistol (n=2) or by anesthesia (ketamine) (n=3). (31)P-NMR spectroscopy revealed significant effects of stunning method on changes of the various phosphorus metabolites in the muscle post mortem, with the effect being most pronounced on the degradation of phosphocreatine (PCr). Moreover, the four stunning methods gave rise to large differences in the progress of pH as determined by (31)P-NMR spectroscopy. Using anesthesia as the reference showed that the captive bolt pistol caused the highest rates of post mortem degradation of phosphorus metabolites, electrical stunning intermediate, and CO(2)-stunning causing the lowest post mortem degradation rates, even though CO(2)-stunning also was associated with higher post mortem degradation rates compared with anesthesia. Finally, it was demonstrated that the water-holding capacity (WHC) of the meat was affected by the applied stunning method, as CO(2)-stunning, electrical stunning and captive bolt pistol resulted in mean drip losses of 6.4, 8.3 and 8.6%, respectively (P=0.02). The result displays the significance of induction and progress in post mortem changes on WHC in meat. PMID:22061199

  15. Measurement of delta(1)J((199)Hg, (31)P) in [HgPCy3(OAc)2]2 and relativistic ZORA DFT investigations of mercury-phosphorus coupling tensors.

    Bryce, David L; Courchesne, Noémie Manuelle Dorval; Perras, Frédéric A

    2009-12-01

    Using 31P solid-state NMR spectroscopy, anisotropy in the indirect 199Hg-31P spin-spin coupling tensor (DeltaJ) for powdered [HgPCy3(OAc)2]2 (1) has been measured as 4700 +/- 300 Hz. Zeroth-order regular approximation (ZORA) density functional theory (DFT) calculations, including scalar and spin-orbit relativistic effects, performed on 1 and a series of other related compounds show that DeltaJ(199Hg, (31)P) arises entirely from the ZORA Fermi-contact-spin-dipolar cross term. The calculations validate assumptions made in the spectral analysis of 1 and in previous determinations of DeltaJ in powder samples, namely that J is axially symmetric and shares its principal axis system with the direct dipolar coupling tensor (D). Agreement between experiment and theory for various 199Hg, 31P spin-spin coupling anisotropies is reasonable; however, experimental values of 1J(199Hg, 31P)(iso) are significantly underestimated by the calculations. The most important improvements in the agreement were obtained as a result of including more of the crystal lattice in the model used for the calculations, e.g., a change of 43% was noted for 1J(199Hg, 31P)(iso) in [HgPPh3(NO3)2]2 depending on whether the two or three nearest nitrate ions are included in the model. Finally, we have written a computer program to simulate the effects of non-axial symmetry in J and of non-coincidence of the J and D on powder NMR spectra. Simulations clearly show that both of these effects have a pronounced impact on the 31P NMR spectrum of 199Hg-31P spin pairs, suggesting that the effects should be observable experimentally if a suitable compound can be identified. PMID:20056396

  16. 1-Benzyl-1H-benzotriazole 3-oxide–1-hydroxy-1H-benzotriazole (1/1

    P. Selvarathy Grace

    2012-08-01

    Full Text Available In the title compound, C6H5N3O·C13H11N3O, the benzotriazole ring system in the 1-benzyl-1H-benzotriazole 3-oxide (A molecule is close to being planar (r.m.s. deviation = 0.011 Å; its mean plane forms a dihedral angle of 67.56 (7° with that of the attached phenyl ring. The benzotriazole ring system in the 1-hydroxybenzotriazole (B molecule is also close to being planar (r.m.s. deviation = 0.010 Å. In the crystal, weak C—H...O and C—H...π interactions are present. The A and B molecules are linked by an O—H...N hydrogen bond.

  17. 1H NMR spectroscopic identification of a glue sniffing biomarker.

    Kwon, Bobae; Kim, Siwon; Kim, Sosun; Lee, Dong-Kye; Park, Yu-Jin; Kim, Myung-Duck; Lee, Jae-Shin; Kim, Suhkmann

    2011-06-15

    Organic solvent abuse typically involves sniffing organic solvents to experience the mind-altering conditions they induce. In Republic of Korea, organic solvent abuse is a serious social problem, especially among teenagers. Several studies have addressed the effects of organic solvent abuse on mind and body, but there are no simple methods by which such abuse can be positively identified. In this report, we describe a method for analyzing toluene metabolites (toluene is the main ingredient of glue) in glue-sniffers' urine using (1)H NMR spectroscopy. Toluene is a commonly used solvent in the rubber, paint, plastics, leather, printing, and chemical industries. Inhaled toluene is metabolized to hippuric acid in the liver and excreted in the urine. Hippuric acid is known as a good biomarker for biological monitoring of toluene exposure. We have scanned hippuric acid and other toluene metabolites by NMR spectroscopy and performed statistical multivariate analysis of the data. Based on this analysis, we sought to determine parameters by which glue-sniffing (toluene inhalation) behavior may be verified. We also demonstrate the use of a pattern recognition method for accurate and efficient analysis of NMR data. In comparison to conventional methods, such as mass spectroscopy coupled with liquid chromatography or gas chromatography, nuclear magnetic resonance spectroscopy has several advantages, including simple sample preparation, non-destructive sampling, accuracy, short acquisition time, and reproducibility in the determination of urinary hippuric acid. PMID:21316881

  18. 1H homonuclear editing of rat brain using semiselective pulses

    The authors have used a semiselective Hahn spin-echo sequence of the form (1331)-tau-(2662)-tau-AQ, delivered by a surface coil to obtain high-resolution 1H NMR spectra from the brains of intact dead rats. This sequence gave suppression of the tissue water resonance by a factor of 80,000 when tau = 68 ms. Delivery of a frequency-selective Dante pulse train to the alpha-CH resonance of lactate at 4.11 ppm, simultaneously with the 2662 refocusing pulse, altered the j-modulation in the spin-coupled beta-CH3 protons. Subtraction of this spectrum from one in which the Dante was ineffective gave an edited spectrum containing only the beta-CH3 resonance of lactate at 1.31 ppm. When the position of the Dante was shifted to 3.78 ppm to selectively invert the alpha-CH protons of alanine, an edited spectrum of alanine was obtained

  19. The effect of gingko biloba extract on energy metabolic status in C3H mouse fibrosarcoma: evaluated by in vivo 31P magnetic resonance spectroscopy

    Gingko biloba extract (GBE), a natural product extracted from Gingko leaves, is known to increase the radiosensitivity of tumors. This radiosensitization probably arises from the increase in the peripheral blood flow by decreasing the blood viscosity and relaxing the vasospasm. The influence of a GBE on the metabolic status in fibrosarcoma II (FSall) of a C3H mouse was investigated using 31P magnetic resonance spectroscopy (MRS). Eighteen C3H mice with fibrosarcoma II (from 100 mm3 to 130 mm3) were prepared for this experiment. The mice were divided into 2 groups; one (9 mice) without a priming dose, and the other (9 mice) with a priming dose of GBE. The GBE priming dose (100 mg/kg) was administered by an intraperitoneal (i.p.) injection 24 hours prior to the measurement. First 31P MRS spectra were measured in the mice from each group as a baseline and test dose of GBE (100 mg/kg) was then administered to each group. One hour later, the 31P MRS spectra were measured again to evaluate the change in the energy metabolic status. In the group without the priming dose, the mean pH, PCr/Pi, PME/ATP, Pi/ATP, PCr/(Pi + PME) values 1 hour after the test dose were not changed significantly compared to the values at the baseline. However, in the group with the priming dose, the mean PCr/Pi, Pi/ATP, PCr/(Pi + PME) values 1 hour after the test dose changed from the baseline values of 0.49, 0.77, 0.17 to 0.74, 0.57, 0.28 respectively. According to the paired t-test, the differences were statistically significant. The above findings suggest that the metabolic status is significantly improved after administering GBE if the priming dose is given 24 hours earlier. This shows that the radiosensitizing effect of GBE is based on the increase of tumor blood flow and the improvement in the metabolic status

  20. The effect of gingko biloba extract on energy metabolic status in C3H mouse fibrosarcoma: evaluated by in vivo {sup 31}P magnetic resonance spectroscopy

    Ha, Sung Whan; Kim, Won Dong; Ahn, Yong Chan; Park, Charn Il [Seoul National University, College of Medicine, Seoul (Korea, Republic of); Lim, Tae Hwan; Lee, Tae Kuen [Ulsan University, Seoul (Korea, Republic of)

    2002-06-15

    Gingko biloba extract (GBE), a natural product extracted from Gingko leaves, is known to increase the radiosensitivity of tumors. This radiosensitization probably arises from the increase in the peripheral blood flow by decreasing the blood viscosity and relaxing the vasospasm. The influence of a GBE on the metabolic status in fibrosarcoma II (FSall) of a C3H mouse was investigated using {sup 31}P magnetic resonance spectroscopy (MRS). Eighteen C3H mice with fibrosarcoma II (from 100 mm{sup 3} to 130 mm{sup 3}) were prepared for this experiment. The mice were divided into 2 groups; one (9 mice) without a priming dose, and the other (9 mice) with a priming dose of GBE. The GBE priming dose (100 mg/kg) was administered by an intraperitoneal (i.p.) injection 24 hours prior to the measurement. First {sup 31}P MRS spectra were measured in the mice from each group as a baseline and test dose of GBE (100 mg/kg) was then administered to each group. One hour later, the {sup 31}P MRS spectra were measured again to evaluate the change in the energy metabolic status. In the group without the priming dose, the mean pH, PCr/Pi, PME/ATP, Pi/ATP, PCr/(Pi + PME) values 1 hour after the test dose were not changed significantly compared to the values at the baseline. However, in the group with the priming dose, the mean PCr/Pi, Pi/ATP, PCr/(Pi + PME) values 1 hour after the test dose changed from the baseline values of 0.49, 0.77, 0.17 to 0.74, 0.57, 0.28 respectively. According to the paired t-test, the differences were statistically significant. The above findings suggest that the metabolic status is significantly improved after administering GBE if the priming dose is given 24 hours earlier. This shows that the radiosensitizing effect of GBE is based on the increase of tumor blood flow and the improvement in the metabolic status.

  1. Importance of the 31-p-nmr-spectroscopy for prediction and early detection of coronary heart disease in patients with diabetes mellitus type I

    Steinboeck, P

    2001-01-01

    Microvascular abnormalities and dysfunction via thickening of the basement membrane are known to occur in diabetic patients. Myocardial high energy phosphates have been shown to be reduced by ischemia and alterations of the cardiac metabolism are the primary consequence of myocardial ischemia. The present study involved 30 male patients with diabetes mellitus type I and 36 healthy male volunteers as age-matched controls. Phosphorus-31-P-nuclear-magnetic-resonance-spectroscopic-imaging of the heart was performed in all subjects using a 1.5 Tesla whole-body-magnetic-resonance-scanner. The ratios of phosphocreatinine (PCr) to adenosine-triphosphate (ATP) were calculated. Moreover, echocardiographic evaluation and stress tests were performed in all individuals. The myocardium of patients with diabetes mellitus type I showed significantly decreased ratios of PCr/ATP compared with healthy controls. This study demonstrates for the first time a decreased ratio of PCr/ATP in the myocardium of patients with diabetes me...

  2. Molecular Structure of P_xSe_1-x Glasses from Raman Scattering, ^31P NMR and T-modulated DSC

    Georgiev, D. G.; Mitkova, M.; Boolchand, P.; Brunklaus, G.; Eckert, H.; Micoulaut, M.

    2000-03-01

    Our spectroscopic results show that the backbone of these glasses is composed of Se_n chains/rings, pyramidal P(Se_1/2)3 units, quasi-tetrahedral Se=P(Se_1/2)3 units and ethylene-like P_2(Se_1/2)4 units at low P-content (x0.47), P_4Se3 monomers decouple from the backbone. The concentrations of the various building blocks established from Raman Scattering and ^31P NMR are found to correlate well with each other. T_g(x) trend is established from the reversing heat flow in MDSC experiments. When compared with the prediction of a stochastic model, the T_g(x) trend shows that only at low x (x<0.12) can the glasses really be described as random networks. At higher x, structural correlations emerge between building blocks defining medium range structure.

  3. Phosphorolytic activity of Escherichia coli glycyl-tRNA synthetase towards its cognate aminoacyl adenylate detected by 31P-NMR spectroscopy and thin-layer chromatography

    Led, Jens Jørgen; Switon, Werner K.; Jensen, Kaj Frank

    1983-01-01

    The catalytic activity of highly purified Escherichia coli glycyl-tRNA synthetase has been studied by 31P-NMR spectroscopy and thin-layer chromatography on poly(ethyleneimine)-cellulose. It was found that this synthetase, besides the activation of its cognate amino acid and the syntheses of...... adenosine(5')tetraphospho(5')adenosine (Ap4A) and adenosine(5')triphospho(5')adenosine (Ap3A), also catalyzes the formation of ADP from inorganic phosphate and the enzyme-bound glycyl adenylate. Accordingly it was shown that E. coli glycyl-tRNA synthetase, in the presence of inorganic phosphate, glycine...... remaining catalytic activities of aminoacyl-tRNA synthetases is discussed, as well as the biological significance of the reaction....

  4. 31P NMR analysis of intracellular pH of Swiss Mouse 3T3 cells: effects of extracellular Na+ and K+ and mitogenic stimulation.

    Civan, M M; Williams, S R; Gadian, D G; Rozengurt, E

    1986-01-01

    Swiss mouse 3T3 cells grown on microcarrier beads were superfused with electrolyte solution during continuous NMR analysis. Conventional 31P and 19F probes of intracellular pH (pHc) were found to be impracticable. Cells were therefore superfused with 1 to 4 mM 2-deoxyglucose, producing a large intracellular, pH-sensitive signal of 2-deoxyglucose phosphate (2DGP). The intracellular incorporation of 2DGP inhibited the Embden-Meyerhof pathway. However, intracellular ATP was at least in part retained and the cellular responsivity to changes in extracellular ionic composition and to the application of growth factors proved intact. Transient replacement of external Na+ with choline or K+ reversibly acidified the intracellular fluids. Quiescent cells and mitogenically stimulated cells displayed the same dependence of shifts in pHc on external Na+ concentration (CoNa). PHc also depended on intracellular Na+ concentration (CcNa). Increasing ccNa by withdrawing external K+ (thereby inhibiting the Na,K-pump) caused reversible intracellular acidification; subsequently reducing CoNa produced a larger acid shift in pHc than with external K+ present. Comparison of separate preparations indicated that pHc was higher in stimulated than in quiescent cells. Transient administration of mitogens also reversibly alkalinized quiescent cells studied continuously. This study documents the feasibility of monitoring pHc of Swiss mouse 3T3 cells using 31P NMR analysis of 2DGP. The results support the concept of a Na/H antiport operative in these cells, both in quiescence and after mitogenic stimulation. The data document by an independent technique that cytoplasmic alkalinization is an early event in mitogenesis, and that full activity of the Embden-Meyerhof pathway is not required for the expression of this event. PMID:3543375

  5. 31P-MR spectroscopy of the brain in patients with anorexia nervosa: characteristic differences in the spectra between patients and healthy control subjects

    Purpose: To investigate whether 31P-MR spectroscopy can detect reduced concentrations of high-energy phosphates, like PCr and NTP, caused by decreased metabolic activity in the brain of patients with anorexia nervosa (AN) and, furthermore, whether any impairment of the cerebral membrane metabolism can be derived from the spectra. Material and Methods: 10 female patients, age range 12 - 20 years and mean BMI (body mass index) of 14.8 ± 1.6 kg/m2, with clinically diagnosed AN (ICD-10, F50.0) and 10 healthy control subjects, age range 12 - 21 years and mean BMI 19.0 ± 2.1 kg/m2, without nutritional disturbances: were investigated. 31P-MR spectroscopy was performed with a 1.5 T MRI unit using single volume selection in the frontal/prefrontal region of brain. Relative metabolic concentrations were quantified by normalizing the peak areas of the metabolites with the total area of the complete phosphorous spectrum, Ptot, as well as with the peak area of β;-NTP. Results: Significant differences between the two groups were observed for the metabolic ratios PDE/Ptot, PDE/β;-NTP and α-NTP/Ptot which were lower in the patient group except for α-NTP/Ptot. These ratios also revealed a statistically significant correlation with the BMI (rPDE/Ptot = 0.747, rPDE/β;-NTP = 0.57, rα-NTP/Ptot = -0.56; p ≤ 0.1). Reduced relative concentrations of PCr/Ptot, β;-NTP/Ptot or Pi/Ptot were not encountered. Conclusion: The lowered PDE/Ptot ratio for patients with AN and its correlation with BMI suggests that decreased BMI induces compositional changes of the phospholipids in the brain, which decrease the fraction of mobile phospholipids. (orig.)

  6. Effects of Coenzyme Q10 on Skeletal Muscle Oxidative Metabolism in Statin Users Assessed Using 31P Magnetic Resonance Spectroscopy: a Randomized Controlled Study

    Buettner, Catherine; Greenman, Robert L.; Ngo, Long H.; Wu, Jim S.

    2016-01-01

    Objectives Statins partially block the production of coenzyme Q10 (CoQ10), an essential component for mitochondrial function. Reduced skeletal muscle mitochondrial oxidative capacity has been proposed to be a cause of statin myalgia and can be measured using 31phosphorus magnetic resonance spectroscopy (31P-MRS). The purpose of this study is to assess the effect of CoQ10 oral supplementation on mitochondrial function in statin users using 31P-MRS. Design/Setting In this randomized, double-blind, placebo-controlled pilot study, 21 adults aged 47–73 were randomized to statin+placebo (n=9) or statin+CoQ10 (n=12). Phosphocreatine (PCr) recovery kinetics of calf muscles were assessed at baseline (off statin and CoQ10) and 4 weeks after randomization to either statin+CoQ10 or statin+placebo. Results Baseline and post-treatment PCr recovery kinetics were assessed for 19 participants. After 4 weeks of statin+ CoQ10 or statin+placebo, the overall relative percentage change (100*(baseline−follow up)/baseline) in PCr recovery time was −15.1% compared with baseline among all participants, (p-value=0.258). Participants randomized to statin+placebo (n=9) had a relative percentage change in PCr recovery time of −18.9%, compared to −7.7% among participants (n=10) receiving statin+CoQ10 (p-value=0.448). Conclusions In this pilot study, there was no significant change in mitochondrial function in patients receiving 4 weeks of statin+CoQ10 oral therapy when compared to patients on statin+placebo.

  7. High-energy phosphate metabolism during incremental calf exercise in humans measured by 31 phosphorus magnetic resonance spectroscopy (31P MRS).

    Schocke, Michael F H; Esterhammer, Regina; Kammerlander, Christian; Rass, Anton; Kremser, Christian; Fraedrich, Gustav; Jaschke, Werner R; Greiner, Andreas

    2004-01-01

    Several previous 31 phosphorus magnetic resonance spectroscopy ((31)P MRS) studies performing incremental or progressive muscle exercises have observed that a decrease in pH is accompanied with an acceleration in phosphocreatine (PCr) hydrolysis. The purpose of this study was to investigate the relationship between PCr breakdown and pH during isotonic, exhaustive, incremental plantar flexion exercises. We included eight healthy, male volunteers into this study. Using a 1.5 Tesla MR scanner and a self-built exercise bench, we performed serial free induction decay (FID) (31)P MRS measurements with a time resolution of 1 min at rest, isotonic calf muscle exercise, and recovery. The exercise protocol consisted of 5-min intervals with 4.5, 6, 7.5, and 9 W workload followed by 9-min recovery. Changes in PCr and inorganic phosphate (Pi) were determined as percent changes in comparison to the baseline. In addition, pH values were calculated. This study obtained significant decreases in PCr corresponding to the gradual increases in workload. In each workload level that was succeeded by all volunteers, PCr hydrolysis passed into a steady state. After an early biphasic response, we detected a significant decrease in pH from the first to the second minute of the 6-W workload level followed by a further continuous decrease in pH up to the second minute of the recovery phase. The decrease in pH was not accompanied by acceleration in PCr hydrolysis. In conclusion, this study shows that PCr hydrolysis during incremental plantar flexion exercises passes into a steady state at different workload levels. The observed decrease in pH does not result in acceleration of PCr hydrolysis. PMID:14972400

  8. Structural and 31P NMR investigation of Bi(MM')2PO6 statistic solid solutions: Deconvolution of lattice constraints and cationic influences

    Two solid solutions BiMx Mg(2-x)PO6 (with M 2+=Zn or Cd) have been studied through 31P MAS NMR. The analysis has been performed on the basis of refined crystal structures through X-ray diffraction and neutron diffraction. The BiZn x Mg(2-x)PO6 does not provide direct evidence for sensitive changes in the phosphorus local symmetry. This result is in good agreement with structural data which show nearly unchanged lattices and atomic separations through the Zn2+ for Mg2+ substitution. On the other hand, the Cd2+ for Mg2+ substitution behaves differently. Indeed, up to five resonances are observed, each corresponding to one of the five first-cationic neighbour distributions, i.e. 4Mg/0Cd, 3Mg/1Cd, 2Mg/2Cd, 1Mg/3Cd and 0Mg/4Cd. Their intensities match rather well the expected weight for each configuration of the statistical Cd2+/Mg2+ mixed occupancy. The match is further improved when one takes into account the influence of the 2nd cationic sphere that is available from high-field NMR data (18.8 T). Finally, the fine examination of the chemical shift for each resonance versus x allows to de-convolute the mean Z/a 2 effective field into two sub-effects: a lattice constraint-only term and a chemical-only term whose effects are directly quantifiable. - Graphical abstract: First (CdMg)4 cationic sphere influence on the 31P NMR signal in Bi(Cd,Mg)2PO6. Display Omitted

  9. 31P-MR spectroscopy of all regions of the human heart at 1.5 T with acquisition-weighted chemical shift imaging

    Aim: Aim of this study was to show whether or not acquisition-weighted chemical shift imaging (AW-CSI) allows the determination of PCr and ATP in the lateral and posterior wall of the human heart at 1.5 T. Methods: 12 healthy volunteers were examined using a conventional chemical shift imaging (CSI) and an AW-CSI. The sequences differed only in the number of repetitions for each point in k space. A hanning function was used as filter function leading to 7 repetitions in the center of the k space and 0 in the corners. Thus, AW-CSI had the same resolution as the CSI sequence. The results for both sequences were analyzed using identically positioned voxels in the septal, anterior, lateral and posterior wall. Results: The determined averaged AW-CSI signal to noise ratios were higher for PCr by a factor of 1.3 and for ATP by 1.4 than those of CSI. The PCr/ATP ratios were higher by a factor of 1.2 - 1.3 and showed a smaller standard deviation in all locations for AW-CSI. The mean PCr/ATP ratios determined by AW-CSI of septal, lateral and posterior wall were almost identical (1.72 - 1.76), while it was higher in the anterior wall (1.9). Conclusions: The reduced contamination in AW-CSI improves the signal to noise ratio and the determination of the PCr/ATP ratio in cardiac 31P spectroscopy compared to CSI with the same resolution. The results in volunteers indicate that AW-CSI renders 31P spectroscopy of the lateral and posterior wall of the human heart feasible for patient studies at 1.5 T. (orig.)

  10. Metabolism of D-glucose in a wall-less mutant of Neurospora crassa examined by 13C and 31P nuclear magnetic resonances: effects of insulin

    13C NMR and 31P NMR have been used to investigate the metabolism of glucose by a wall-less strain of Neurospora crassa (slime), grown in a supplemented nutritionally defined medium and harvested in the early stationary stage of growth. With D-[1-13C]- or D-[6-13C]glucose as substrates, the major metabolic products identified from 13C NMR spectra were [2-13C]ethanol, [3-13C]alanine, and C1- and C6-labeled trehalose. Several observations suggested the existence of a substantial hexose monophosphate (HMP) shunt: (i) a 70% greater yield of ethanol from C6- than from C1-labeled glucose; (ii) C1-labeled glucose yielded 19% C6-labeled trehalose, while C6-labeled glucose yielded only 4% C1-labeled trehalose; (iii) a substantial transfer of 13C from C2-labeled glucose to the C2-position of ethanol. 31P NMR spectra showed millimolar levels of intracellular inorganic phosphate (Pi), phosphodiesters, and diphosphates including sugar diphosphates and polyphosphate. Addition of glucose resulted in a decrease in cytoplasmic Pi and an increase in sugar monophosphates, which continued for at least 30 min. Phosphate resonances corresponding to metabolic intermediates of both the glycolytic and HMP pathways were identified in cell extracts. Addition of insulin (100 nM) with the glucose had the following effects relative to glucose alone: (i) a 24% increase (P less than 0.01) in the rate of ethanol production; (ii) a 38% increase (P less than 0.05) in the rate of alanine production; (iii) a 27% increase (P less than 0.05) in the rate of glucose disappearance. Insulin thus increases the rates of production of ethanol and alanine in these cells, in addition to increasing production of CO2 and glycogen, as previously shown. (author)

  11. A 1H NMR study of human calcitonin in solution

    Human calcitonin (hCT) has been investigated by NMR at 400 MHz in DMSOd6 and in an 85% DMSOd6-15% 1H2O (v/v) cryoprotective mixture. All backbone and side-chain resonances have been assigned and the secondary structure has been determined in both solvents. In DMSOd6, the simultaneous presence of dαN, dNN, and some specific weak medium-range nuclear Overhauser effects, together with the amide temperature coefficients and the analysis of the NH-αCH spin-spin coupling constants, indicates that hCT is highly flexible but with three domains (comprising segments Asn3-Gly10, Gln14-Thr21, and Thr25-Ala31) in extended conformations which dynamically transform into isolated β turns in the N- and C-terminal regions and into adjacent tight turns, resembling a 310 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 β 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 β 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 α helix, postulated to be responsible for the interaction of hCT with lipids. The possible role of the cis-trans isomerism of Pro is discussed

  12. Analyzing Ph value, energy and phospholipid metabolism of various cerebral tumors and normal brain tissue with 31P magnetic resonance spectroscopy

    Wei Tan; Guangyao Wu; Junmo Sun

    2006-01-01

    BACKGROUND: 31P magnetic resonance spectroscopy (31P MRS) can be used to non-injuredly and dynamicly detect various metabolites including phosphorus in organis and reflect changes of phospholipid metabolism and energy metabolism in tissue and pH value in cells.OBJECTIVE: To observe changes of pH value, phospholipid metabolism and energy metabolism of various cerebral tumors and normal brain tissue with 31P MRS.DESIGN: Semi-quantitative contrast observation.PARTICIPANTS: A total of 44 patients with cerebral tumor diagnosed with surgery operation were selected from the Department of Magnetic Resonance, Central South Hospital, Wuhan University from September 2004 to June 2006. All the subjects had complete 31P MRS data before steroid and operation. Among them,16 patients had glioma of grade Ⅱ-Ⅲ, 12 spongioblastoma and 16 meningioma. The mean age was (45±6)years. Another 36 subjects without focus on cerebral MRI were regarded as normal group, including 19 males and 18 females, and the mean age was (41±4) years. Included subjects were consent.METHODS: Eclipse1.5T MRS (Philips Company) was used to collect wave spectrum; jMRUI(1.3) was used to analyze experimental data and calculate pH value in voxel and ratios of phosphocreatine (PCr)/inorganic phosphate (Pi), PCr/phosphodiesterase (PDE) and phosphomonoesterase (PME)/β-adenosine triphosphate (β-ATP) of various metabolites. 31P MRS results were compared with t test between tumor patients and normal subjects.MAIN OUTCOME MEASURES: Changes of phospholipid metabolism (PME/PDE), energy metabolism (PCr/ATP) and pH value of various cerebral tumors and normal brain tissues.RESULTS: A total of 44 cases with cerebral tumor and 36 normal subjects were involved in the final analysis. pH value and semi-quantitative measurements of normal brain tissues and various cerebral tumors: ① pH value at top occipital region and temple occipital region of normal brain tissue was 7.04±0.02;PCt/β-ATP was 1.51 ±0.03; PCt/Pi was 2.85

  13. Contribution to the study of the {sup 31}P, {sup 1}H spin spin coupling constant N. M. R. in three co-ordinated phosphorus compounds. Influence of the bond orientation and of the nature of the substituent around the phosphorus atom; Contribution a l'etude des constantes de couplage {sup 31}P, {sup 1}H en R.M.N. dans les composes organo-phosphores tricoordines. Influence des facteurs geometriques et de la nature des substituants au niveau du phosphore

    Robert, J.B. [Commissariat a l' Energie Atomique, Grenoble (France). Centre d' Etudes Nucleaires

    1969-07-01

    In order to investigate the influence of the configuration at the phosphorus atom and the influence of the substituents attached to the phosphorus atom on the J{sub PH} spin spin coupling constant, we have performed the NMR spectrum analysis of some three coordinated organo-phosphorus compounds. The studied coupling constants are {sup 3}J{sub PH} through P-O-C-H and P-C-C-H fragments and {sup 2}J{sub PH} through P-C-H fragment. The results clearly show that on the NMR time scale, in all the studied compounds (1,3,2-dioxaphospholanes, 1,3,2-dioxaphosphorinanes, 3-phospha-cyclopentene and 4-phosphorinanone) there is no inversion of the bonds around phosphorous. This conclusion held also for secondary phosphines. For a given geometry of the bonds joining the P and H atoms, and a given disposition of the bonds around the phosphorus atom, there is only a little influence of the nature of the substituents on the J{sub PH} spin coupling constants. The geometrical dependence of the {sup 3}J{sub PH} cannot be explained by a 'Karplus law'. There is an influence of the bond disposition around phosphorus. In the case of the {sup 2}J{sub P-C-H}, one can plot a curve {sup 2}J{sub P-C-H} = f({alpha}) (0{<=} {alpha} {<=} 180), {alpha} denote the dihedral angle of the two plane defined the first one by the P, C and H atoms, and the second one by the P-C bond together with the three-fold axis of the bond around phosphorus assuming a regular pyramidal arrangement. The function {sup 2}J{sub P-C-H} = f({alpha}) has two maxima, one for {alpha} = 0 degrees and the other for {alpha} = 180 degrees, and also a minimum for {alpha} = 110 degrees. (author) [French] Ce travail consiste en l'analyse par resonance magnetique nucleaire des constantes de couplage phosphore-proton dans des derives organo-phosphores tricoordines dans un double but: examen de la stabilite des liaisons au niveau du phosphore et etude de l'influence de la disposition des liaisons et de la nature de substituants au niveau du phosphore. Les constantes de couplage sont du type {sup 3}J{sub PH} au travers des fragments P-C-C-H et P-O-C-H, et {sup 2}J{sub PH} au travers du fragment P-CH. Les resultats montrent que, pour les temps d'observation de la RMN, la disposition des liaisons au niveau du phosphore dans l'ensemble des composes etudies (dioxaphospholanes-1,3,2, dioxaphosphorinanes-1,3,2, phosphacyclopentenes-3, phosphorinanones-4) qui portent des substituants varies au niveau du phosphore, est pyramidale et fixe. Ce resultat s'applique egalement aux phosphines secondaires. Le couplage depend tres peu des substituants fixes sur le phosphore sauf dans le cas d'un azote. Pour les couplages {sup 3}J, les resultats montrent que la dependance attendue, basee uniquement sur l'angle diedre de type ''Karplus'', ne suffit pas. La direction du doublet libre donne lieu a une variation supplementaire sur J. Dans le cas des couplages {sup 2}J{sub P-C-H} cette influence est le facteur principal, les variations de J allant de + 25 cps a -6 cps: les valeurs peuvent etre traduites par une loi J = f({alpha}) (0 {<=} {alpha} {<=} 180) {alpha} etant l'angle diedre des plans H-C-P et C-P-X, X representant la direction du doublet libre (axe ternaire de la pyramide passant par le phosphore). (auteur)

  14. Fósforo num Cambissolo cultivado com cana-de-açúcar por longo tempo: II - análise de ácidos húmicos por RMN 31P Phosphorus in an Inceptsoil under long-term sugarcane: II - humic acid analysis by NMR 31P

    Jader Galba Busato

    2005-12-01

    Full Text Available Sistemas de manejo da lavoura de cana-de-açúcar que favoreçam a matéria orgânica do solo podem aumentar o conteúdo de nutrientes disponíveis e diminuir a necessidade de aplicação de fertilizantes industriais. Apesar da importância dos componentes orgânicos no fornecimento de P, pouco se conhece sobre a sua dinâmica em ambientes tropicais. O objetivo deste trabalho foi identificar, por meio da ressonância magnética nuclear (RMN 31P, as espécies de P nos ácidos húmicos de um Cambissolo Háplico Ta eutrófico vértico, localizado no Município de Campos dos Goytacazes, norte do Estado do Rio de Janeiro, e cultivado com cana-de-açúcar com preservação do palhiço e adição de vinhaça por longo tempo. Por meio da análise de RMN 31P foi possível observar acúmulo de P orgânico em formas mais facilmente mineralizadas nas áreas com preservação de matéria orgânica, tal como P em ligações diésteres. Nas áreas de cana queimada, houve maior participação de espécies orgânicas mais estáveis, como o ortofosfato em ligações monoésteres. Os resultados da espectroscopia de RMN 31P mostram que, nas áreas com maior aporte de resíduo orgânico (i.e., cana crua e cana queimada com adição de vinhaça, os ácidos húmicos constituem uma reserva importante de P orgânico prontamente disponível. Já, nas áreas de cana queimada, o acúmulo de P orgânico recalcitrante nos ácidos húmicos indica utilização do P-lábil das substâncias húmicas como fonte importante para nutrição das plantas.Crop management systems that favor soil organic matter can improve the available nutrient content for plants and reduce the use of industrial fertilizer. Despite the importance of organic compounds as a P source, little is known about its dynamics in tropical environments. The objective of this study was to identify organic P species present in humic acids by NMR 31P analysis in a fine clay Fluventic Eutrochrepts in Campos dos

  15. Identification, synthesis and characterization of an unknown process related impurity in eslicarbazepine acetate active pharmaceutical ingredient by LC/ESI-IT/MS, 1H, 13C and 1H-1H COSY NMR

    Saji Thomas; Saroj Kumar Paul; Subhash Chandra Joshi; Vineet Kumar; Ashutosh Agarwal; Dharam Vir

    2014-01-01

    A new impurity was detected during high performance liquid chromatographic (HPLC) analysis of eslicarbazepine acetate active pharmaceutical ingredient. The structure of unknown impurity was postulated based on liquid chromatography mass spectrometry using electrospray ionization and ion trap analyzer (LC/ESI-IT/MS) analysis. Proposed structure of impurity was unambiguously confirmed by synthesis followed by characterization using 1H, 13C nuclear magnetic resonance spectrometry (NMR), 1H-1H correlation spectro-scopy (COSY) and infrared spectroscopy (IR). Based on the spectroscopic and spectrometric data, unknown impurity was characterized as 5-carbamoyl-10,11-dihydro-5H-dibenzo[b,f]azepin-10-yl propionate.

  16. Electro-gene therapy in a human oral tongue cancer cell by intratumoral injection of pcDNA3.1-p27Kip1 wt

    Supriatno Supriatno

    2007-03-01

    Full Text Available Oral tongue cancers are characterized by a high degree of local invasion and a high rate of metastases to the cervical lymph nodes. Also, treatment options for this cancer are limited. However, a new strategy for refractory cancer, gene therapy is watched with keen interest. Recently, a novel method for high-efficiency and region-controlled in vivo gene transfer was developed by combining in vivo electro-gene therapy and intratumoral plasmid DNA injection. In the present study, a nonviral gene transfer system, in vivo electrogene therapy in human oral tongue cancer cell, SP-C1 xenograft was examined. The aim of the study is to examine the efficiency of transfection of exogenous p27Kip1 gene by electroporation and the antitumor activity of p27Kip1 gene therapy in human oral tongue cancer xenografts using pcDNA3.1-p27Kip1 wild type (wt and pcDNA3.1 empty vector with the local application of electric pulses. To evaluate this in vivo gene transfer method, the enhanced green fluorescence protein (EGFP gene was transfected into xenografts by electroporation. The efficiency of transfection of exogenous p27Kip1 gene by electroporation was confirmed by Western blotting analysis. To estimate the reduction of oral tongue cancer xenografts by this method, the size of SP-C1 xenografts in nude mice after electroporation with wild type p27Kip1 gene was measured. The growth of tumors was markedly suppressed by wild type p27Kip1 gene transfection by electroporation compared with transfection of empty vector only. Moreover, histological specimens revealed apoptotic cell death was increased in wild type p27Kip1-transfected tumors than empty vector. These results suggest that it is possible to transfer wild type p27Kip1 into human oral tongue cancer xenografts using electroporation. Wild type p27Kip1 has a high-potencially to suppress the growth of tumors. Finally, combination system of pcDNA3.1-p27Kip1 wt-injected tumor and electroporationmight be used for human oral cancer.

  17. Efficient synthesis and in vitro antifungal activity of 1H-benzimidazol-1-yl acetates/propionates containing 1H-1,2,4-triazole moiety

    Pei Zhi Zhang; Shao Fang Zhou; Tian Ren Li; Lin Jiang

    2012-01-01

    A series of novel 1H-benzimidazol-1-yl acetates and 1H-benzimidazol-1-yl propionates containing 1H-1,2,4-triazole moiety were synthesized under microwave irradiation by multi-step reactions,in yields of 87-94%.Their in vitro antifungal activities against Botrytis cinerea and Sclerotinia sclerotiorum were evaluated by mycelial growth rate method.All the target compounds exhibit high activities against B.cinerea with the EC50 values of 7.96-21.74 μg/mL,higher than that of carbendazim.

  18. Importance of the 31-p-nmr-spectroscopy for prediction and early detection of coronary heart disease in patients with diabetes mellitus type I

    Microvascular abnormalities and dysfunction via thickening of the basement membrane are known to occur in diabetic patients. Myocardial high energy phosphates have been shown to be reduced by ischemia and alterations of the cardiac metabolism are the primary consequence of myocardial ischemia. The present study involved 30 male patients with diabetes mellitus type I and 36 healthy male volunteers as age-matched controls. Phosphorus-31-P-nuclear-magnetic-resonance-spectroscopic-imaging of the heart was performed in all subjects using a 1.5 Tesla whole-body-magnetic-resonance-scanner. The ratios of phosphocreatinine (PCr) to adenosine-triphosphate (ATP) were calculated. Moreover, echocardiographic evaluation and stress tests were performed in all individuals. The myocardium of patients with diabetes mellitus type I showed significantly decreased ratios of PCr/ATP compared with healthy controls. This study demonstrates for the first time a decreased ratio of PCr/ATP in the myocardium of patients with diabetes mellitus type I without a known history of coronary heart disease. (author)

  19. Thin-layer chromatography combined with MALDI-TOF-MS and 31P-NMR to study possible selective bindings of phospholipids to silica gel.

    Teuber, Kristin; Riemer, Thomas; Schiller, Jürgen

    2010-12-01

    High-performance thin-layer chromatography (HPTLC) is a highly established separation method in the field of lipid and (particularly) phospholipid (PL) research. HPTLC is not only used to identify certain lipids in a mixture but also to isolate lipids (preparative TLC). To do this, the lipids are separated and subsequently re-eluted from the silica gel. Unfortunately, it is not yet known whether all PLs are eluted to the same extent or whether some lipids bind selectively to the silica gel. It is also not known whether differences in the fatty acyl compositions affect the affinities to the stationary phase. We have tried to clarify these questions by using a readily available extract from hen egg yolk as a selected example of a lipid mixture. After separation, the complete lanes or selected spots were eluted from the silica gel and investigated by a combination of MALDI-TOF MS and (31)P NMR spectroscopy. The data obtained were compared with the composition of the total extract (without HPTLC). Although there were significant, solvent-dependent losses in the amount of each lipid, the relative composition of the mixture remained constant; there were also only very slight changes in the fatty acyl compositions of the individual PL classes. Therefore, lipid isolation by TLC may be used without any risk of major sample alterations. PMID:20694807

  20. Changes in energy metabolism following roentgen irradiation of in vivo growing Ehrlich ascites tumour cells studied by 31P magnetic resonance spectroscopy

    The energy metabolism in Ehrlich ascites tumour cells following in vivo irradiation of a dose of 5.0 Gy was studied in vitro in their ascites fluid up to 48 hours using 31P magnetic resonance spectroscopy measuring ATP, ADP and inorganic phosphate (Psub(i)). The results are also related to radiation induced changes in cell cycle composition. ATP was reduced by more than 50 per cent 20 to 24 hours after irradiation but normalized at 48 hours. ADP was reduced to about half the normal level 24 to 48 hours after irradiation. When the ATP and ADP had reduced levels, the inorganic phosphate increased correspondingly. Addition of glucose to the ascites cell suspension at the time of minimum ATP level immediately raised the ATP:Psub(i) ratio. Since the glucose concentrations in blood and in ascites fluid following irradiation were also reduced, lack of glucose for energy production might have been a major contributing factor for the reduced ATP production. (orig.)

  1. Effects of severe hypercapnia on brain cell pH and high energy phosphate levels in conscious mice by 31P NMR

    The authors have measured the effects of 10% CO2 breathing (10% CO2 in room air) on brain cell pH (pHi) and levels of phosphocreatine (PCr) and ATP in conscious mice (n=3) using 31P high resolution (8.4 tesla magnet) nuclear magnetic resonance spectroscopy (NMR) with surface coils. Brain cell pH decreased by 0.22 (+/- 0.02) pH units during the first 10 minutes of CO2, but were restored to control values during the next 10 minutes. Washout of the CO2, by substituting room air for the CO2 mixture, resulted in a 0.15 (+/- 0.02) pH unit increase over controls within 10 minutes. The ratios of PCr/ATP remained unchanged throughout the experiment. They conclude that pHi regulation is rapid and complete during severe hypercapnia and that this compensation involves movement of ions rather than intracellular protein buffering since there is hysteresis in the compensatory process (pHi is alkaline during washout). Additionally, unlike previous reports using other techniques, they find no decrease in the levels of PCr with 10% CO2 breathing

  2. Early estrogen-induced metabolic changes and their inhibition by actinomycin D and cycloheximide in human breast cancer cells: 31P and 13C NMR studies

    Metabolic changes following estrogen stimulation and the inhibition of these changes in the presence of actinomycin D and cycloheximide were monitored continuously in perfused human breast cancer T47D clone 11 cells with 31P and 13C NMR techniques. The experiments were performed by estrogen rescue of tamoxifen-treated cells. Immediately after perfusion with estrogen-containing medium, a continuous enhancement in the rates of glucose consumption, lactate production by glycolysis, and glutamate synthesis by the Krebs cycle occurred with a persistent 2-fold increase at 4 hr. Pretreatment with either actinomycin D or cycloheximide, at concentrations known to inhibit mRNA and protein synthesis, respectively, and simultaneous treatment with estrogen and each inhibitor prevented the estrogen-induced changes in glucose metabolism. This suggested that the observed estrogen stimulation required synthesis of mRNA and protein. These inhibitors also modulated several metabolic activities that were not related to estrogen stimulation. The observed changes in the in vivo kinetics of glucose metabolism may provide a means for the early detection of the response of human breast cancer cells to estrogen versus tamoxifen treatment

  3. The effect of ethanol on hydroxyl and carbonyl groups in biopolyol produced by hydrothermal liquefaction of loblolly pine: (31)P-NMR and (19)F-NMR analysis.

    Celikbag, Yusuf; Via, Brian K; Adhikari, Sushil; Buschle-Diller, Gisela; Auad, Maria L

    2016-08-01

    The goal of this study was to investigate the role of ethanol and temperature on the hydroxyl and carbonyl groups in biopolyol produced from hydrothermal liquefaction of loblolly pine (Pinus spp.) carried out at 250, 300, 350 and 390°C for 30min. Water and water/ethanol mixture (1/1, wt/wt) were used as liquefying solvent in the HTL experiments. HTL in water and water/ethanol is donated as W-HTL and W/E-HTL, respectively. It was found that 300°C and water/ethanol solvent was the optimum liquefaction temperature and solvent, yielding up to 68.1wt.% bio-oil and 2.4wt.% solid residue. (31)P-NMR analysis showed that biopolyol produced by W-HTL was rich in phenolic OH while W/E-HTL produced more aliphatic OH rich biopolyols. Moreover, biopolyols with higher hydroxyl concentration were produced by W/E-HTL. Carbonyl groups were analyzed by (19)F-NMR, which showed that ethanol reduced the concentration of carbonyl groups. PMID:27126078

  4. Neutral zinc(II) O,O-di-alkyldithiopho- sphates-variable temperature 31P NMR and quantum chemical study of the ZDDP monomer-dimer equilibrium.

    Harrison, J J; Chan, C Y; Onopchenko, A; Pradhan, A R; Petersen, M

    2008-02-01

    A full line-shape analysis of the VT 31P NMR spectra was carried out for the monomer-dimer equilibrium of neutral ZDDP. The energy surface and the energetics of the monomer-dimer equilibrium (DeltaH degrees , DeltaG degrees , Ea, DeltaH(not equal), and DeltaG(not equal)) are reported for three variants wherein the alkyl groups in the ZDDP are 2-ethylhexyl, isopropyl, and isobutyl. We explored a reaction pathway between the monomer and dimer form by means of density functional theory (DFT). The linear combination of atomic orbitals (LCAO) code DMol3 was used together with a synchronous transient method to effectively locate transition states. Vibrational eigenmodes of all intermediates were computed to capture finite temperature effects. Methyl and ethyl were considered as alkyl groups. Two novel intermediates were located-a four-membered ring and a six-membered ring intermediate along the reaction coordinate. Comparison of the experimentally derived and computed energy surfaces was carried out. PMID:18098153

  5. Cooperation and competition between adenylate kinase, nucleoside diphosphokinase, electron transport, and ATP synthase in plant mitochondria studied by 31P-nuclear magnetic resonance

    Nucleotide metabolism in potato (Solanum tuberosum) mitochondria was studied using 31P-nuclear magnetic resonance spectroscopy and the O2 electrode. Immediately following the addition of ADP, ATP synthesis exceeded the rate of oxidative phosphorylation, fueled by succinate oxidation, due to mitochondrial adenylate kinase (AK) activity two to four times the maximum activity of ATP synthase. Only when the AK reaction approached equilibrium was oxidative phosphorylation the primary mechanism for net ATP synthesis. A pool of sequestered ATP in mitochondria enabled AK and ATP synthase to convert AMP to ATP in the presence of exogenous inorganic phosphate. During this conversion, AK activity can indirectly influence rates of oxidation of both succinate and NADH via changes in mitochondrial ATP. Mitochondrial nucleoside diphosphokinase, in cooperation with ATP synthase, was found to facilitate phosphorylation of nucleoside diphosphates other than ADP at rates similar to the maximum rate of oxidative phosphorylation. These results demonstrate that plant mitochondria contain all of the machinery necessary to rapidly regenerate nucleoside triphosphates from AMP and nucleoside diphosphates made during cellular biosynthesis and that AK activity can affect both the amount of ADP available to ATP synthase and the level of ATP regulating electron transport

  6. Studies of vanadium-phosphorus-oxygen selective oxidation catalysts by sup 31 P and sup 51 V NMR spin-echo and volume susceptibility measurements

    Li, Juan.

    1991-10-01

    The purpose of this work is to characterize the vanadium-phosphorous oxide (V-P-O) catalysts for the selective oxidation of n-butane and 1-butene to maleic anhydride. The utility of solid state nuclear magnetic resonance as an analytical tool in this investigation lies in its sensitivity to the electronic environment surrounding the phosphorous and vanadium nuclei, and proximity of paramagnetic species. Spin-echo mapping NMR of {sup 31}p and {sup 51}v and volume magnetic susceptibility measurements were used as local microscopic probes of the presence of V{sup 5+}, V{sup 4+}, V{sup 3+} species in the model compounds: {beta}-VOPO{sub 4}, {beta}-VOPO{sub 4} treated with n-butane/1-butene, (VO){sub 2}P{sub 2}O{sub 7} treated with n-butane/1-butene; and industrial catalysts with P/V (phosphorus to vanadium) ratio of 0.9, 1.0 and 1.1, before and after treatment with n-butane and 1-butene. The NMR spectra provide a picture of how the oxidation states of vanadium are distributed in these catalysts. 73 refs., 32 figs., 8 tabs.

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

    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.

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

    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.

  9. Influence of muscle temperature during fatiguing work with the first dorsal interosseous muscle in man: a 31P-NMR spectroscopy study.

    Wade, A J; Broadhead, M W; Cady, E B; Llewelyn, M E; Tong, H N; Newham, D J

    2000-02-01

    Six healthy subjects rapidly lifted and lowered a small (250 g) weight with the first dorsal interosseous muscle (FDI) of one hand while the work performed was recorded continuously until fatigue (defined as losing the ability to continue lifting). Work was recorded in units of chart recorder trace displacement from baseline (centimeters) as an isotonic transducer followed the movement of the weight. In all experiments, the temperature of the hand was first adjusted by immersion in a controlled-temperature water bath. In the warmest condition, the skin surface temperature over the FDI was 30.5(0.30) degrees C [mean (SE)]. After moderate cooling, this surface temperature was 21.5(0.16) degrees C. Cooling significantly reduced the time taken to reach fatigue and more than halved the work capacity. An intermediate degree of cooling was also used in four subjects, showing that most of the effects seen were changing incrementally. Before work, and at fatigue, intracellular metabolic conditions in the FDI were studied by phosphorus nuclear magnetic resonance (31P-NMR) spectroscopy, with occlusion of the blood flow maintained during measurements. The mean intracellular pH of the FDI was also calculated. The changes observed were all consistent with the fact that intense work requires energy which must be derived largely from intracellular stores of phosphocreatine and glycogen. Less work made less demand upon reserves, and created lower concentrations of waste products and by-products. The observations did not, however, allow us to explain why fatigue occurred at a particular point or why work capacity was reduced by cooling. PMID:10638378

  10. Radiotherapeutic response of Ehrlich Ascites tumor cells perfused in agarose gel threads and implanted in mice. A 31P MR spectroscopy study

    Aim: In order to obtain better understanding of radiation-induced alterations in intracellular metabolism, a dynamic and noninvasive experimental model system is required. A serial study in cultured tumor cell line followed by verification in the in vivo samples may be of considerable value for non-invasive prediction and/or detection of tumor response to therapy. The present study was undertaken to evaluate the radiation response of perfused Ehrlich ascites tumors cells (EATC) immobilized in agarose gel matrix to that observed in mouse bearing EATC tumor, in order to identify biomarkers of radiation response. Materials and Methods: Perfused EAT cells, entrapped in agarose gel threads were irradiated in the perfusion assembly outside the magnet with fast electrons (6 Gy, 1 Gy/min) using 30 MeV Betatron. Solid EATC tumors implanted subcutaneously onto right hand limb of Swiss-albino strain 'A' mice, were focally irradiated using 60Co teletherapy (10 Gy, 0.4 Gy/min). Metabolites changes were monitored by 31P MR spectroscopic techniques. Results: A post-irradiation decrease in the levels of ATP and ADP along with an increase in inorganic phosphate and glycerophosphocholine levels was observed. The ratios of β-phosphate of ATP to inorganic phosphate (β-ATP-Pi), and phosphocholine to glycerophosphocholine (PC/GPC), declined during 1-5 hours following irradiation, in perfused EAT cells and in the solid tumors implanted in mice. Conclusion: Perfused cells could be used as a simple model of tumor for prediction of clinical radiotherapeutic response. The present study demonstrates that radiation damage may be occurring both at the DNA protein as well as the membrane lipid levels. Therefore, the bioenergetics and phospholipid profiles of tumor cells could be used as complimentary, reliable and sensitive indirect indicators for devising predictive assays for assessment and monitoring of radiation response, which will also facilitate the individualization and optimization of

  11. Phosphorus transformation in poultry litter and litter-treated Oxisol of Brazil assessed by 31P-NMR and wet chemical fractionation

    César Roriz de Souza

    2012-11-01

    Full Text Available Large quantities of poultry litter are being produced in Brazil, which contain appreciable amounts of phosphorus (P that could be of environmental concern. To assess the immediate environmental threat, five poultry litters composed of diverse bedding material were incubated for 43 days under greenhouse conditions. The litters consisted of: coffee bean husk (CH; wood chips (WC; rice husk (RH; ground corn cobs (CC and ground napier grass (NG (Pennisetum purpureum Schum., in which the change in forms of soluble P was evaluated using 31P NMR spectroscopy. On average, 80.2 and 19.8 % of the total P in the extract, respectively, accounted for the inorganic and organic forms before incubation and 48 % of the organic P was mineralized to inorganic P in 43 days of incubation. Wide variation in the organic P mineralization rate (from 82 % -WC to 4 % - NG was observed among litters. Inorganic orthophosphate (99.9 % and pyrophosphate (0.1 % were the only inorganic P forms, whereas the organic P forms orthophosphate monoesters (76.3 % and diester (23.7 % were detected. Diester P compounds were mineralized almost completely in all litters, except in the CH litter, within the incubation period. Pyrophosphates contributed with less than 0.5% and remained unaltered during the incubation period. Wood-chip litter had a higher organic P (40 % content and a higher diester: monoester ratio; it was therefore mineralized rapidly, within the first 15 days, achieving steady state by the 29th day. Distinct mineralization patterns were observed in the litter when incubated with a clayey Oxisol. The substantial decrease observed in the organic P fraction (Po of the litter types followed the order: CH (45 % > CC (25 % > RH (13 % ≈ NG (12 % > WC (5 %, whereas the Pi fraction increased. Incubation of RH litter in soil slowed down the mineralization of organic P.

  12. Characterization of soil phosphorus in a fire-affected forest Cambisol by chemical extractions and (31)P-NMR spectroscopy analysis.

    Turrion, María-Belén; Lafuente, Francisco; Aroca, María-José; López, Olga; Mulas, Rafael; Ruipérez, Cesar

    2010-07-15

    This study was conducted to investigate the long-term effects of fire on soil phosphorus (P) and to determine the efficiency of different procedures in extracting soil P forms. Different P forms were determined: labile forms (Olsen-P, Bray-P, and P extracted by anion exchange membranes: AEM-P); moderately labile inorganic and organic P, obtained by NaOH-EDTA extraction after removing the AEM-P fraction; and total organic and inorganic soil P. (31)P-NMR spectroscopy was used to characterize the structure of alkali-soluble P forms (orthophosphate, monoester, pyrophosphate, and DNA). The studied area was a Pinus pinaster forest located at Arenas de San Pedro (southern Avila, Spain). The soils were Dystric Cambisols over granites. Soil samples were collected at 0-2 cm, 2-5 cm, and 10-15 cm depths, two years after a fire in the burned area and in an adjacent unburned forest area. Fire increased the total N, organic C, total P, and organic and inorganic P content in the surface soil layer. In burned soil, the P extracted by the sequential procedure (AEM and NaOH+EDTA) was about 95% of the total P. Bray extraction revealed a fire-induced increase in the sorption surfaces. Analysis by chemical methods overestimated the organic P fraction in the EDTA-NaOH extract in comparison with the determination by ignition procedure. This overestimation was more important in the burned than unburned soil samples, probably due to humification promoted by burning, which increased P sorption by soil particles. The fire-induced changes on the structure of alkali-soluble P were an increase in orthophosphate-P and a decrease in monoester-P and DNA-P. PMID:20452650

  13. Therapeutic effect of 15-deoxyspergualin on acute graft rejection detected by 31P nuclear magnetic resonance spectrography, and its effect on rat heart transplantation

    We investigated the effect of 15-deoxyspergualin (DSG) on graft rejection, starting administration at the onset of rejection and on the induction of immunologic unresponsiveness. Hearts from WKAH rats were transplanted into the neck of ACI rats. The energy metabolism of the grafted hearts was followed by 31P nuclear magnetic resonance spectroscopy. The day that energy metabolism started to fall was defined as the onset of rejection, and intraperitoneal administration of DSG was initiated at 5 mg/kg/day for 15 days from this day. The grafted heart arrested in 2 of 10 rats 9 and 11 days after transplantation, respectively, but the remaining 8 recovered from rejection and 5 of them showed evidence of immunologic unresponsiveness. Of 10 rats treated with DSG from the day of transplantation, only 1 rat showed evidence of unresponsiveness. The initiation of DSG treatment from the onset of rejection resulted in a higher percentage of induction of unresponsiveness. Therefore, DSG was considered to specifically inhibit lymphocyte clone expansion at the onset of rejection. Spleen cells obtained from recipients 7-10 days after the end of DSG treatment were administered to syngeneic ACI rats grafted with WKAH hearts. Graft survival was significantly prolonged, but long-term unresponsiveness could not be transferred. However, immunologic unresponsiveness could be adoptively transferred in 3 of 5 rats receiving spleen cells from syngeneic rats that had recovered from rejection after DSG treatment and had acquired long-term unresponsiveness. These results suggest that suppressor cells are resistant to DSG and are spared and participate in the maintenance of immunologic unresponsiveness

  14. 31P NMR saturation-transfer measurements in Saccharomyces cerevisiae: characterization of phosphate exchange reactions by iodoacetate and antimycin A inhibition

    31P nuclear magnetic resonance (NMR) saturation-transfer (ST) techniques have been used to measure steady-state flows through phosphate-adenosine 5'-triphosphate (ATP) exchange reactions in glucose-grown derepressed yeast. The results have revealed that the reactions catalyzed by glyceraldehyde-3-phosphate dehydrogenase/phosphoglycerate kinase (GAPDH/PGK) and by the mitochondrial ATPase contribute to the observed ST. Contributions from these reactions were evaluated by performing ST studies under various metabolic conditions in the presence and absence of either iodoacetate, a specific inhibitor of GAPDH, or the respiratory chain inhibitor antimycin A. Intracellular phosphate (P/sub i/) longitudinal relaxation times were determined by performing inversion recovery experiments during steady-state ATP/sub λ/ saturation and were used in combination with ST data to determine P/sub i/ consumption rates. 13C NMR and O2 electrode measurements were also conducted to monitor changes in rates of glucose consumption and O2 consumption, respectively, under the various metabolic conditions examined. The results suggest that GAPDH/PGK-catalyzed P/sub i/-ATP exchange is responsible for antimycin-resistant saturation transfer observed in anaerobic and aerobic glucose-fed yeast. Kinetics through GAPDH/PGK were found to depend on metabolic conditions. The coupled system appears to operate in a unidirectional manner during anaerobic glucose metabolism and bidirectionally when the cells are respiring on exogenously supplied ethanol. Additionally, mitochondrial ATPase activity appears to be responsible for the transfer observed in iodoacetate-treated aerobic cells supplied with either glucose or ethanol, with synthesis of ATP occurring unidirectionally

  15. Fósforo num Cambissolo cultivado com cana-de-açúcar por longo tempo: II - análise de ácidos húmicos por RMN 31P Phosphorus in an Inceptsoil under long-term sugarcane: II - humic acid analysis by NMR 31P

    Jader Galba Busato; Luciano Pasqualoto Canellas; Victor Marcos Rumjanek; Ary Carlos Xavier Velloso

    2005-01-01

    Sistemas de manejo da lavoura de cana-de-açúcar que favoreçam a matéria orgânica do solo podem aumentar o conteúdo de nutrientes disponíveis e diminuir a necessidade de aplicação de fertilizantes industriais. Apesar da importância dos componentes orgânicos no fornecimento de P, pouco se conhece sobre a sua dinâmica em ambientes tropicais. O objetivo deste trabalho foi identificar, por meio da ressonância magnética nuclear (RMN 31P), as espécies de P nos ácidos húmicos de um Cambissolo Háplico...

  16. {sup 31}P-MR-spectroscopy of the skeletal muscles under load: demonstration of normal energy metabolism compared to different neuromuscular diseases; {sup 31}P-MR-Spektroskopie der peripheren Skelettmuskulatur unter Belastung: Darstellung des normalen Energiestoffwechsels im Vergleich zu metabolischen Muskelerkrankungen

    Block, W.; Traeber, F.; Kuhl, C.K.; Keller, E.; Rink, H.; Schild, H.H. [Bonn Univ. (Germany). Radiologische Klinik; Lamerichs, R. [Philips Medical Systems, Best (Netherlands); Karitzky, J. [Bonn Univ. (Germany). Neurologische Klinik

    1998-03-01

    Purpose: {sup 31}P-MR spectroscopy of skeletal muscle under ecercise was used to obtain the range of normal variation and comparison was made for different neuromascular diseases. Methods: 41 examinations of 24 volunteers and 41 investigations in 35 patients were performed on 1.5 T MR systems (Gyroscan S15 und S15/ACSII, Philips). Localised {sup 31}P-MR spectra of the calf muscle were obtained in time series with a resolution of 12 s. Results: Two types of muscle energy metabolism were identified from the pattern of spectroscopic time course in volunteers: While the first group was characterised by a remarkable decline to lower pH values during exercise, the second group showed only small pH shifts (minimum pH: 6.48{+-}0.13 vs 6.87{+-}0.07, p<10{sup -6}) although comparable workload conditions were maintained. The pH-values correlated well with blood lactate analysis. Patients with metabolic disorders and chronic fatigue syndrome (CFS) showed decreased resting values of PCr/(PCr+P{sub i}) and increased pH levels during exercise. PCr recovery was significantly delayed (0.31 vs 0.65 min{sup -1}, p<0.00005) in metabolic muscle disorders but was normal in CFS patients. Conclusion: Findings in volunteers indicate utilisation of different metabolic pathways which seems to be related to the fibre type composition of muscle. Reduced resting levels for PCr/(PCr+P{sub i}), altered pH time courses, and decreased PCr recovery seem to be helpful indicators for diagnosis of metabolic muscle disorders. (orig./MG) [Deutsch] Ziel: Bestimmung der Bandbreite des gesunden Energiestoffwechsels der peripheren Skelettmuskulatur mit Hilfe der {sup 31}P-MR-Spektroskopie als Grundlage der Diagnostik neuromuskulaerer Erkrankungen. Methoden: In Mehrfachuntersuchungen an 24 Probanden und 35 Patienten in 1,5 T MR-Systemen (Gyroscan S15 und S15/ACSII, Philips) wurden {sup 31}P-MR-Spektren unter Belastung akquiriert. Ergebnisse: Die Probanden liessen sich streng in zwei Gruppen einteilen

  17. Nuclear reaction analysis of 1H and 2H in hafnium silicate films on Si

    The 1H(15N,αγ)12C and 2H(3He,p)4He nuclear reactions were employed to detect, respectively, 1H and 2H in hafnium silicates films on Si. The methods employed to achieve quantitative analyses are described. Moreover, by performing annealing sequences in vacuum or O2 followed by 1H2 or 2H2, it was observed that the O2-preanneled films incorporate less H, either 1H or 2H. This was explained by O-deficient, H-trapping sites that are eliminated by the O2 preannealing

  18. Predictability of 1-h postload plasma glucose concentration: A 10-year retrospective cohort study

    Kuang, Lifen; Huang, Zhimin; Hong, Zhenzhen; Chen, Ailing; Li, Yanbing

    2015-01-01

    Aims/Introduction Elevated 1-h postload plasma glucose concentration (1hPG) during oral glucose tolerance test has been linked to an increased risk of type 2 diabetes and a poorer cardiometabolic risk profile. The present study analyzed the predictability and cut-off point of 1hPG in predicting type 2 diabetes in normal glucose regulation (NGR) subjects, and evaluated the long-term prognosis of NGR subjects with elevated 1hPG in glucose metabolism, kidney function, metabolic states and athero...

  19. 1H magnetic resonance spectroscopy (1H MRS) in the initially differentiating recurrent brain gliomas after radiation therapy from delayed cerebral necrosis

    Objective: To evaluate 1H magnetic resonance spectroscopy (1H MRS) in the differentiating recurrent brain gliomas after radiation therapy from delayed cerebral necrosis. Methods: Fifteen patients who had clinical and CT, MRI changes that suggested a diagnosis of delayed cerebral necrosis or recurrent brain tumor after radiation therapy and 5 patients who had a definite clinical diagnosis of delayed cerebral necrosis underwent single MR spectroscopy simultaneously both in the lesion's region and the contralateral side. Results: Of the former 15 cases who proved by surgical pathology, 14 cases were gliomas, 1 case was delayed cerebral necrosis, and their etiologic diagnoses of 1H MRS were correct. (1) 1H MRS in 14 cases with gliomas exhibited specific spectral peaks including prominent choline-containing compounds (Cho), decreased or absent acetylaspartate (NAA) and total creatine (Cr), and the metabolic ratios showed significantly increased Cho/Cr, decreased NAA/Cr. Twelve cases showed abnormal lactate (Lac). (2) Among 6 cases with delayed cerebral necrosis, 5 cases exhibited decreased or absent Cho, NAA, Cr, and abnormal Lipid, 1 case showed absent Cho, NAA, and Cr with a flat curve without Lac. Conclusion: 1H MRS was positively claimed for differentiating recurrent brain gliomas after radiation therapy from delayed cerebral necrosis

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

    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...

  1. {sup 1}H MR spectroscopy in histopathological subgroups of mesial temporal lobe epilepsy

    Hajek, Milan; Dezortova, Monika [Institute for Clinical and Experimental Medicine, MR Unit, Department of Diagnostic and Interventional Radiology, Prague (Czech Republic); Krsek, Pavel; Komarek, Vladimir [Charles University, Department of Pediatric Neurology, Prague 5 (Czech Republic); Marusic, Petr; Tomasek, Martin; Krijtova, Hana [Charles University, Department of Neurology, Prague (Czech Republic); Zamecnik, Josef [Charles University, Department of Pathology and Molecular Medicine, Prague (Czech Republic); Kyncl, Martin [Charles University, Department of Radiology, Prague (Czech Republic)

    2009-02-15

    The aim of the study was to analyze the lateralizing value of proton magnetic resonance spectroscopy ({sup 1}H MRS) in histopathologically different subgroups of mesial temporal lobe epilepsies (MTLE) and to correlate results with clinical, MRI and seizure outcome data. A group of 35 patients who underwent resective epilepsy surgery was retrospectively studied. Hippocampal {sup 1}H MR spectra were evaluated. Metabolite concentrations were obtained using LCModel and NAA/Cr, NAA/Cho, NAA/(Cr+Cho), Cho/Cr ratios and coefficients of asymmetry were calculated. MRI correctly lateralized 89% of subjects and {sup 1}H MRS 83%. MRI together with {sup 1}H MRS correctly lateralized 100% of patients. Nineteen subjects had 'classical' hippocampal sclerosis (HS), whereas the remaining 16 patients had 'mild' HS. Nineteen patients had histopathologically proven malformation of cortical development (MCD) in the temporal pole; 16 subjects had only HS. No difference in {sup 1}H MRS findings was found between patients in different histopathological subgroups of MTLE. Our results support the hypothesis that {sup 1}H MRS abnormalities do not directly reflect histopathological changes in MTLE patients. Subjects with non-lateralized {sup 1}H MRS abnormalities did not have a worse postoperative seizure outcome. We found no significant impact of contralateral {sup 1}H MRS abnormality on post-surgical seizure outcome. (orig.)

  2. 1H MR spectroscopy in histopathological subgroups of mesial temporal lobe epilepsy

    The aim of the study was to analyze the lateralizing value of proton magnetic resonance spectroscopy (1H MRS) in histopathologically different subgroups of mesial temporal lobe epilepsies (MTLE) and to correlate results with clinical, MRI and seizure outcome data. A group of 35 patients who underwent resective epilepsy surgery was retrospectively studied. Hippocampal 1H MR spectra were evaluated. Metabolite concentrations were obtained using LCModel and NAA/Cr, NAA/Cho, NAA/(Cr+Cho), Cho/Cr ratios and coefficients of asymmetry were calculated. MRI correctly lateralized 89% of subjects and 1H MRS 83%. MRI together with 1H MRS correctly lateralized 100% of patients. Nineteen subjects had ''classical'' hippocampal sclerosis (HS), whereas the remaining 16 patients had ''mild'' HS. Nineteen patients had histopathologically proven malformation of cortical development (MCD) in the temporal pole; 16 subjects had only HS. No difference in 1H MRS findings was found between patients in different histopathological subgroups of MTLE. Our results support the hypothesis that 1H MRS abnormalities do not directly reflect histopathological changes in MTLE patients. Subjects with non-lateralized 1H MRS abnormalities did not have a worse postoperative seizure outcome. We found no significant impact of contralateral 1H MRS abnormality on post-surgical seizure outcome. (orig.)

  3. Forms of organic C and P extracted from tropical soils as assessed by liquid-state 13C- and 31P-NMR spectroscopy

    Transformation of soil organic phosphorus (SOP) is linked with the transformation of soil organic carbon (SOC). Yet, it is uncertain to which SOC structures the cycling of SOP is related, especially in tropical environments. To clarify this issue, we determined the vertical distribution of extractable C and P chemical structures in 4 soil profiles using solution 13C- and 31P-nuclear magnetic resonance (NMR) spectroscopy after extraction with 0.1 M NaOH/0.4 M NaF (1 : 1). Soils were from a cabbage cultivation with annual burning of weeds, a Pinus reforestation, a secondary forest, and a primary forest in northern Thailand. For all profiles, signals due to O-alkyl and carbonyl C dominated the 13C-NMR spectra (up to 50 and 22% of total spectral area, respectively). The proportions of alkyl and aryl C decreased, whereas carbonyl and O-alkyl C increased with soil depth. Sharp resonances at 135 and 177 ppm appeared in spectra of subsoil horizons. They indicated mellitic acid, an end-product of the oxidation of charred plant residues. The SOP forms comprised mainly orthophosphate diesters in the organic layer of the forests, whereas in the mineral horizons orthophosphate monoesters dominated the chemical composition of extractable SOP. The relationships between SOC and SOP forms in the organic floor layers of the forests were clearly different from those in the mineral soil horizons, indicating changed SOM dynamics upon contact with soil minerals. In the forest mineral soils, significant correlations between monoester-P and O-alkyl C (R = 0.84, P < 0.001) were found. Diester-P, teichoic acids, and phosphonates were positively correlated with aromatic C and negatively with O-alkyl C. At the same time, teichoic acids and phosphonates were positively correlated with short range-ordered Al and Fe oxide phases. These findings can be explained through an increasing microbial decay of aryl C and diester-P compounds that may be less effectively stabilised at lower depths

  4. {sup 31}P-MR spectroscopy of the brain in patients with anorexia nervosa: characteristic differences in the spectra between patients and healthy control subjects; {sup 31}P-MRS des Hirns bei Anorexia nervosa: charakteristische Unterschiede in den Spektren von Patienten und gesunden Vergleichspersonen

    Rzanny, R.; Reichenbach, J.R.; Mentzel, H.J.; Pfleiderer, S.O.R.; Kaiser, W.A. [Inst. fuer Diagnostische und Interventionelle Radiologie, Klinikum der Friedrich-Schiller-Univ. Jena (Germany); Freesmeyer, D.; Klemm, S.; Gerhard, U.J.; Blanz, B. [Klinik fuer Kinder- und Jugendpsychiatrie, Klinikum der Friedrich-Schiller-Univ. Jena (Germany)

    2003-01-01

    Purpose: To investigate whether {sup 31}P-MR spectroscopy can detect reduced concentrations of high-energy phosphates, like PCr and NTP, caused by decreased metabolic activity in the brain of patients with anorexia nervosa (AN) and, furthermore, whether any impairment of the cerebral membrane metabolism can be derived from the spectra. Material and Methods: 10 female patients, age range 12 - 20 years and mean BMI (body mass index) of 14.8 {+-} 1.6 kg/m{sup 2}, with clinically diagnosed AN (ICD-10, F50.0) and 10 healthy control subjects, age range 12 - 21 years and mean BMI 19.0 {+-} 2.1 kg/m{sup 2}, without nutritional disturbances: were investigated. {sup 31}P-MR spectroscopy was performed with a 1.5 T MRI unit using single volume selection in the frontal/prefrontal region of brain. Relative metabolic concentrations were quantified by normalizing the peak areas of the metabolites with the total area of the complete phosphorous spectrum, P{sub tot}, as well as with the peak area of β-NTP. Results: Significant differences between the two groups were observed for the metabolic ratios PDE/P{sub tot}, PDE/β-NTP and {alpha}-NTP/P{sub tot} which were lower in the patient group except for {alpha}-NTP/P{sub tot}. These ratios also revealed a statistically significant correlation with the BMI (r{sub PDE/Ptot} = 0.747, r{sub PDE/β-NTP} = 0.57, r{sub {alpha}}{sub -NTP/Ptot} = -0.56; p {<=} 0.1). Reduced relative concentrations of PCr/P{sub tot}, β-NTP/P{sub tot} or Pi/P{sub tot} were not encountered. Conclusion: The lowered PDE/P{sub tot} ratio for patients with AN and its correlation with BMI suggests that decreased BMI induces compositional changes of the phospholipids in the brain, which decrease the fraction of mobile phospholipids. (orig.) [German] Problemstellung: Das Ziel dieser Studie war es zu untersuchen, ob mit Hilfe der {sup 31}P-MR-Spektroskopie ({sup 31}P-MRS) im Gehirn von Patienten mit Anorexia nervosa (AN) verringerte Konzentrationen an

  5. Dimethyl sulfone in human cerebrospinal fluid and blood plasma confirmed by one-dimensional (1)H and two-dimensional (1)H-(13)C NMR.

    Engelke, U.F.H.; Tangerman, A.; Willemsen, M.A.A.P.; Moskau, D.; Loss, S.; Mudd, S.H.; Wevers, R.A.

    2005-01-01

    (1)H-NMR spectroscopy at 500 MHz was used to confirm that a previously unidentified singlet resonance at 3.14 ppm in the spectra of cerebrospinal fluid and plasma samples corresponds to dimethyl sulfone (DMSO(2)). A triple resonance inverse cryogenic NMR probe, with pre-amplifier and the RF-coils co

  6. A new AgI complex based on 1-[(1H-benzimidazol-1-ylmethyl]-1H-1,2,4-triazole

    Yan-zhi Wang

    2011-12-01

    Full Text Available In the title complex, bis{μ-1-[(1H-benzimidazol-1-ylmethyl]-1H-1,2,4-triazole}disilver(I dinitrate, [Ag2(C10H9N52](NO32, the AgI ion is nearly linearly coordinated [N—Ag—N angle is 155.72 (14°] by two 1-[(1H-benzimidazole-1-ylmethyl]-1H-1,2,4-triazole (bmt ligands. In addition, two bmt ligands link two AgI ions, forming a dinuclear unit with an Ag...Ag distance of 5.0179 (15 Å. The whole complex is generated by an inversion centre. The dinuclear units and the NO3− counter-ions are connected by N—H...O hydrogen bonds and weak Ag...O interactions [2.831 (5, 2.887 (5 and 2.908 (5 Å], leading to a three-dimensional structure.

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

    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.

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

    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

  9. 1H-MRS study of brain metabolic disorder in patients with cyanosed congenital heart disease

    Objective: To study the metabolic alteration in the brain of patients with cyanosed congenital heart disease (CCHD) by using 1H-magnetic resonance spectroscopy (1H-MRS) and discover the pathophysiology of chronic hypoxic brain, which will help to diagnose and treat this disease completely. Methods: Twenty-five patients with CCHD and 25 controls were performed PRESS 1H-MRS and MRI. The areas under the resonance of metabolites were measured, the ratios of the other metabolites to Cr were calculated and compared. Results: In patients with CCHD, the mean value of NAA/Cr was significantly lower than that in controls (P 0.05). Conclusion: 1H-MRS can detect brain metabolic changes in patients with cyanosed congenital heart disease in vivo noninvasively and can detect the metabolism disorder of the energy and amino acid, so the pathophysiology of this disease can be understood

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

    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.

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

    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)

  12. 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

    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.

  13. 1H NMR profiling as an approach to differentiate conventionally and organically grown tomatoes.

    Hohmann, Monika; Christoph, Norbert; Wachter, Helmut; Holzgrabe, Ulrike

    2014-08-20

    This study describes the approach of (1)H NMR profiling for the authentication of organically produced tomatoes (Solanum lycopersicum). Overall, 361 tomato samples of two different cultivars and four different producers were regularly analyzed during a 7 month period. The results of principal component analysis showed a significant trend for the separation between organically and conventionally produced tomatoes (p cultivation method, yet the results indicate significant differences between (1)H NMR spectra of organically and conventionally grown tomatoes. PMID:25066078

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

    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.

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

    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. PMID:26878852

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

    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.

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

    Yu-xian Li

    2011-08-01

    Full Text Available In the title complex, [Co(SO4(C9H8N6(H2O4]·2H2O, the CoII ion is six-coordinated by one N atom from a 1H-1,2,3-benzotriazol-1-ylmethyl]-1H-1,2,4-triazole ligand, one O atom from a monodentate sulfate ligand and four water molecules in a slightly distorted octahedral geometry. The sulfate ligand is rotationally disordered over two sets of sites with refined occupancies of 0.662 (15 and 0.338 (15. In the crystal, complex molecules and solvent water molecules are linked through intermolecular O—H...O and O—H...N hydrogen bonds into a three-dimensional network.

  18. Crystal structures and luminescence properties of two Cd(II) complexes based on 2-(1H-imidazol-1methyl)-6-methyl-1H-benzimidazole

    Zhang, Yuhong; Meng, Xiangru; Wen, Yu; Li, Peng; Ma, Lin [Zhengzhou Univ. (China). College of Chemistry and Molecular Engineering; Zhang, Qiuju [Zhengzhou Univ. (China). Clinical Testing Section

    2015-11-01

    Two new complexes, {[Cd(immb)I_2].DMF}{sub n} (1) and {[Cd_3(immb)(btc)_2]. H_2O}{sub n} (2) (immb = 2-(1H-imidazol- 1-methyl)-6-methyl-1H-benzimidazole, btc = 1,2,3-benzenetricarboxylate, DMF = dimethyl formamide), have been synthesized and characterized. Single crystal X-ray diffraction shows that 1 exhibits a chain structure constructed by immb ligands bridging Cd(II) ions. In 2, Cd(II) ions are linked by immb ligands with bridging mode and btc3- anions with the μ{sub 2}-η{sup 2}:η{sup 1} bonding pattern leading to a 2D structure. Luminescent properties have been investigated in the solid state at room temperature.

  19. 糖尿病大鼠脑能量代谢改变的核磁共振磷谱研究%Studies on Changes of Brain Energy Metabolism in Diabetic Rats by 31 P Magnetic Resonance Spectroscopy

    王娜; 郑涌泉; 许翠翠; 苏永超; 赵良才; 叶信健; 高红昌

    2014-01-01

    Considerable attention has been directed toward studying the impact of diabetes on the central nervous system. The current study investigates the biochemical changes in the brain tissue of streptozotocin (STZ)-induced diabetic rat using 31P magnetic resonance spectroscopy (31P MRS). The 31P NMR spectra of the whole brain show no significant changes of phosphomonoesters and phosphodiesters levels one week after STZ induction, suggesting no apparent structural changes in cell membranes. The results identifies the increased level of adenosine diphosphate, negligible changes of phosphocreatine ( PCr ) and adenosine triphosphate ( ATP) , but the decreased ratio of PCr/ATP, indicating that PCr plays a role of balancing the energy. Moreover, the decreased pH value indicates the changes of the intracellular environment in STZ-diabetic brains in rats. After 15 weeks of STZ injection, the metabolism of phospholipid membrane and brain energy metabolism has been obviously disturbed. Our study successfully shows that 31 P MRS can not only study phospholipid and energy metabolism non-invasively, but also measure intracellular pH and other important biochemical information. All of these spectroscopic characterizations contribute significantly to the understanding of pathogenesis and evolution of diabetes, and provide theoretical basis for early diagnosis and clinical treatment in diabetes.%应用链脲佐菌素( Streptozocin, STZ)制备糖尿病( Diabetes mellitus, DM)大鼠模型,采用离体的核磁共振磷谱(31 P Magnetic resonance spectroscopy, MRS)方法检测糖尿病大鼠脑组织的生化改变。全脑的31 P MRS谱图结果显示,STZ诱导1周后,磷酸单酯和磷酸二酯的含量无明显改变,表明糖尿病大鼠脑中并没有发生膜性结构的改变。二磷酸腺苷峰增高,磷酸肌酸( Phosphocreatine, PCr)和三磷酸腺苷( Adenosine triphosphate, ATP)含量无明显改变,但是PCr/ATP降低,说明PCr作为能量缓冲底

  20. Predictability of 1-h postload plasma glucose concentration: A 10-year retrospective cohort study

    Kuang, Lifen; Huang, Zhimin; Hong, Zhenzhen; Chen, Ailing; Li, Yanbing

    2015-01-01

    Aims/Introduction Elevated 1-h postload plasma glucose concentration (1hPG) during oral glucose tolerance test has been linked to an increased risk of type 2 diabetes and a poorer cardiometabolic risk profile. The present study analyzed the predictability and cut-off point of 1hPG in predicting type 2 diabetes in normal glucose regulation (NGR) subjects, and evaluated the long-term prognosis of NGR subjects with elevated 1hPG in glucose metabolism, kidney function, metabolic states and atherosclerosis. Materials and Methods A total of 116 Han Chinese classified as NGR in 2002 at the First Affiliated Hospital of Sun Yat-sen University, Guangzhou, Guangdong, China, were investigated. Follow-up was carried out in 2012 to evaluate the progression of glucose metabolism, kidney function, metabolic syndrome and carotid atherosclerosis. Results The areas under receiver operating characteristic curves were higher for 1hPG than FPG or 2hPG (0.858 vs 0.806 vs 0.746). The cut-off value of 1hPG with the maximal sum of sensitivity and specificity in predicting type 2 diabetes in NGR subjects was 8.85 mmol/L. The accumulative incidence of type 2 diabetes in subjects with 1hPG ≥8.85 mmol/L was higher than those <8.85 mmol/L (46.2% vs 3.3%, P = 0.000; relative risk 13.846, 95% confidence interval 4.223–45.400). On follow up, the prevalence of metabolic syndrome and abnormal carotid intima-media thickness in the subjects with 1hPG ≥8.85 mmol/L tended to be higher compared with those <8.85 mmol/L. Conclusions 1hPG is a good predictor of type 2 diabetes in NGR subjects, and the best cut-off point is 8.85 mmol/L. Some tendency indicates that NGR subjects with 1hPG ≥8.85 mmol/L are more prone to metabolic syndrome and carotid atherosclerosis. PMID:26543538

  1. Higgs phenomenology in Type-I 2HDM with U(1)H Higgs gauge symmetry

    It is well known that generic two-Higgs-doublet models (2HDMs) suffer from potentially large Higgs-mediated flavor-changing neutral current (FCNC) problem, unless additional symmetries are imposed on the Higgs fields thereby respecting the Natural Flavor Conservation Criterion (NFC) by Glashow and Weinberg. A common way to respect the NFC is to impose Z2 symmetry which is softly broken by a dim-2 operator. Another new way is to introduce local U(1)H Higgs flavor symmetry that distinguishes one Higgs doublet from the other. In this paper, we consider the Higgs phenomenology in Type-I 2HDMs with the U(1)H symmetry with the simplest U(1)H assignments that the SM fermions are all neutral under U(1)H, and we make detailed comparison with the ordinary Type-I 2HDM. After imposing various constraints such as vacuum stability and perturbativity as well as the electroweak precision observables and collider search bounds on charged Higgs boson, we find that the allowed Higgs signal strengths in our model are much broader than those in the ordinary Type-I 2HDM, because of newly introduced U(1)H-charged singlet scalar and U(1)H gauge boson. Still the ATLAS data on gg→h→γγ cannot be accommodated. Our model could be distinguished from the ordinary 2HDM with the Z2 symmetry in a certain parameter region and some channels. If the couplings of the new boson turn out to be close to those in the SM, it would be essential to search for extra U(1)H gauge boson and/or one more neutral scalar boson to distinguish two models

  2. 家兔肝脏31P MR波谱重复性检测及其影响因素探讨%Reproducibility and influencing factors of 31p MR spectroscopy in rabbit liver with two-dimensional chemical shift imaging

    余日胜; 孙建忠; 丁文洪; 徐秀芳; 王志康

    2009-01-01

    目的 探讨MR二维化学位移成像(2D CSI)在家兔肝脏磷代谢物相对量检测中的重复能力及其影响因素.方法 对浓度为0.05 mol/L的500 ml磷酸盐(NaH2PO4)溶液体模及1只家兔在1 d内分别进行30次并于次日重复30次2D CSI MR扫描,分析MR机的稳定性及同一个体磷代谢物的重复能力;对30只家兔在2 d内各行1次31P MRS扫描,分析同一群体磷代谢物的重复能力.在每一次家兔检测前均先行体模31P MRS扫描,测得校正系数,对不同时间段内所检测得的家兔磷代谢物相对值进行校正,获得校正相对值,采用变异系数分析各代谢物相对最检测误差,并采用t检验进行比较.结果 (1)体模检测:2 d内磷酸盐体模输测误差分别为4.92%和5.12%,2 d内磷化合物相对值分别为16.68±0.82和16.56±0.85,差异无统计学意义(t=0.665,P>0.05).(2)同一家兔检测:各磷化合物的检测误筹在8.04%~34.13%之间,其中以β-ATP重复性最好,误差均在10%以内;不同2 d 2次检测磷酸单脂(PME)分别为0.88±0.28和0.88±0.30,磷酸二脂(PDE)分别为4.35±0.66和4.35±0.66,无机磷(Pi)分别为0.95±0.30和0.97±0.28,α-ATP分别为5.58±0.60和5.61±0.61,β-ATP分别为2.70±0.22和2.71±0.22,γ-ATP分别为2.20±0.63和2.18±0.44,差异均无统计学意义(P值均>0.05).(3)同一群体家兔检测:各磷化合物的检测误差在8.48%~36.21%之间,其中以β-ATP重复性最好,误差均在10%以内,2次检测PME分别为0.84±0.30和0.79±0.28,PDE分别为4.29±0.72和3.94±0.84,Pi分别为0.91±0.28和0.92±0.31,α-ATP分别为5.65±0.66和5.36±0.60,β-ATP分别为2.71±0.23和2.66±0.25,γ-ATP分别为2.07±0.29和1.99±0.37,差异均无统计学意义(P值均>0.05).结论 在各磷化合物中,β-ATP相对量误差小,将它作为评价实验性肝病的指标最可靠.家兔的2D CSI肝脏31P MRS技术受多种因素影响.%Objective To investigate the reproducibility and influencing factors of relative quantification of

  3. The structure and properties of 5,6-dinitro-1H-benzotriazole

    Santa María, Dolores; Claramunt, Rosa M.; Torralba, M. Carmen; Torres, M. Rosario; Alkorta, Ibon; Elguero, José

    2016-06-01

    5,6-Dinitro-1H-benzotriazole crystallizes in the monoclinic system, space group P21/c. The asymmetric unit contains the planar 1H-tautomer together with a water molecule of crystallization. Each water molecule is hydrogen bonded to three adjacent 5,6-dinitrobenzotriazoles forming a tape along the b-axis of the crystal. These tapes stack along the c-axis through hydrogen bonds involving the water molecules and one of the nitro groups leading to a bidimensional structure. Solid-state 13C and 15N CPMAS NMR allow to confirm that the tautomer present is the 1H one. In DMSO-d6 solution the results are quite different and, based on GIAO/B3LYP/6-311++G(d,p) calculations, lead us to conclude that the major tautomer is the 5,6-dinitro-2H-benzotriazole, a surprising result that contradicts the rule that the major tautomer in solution coincides with the one present in the crystal. An anhydrous pseudopolymorph of 5,6-dinitro-1H-benzotriazole has been obtained as a non-crystalline form and from solid-state NMR and theoretical calculations, we conclude that it is an 1H-tautomer.

  4. Hematocrit and oxygenation dependence of blood (1)H(2)O T(1) at 7 Tesla.

    Grgac, Ksenija; van Zijl, Peter C M; Qin, Qin

    2013-10-01

    Knowledge of blood (1)H2O T1 is critical for perfusion-based quantification experiments such as arterial spin labeling and cerebral blood volume-weighted MRI using vascular space occupancy. The dependence of blood (1)H2O T1 on hematocrit fraction (Hct) and oxygen saturation fraction (Y) was determined at 7 T using in vitro bovine blood in a circulating system under physiological conditions. Blood (1)H2O R1 values for different conditions could be readily fitted using a two-compartment (erythrocyte and plasma) model, which are described by a monoexponential longitudinal relaxation rate constant dependence. It was found that T1 = 2171 ± 39 ms for Y = 1 (arterial blood) and 2010 ± 41 ms for Y = 0.6 (venous blood), for a typical Hct of 0.42. The blood (1)H2O T1 values in the normal physiological range (Hct from 0.35 to 0.45, and Y from 0.6 to 1.0) were determined to range from 1900 to 2300 ms. The influence of oxygen partial pressure (pO2) and the effect of plasma osmolality for different anticoagulants were also investigated. It is discussed why blood (1)H2O T1 values measured in vivo for human blood may be about 10-20% larger than found in vitro for bovine blood at the same field strength. PMID:23169066

  5. 1H NMR based metabolic profiling in the evaluation of Japanese green tea quality.

    Tarachiwin, Lucksanaporn; Ute, Koichi; Kobayashi, Akio; Fukusaki, Eiichiro

    2007-11-14

    Classification of tea quality is now mainly performed according to the sensory results by professional tea tasters. However, this evaluation method is inconsistent in differentiating their qualities. A combination of a (1)H NMR technique and a multivariate analysis was introduced to the quality evaluation of green tea by means of a metabolomic technique. A broad range of metabolites were detected by (1)H NMR spectrometry. The principal component analysis (PCA) was used to reduce the complexity of the (1)H NMR spectra data set and provided the quality discrimination result. It offered an extensive clue for classification and quality assessment without any prepurification method. A set of green teas from a Japanese tea contest were analyzed by (1)H NMR to classify the quality with respect to that judged by tea tasters and to conceive a quality prediction model. Metabolic profiling and fingerprinting of (1)H NMR spectra of green teas with different quality were studied. PCA showed a separation between the high- and the low-quality green teas. The taste marker compounds contributing to the discrimination of tea quality were identified. Reliable prediction models were obtained by the partial least-squares projection to latent structure (PLS) analysis together with a preprocessing filter of both orthogonal signal correction (OSC) and a combination between OSC and wavelet transform algorithms. PMID:17944534

  6. Synthesis and preliminary evaluation of 3-thiocyanato-1H-indoles as potential anticancer agents.

    Fortes, Margiani P; da Silva, Paulo B N; da Silva, Teresinha G; Kaufman, Teodoro S; Militão, Gardenia C G; Silveira, Claudio C

    2016-08-01

    A novel series of twenty 3-thiocyanato-1H-indoles, carrying diversification at positions N-1, C-2 and C-5 of the heterocyclic core, were synthesized; their antiproliferative activity against four human cancer cell lines (HL60, HEP-2, NCI-H292 and MCF-7) was evaluated, employing doxorubicin as positive control. Indole, N-methylindole and 2-(4-chlorophenyl)-N-methylindole demonstrated to be essentially inactive, whereas several of their congener 3-thiocyanato-1H-indoles displayed good to excellent levels of potency (IC50 ≤ 6 μM), while being non-hemolytic. N-Phenyl-3-thiocyanato-1H-indole and 1-methyl-2-(4-chlorophenyl)-3-thiocyanato-1H-indole showed good to high potency against all the cell lines. On the other side, the N-(4-chlorophenyl)-, 2-(4-chlorophenyl)- and 2-phenyl- 3-thiocyanato-1H-indole derivatives were slightly less active against the test cell lines. Overall, these results suggest that the indole-3-thiocyanate motif can be suitably decorated to afford highly cytotoxic compounds and that the substituted indole can be employed as a useful scaffold toward more potent compounds. PMID:27116711

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

    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 99mTc- ECD SPECT. Frontal white matter and the basal ganglia of both hemispheres were subjected to localized 1H-MRS, and after revascularization surgery, four patients underwent follow-up 1H-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, 1H-MRS is potentially useful for the preoperative evaluation of metabolic abnormalities and their postoperative monitoring

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

    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.

  9. Selective excitation enables assignment of proton resonances and {sup 1}H-{sup 1}H distance measurement in ultrafast magic angle spinning solid state NMR spectroscopy

    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)

    2015-07-21

    Remarkable developments in ultrafast magic angle spinning (MAS) solid-state NMR spectroscopy enabled proton-based high-resolution multidimensional experiments on solids. To fully utilize the benefits rendered by proton-based ultrafast MAS experiments, assignment of {sup 1}H resonances becomes absolutely necessary. Herein, we propose an approach to identify different proton peaks by using dipolar-coupled heteronuclei such as {sup 13}C or {sup 15}N. In this method, after the initial preparation of proton magnetization and cross-polarization to {sup 13}C nuclei, transverse magnetization of desired {sup 13}C nuclei is selectively prepared by using DANTE (Delays Alternating with Nutations for Tailored Excitation) sequence and then, it is transferred to bonded protons with a short-contact-time cross polarization. Our experimental results demonstrate that protons bonded to specific {sup 13}C atoms can be identified and overlapping proton peaks can also be assigned. In contrast to the regular 2D HETCOR experiment, only a few 1D experiments are required for the complete assignment of peaks in the proton spectrum. Furthermore, the finite-pulse radio frequency driven recoupling sequence could be incorporated right after the selection of specific proton signals to monitor the intensity buildup for other proton signals. This enables the extraction of {sup 1}H-{sup 1}H distances between different pairs of protons. Therefore, we believe that the proposed method will greatly aid in fast assignment of peaks in proton spectra and will be useful in the development of proton-based multi-dimensional solid-state NMR experiments to study atomic-level resolution structure and dynamics of solids.

  10. Dynamics-based selective 2D {sup 1}H/{sup 1}H chemical shift correlation spectroscopy under ultrafast MAS conditions

    Zhang, Rongchun; Ramamoorthy, Ayyalusamy, E-mail: ramamoor@umich.edu [Biophysics and Department of Chemistry, University of Michigan, Ann Arbor, Michigan 48109-1055 (United States)

    2015-05-28

    Dynamics plays important roles in determining the physical, chemical, and functional properties of a variety of chemical and biological materials. However, a material (such as a polymer) generally has mobile and rigid regions in order to have high strength and toughness at the same time. Therefore, it is difficult to measure the role of mobile phase without being affected by the rigid components. Herein, we propose a highly sensitive solid-state NMR approach that utilizes a dipolar-coupling based filter (composed of 12 equally spaced 90° RF pulses) to selectively measure the correlation of {sup 1}H chemical shifts from the mobile regions of a material. It is interesting to find that the rotor-synchronized dipolar filter strength decreases with increasing inter-pulse delay between the 90° pulses, whereas the dipolar filter strength increases with increasing inter-pulse delay under static conditions. In this study, we also demonstrate the unique advantages of proton-detection under ultrafast magic-angle-spinning conditions to enhance the spectral resolution and sensitivity for studies on small molecules as well as multi-phase polymers. Our results further demonstrate the use of finite-pulse radio-frequency driven recoupling pulse sequence to efficiently recouple weak proton-proton dipolar couplings in the dynamic regions of a molecule and to facilitate the fast acquisition of {sup 1}H/{sup 1}H correlation spectrum compared to the traditional 2D NOESY (Nuclear Overhauser effect spectroscopy) experiment. We believe that the proposed approach is beneficial to study mobile components in multi-phase systems, such as block copolymers, polymer blends, nanocomposites, heterogeneous amyloid mixture of oligomers and fibers, and other materials.

  11. Bis{1-[(1H-benzimidazol-1-ylmethyl-κN3]-1H-1,2,3,4-tetrazole}silver(I nitrate

    Xiang-ru Meng

    2010-03-01

    Full Text Available In the title salt, [Ag(C9H8N62]NO3, the central AgI atom is linearly coordinated by the N atoms [171.97 (8°] from two 1-[(benzimidazol-1-ylmethyl]-1H-1,2,3,4-tetrazole ligands. The benzimidazole rings in adjacent molecules are parallel with an average interplanar distance of 3.461 Å; adjacent molecules are linked through N—H...O hydrogen bonds into a linear chain along the b-axis direction.

  12. Balo's concentric sclerosis: a correlative study of MRI, 1H-MR spectroscopy and biopsy

    Objective: To describe the features of Balo's concentric sclerosis on MRI and 1H-MRS. Methods: Three patients of Balo's concentric sclerosis were reported on the basis of brain MRI and stereotactic brain biopsy. Proton MR spectroscopy was carried out on 1 patient. Results: Multiple ring-like lesions of laminated demyelination alternating with spared white matter were demonstrated in all 3 patients, and the lesions were best seen in post-contrast images. 1H-MRS showed a decreased NAA peak, an increased choline peak, and the presence of large lipid peak. Conclusion: Balo's concentric sclerosis has characteristic findings on MRI and 1H-MRS. MRI is very useful in the diagnosis of Balo's concentric sclerosis

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

    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". PMID:26414291

  14. The (1) H NMR spectrum of pyrazole in a nematic phase.

    Provasi, Patricio; Jimeno, María Luisa; Alkorta, Ibon; Reviriego, Felipe; Elguero, José; Jokisaari, Jukka

    2016-08-01

    The experimental (1) H nuclear magnetic resonance (NMR) spectrum of 1H-pyrazole was recorded in thermotropic nematic liquid crystal N-(p-ethoxybenzylidene)-p-butylaniline (EBBA) within the temperature range of 299-308 K. Two of three observable dipolar DHH -couplings appeared to be equal at each temperature because of fast prototropic tautomerism. Analysis of the Saupe orientational order parameters using fixed geometry determined by computations and experimental dipolar couplings results in a situation in which the molecular orientation relative to the magnetic field (and the liquid crystal director) can be described exceptionally by a single parameter. Copyright © 2016 John Wiley & Sons, Ltd. PMID:26947581

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

    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)

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

    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 metabolism and compared the results to healthy controls. 1H-MRS was acquired by the method of single voxels in white and grey matter. Proton MRS was performed after image guided localization using st...

  17. A childhood acute lymphoblastic leukemia (ALL case with t(3;17(q23;p13,t(5;12(q31;p13,inv(11(p15q12

    Ayse Cirakoglu

    2008-09-01

    Full Text Available It is known that clonal chromosomal changes in childhood ALL are nonrandom and important markers for diagnosis, prognosis and relaps. In this report we present 4 year-old boy with ALL-L1 who has complex chromosomal rearrangements. Chromosome analysis was performed on bone marrow aspiration sample in relaps after one year from diagnosis and induction chemotherapy. The karyotype was; 46,XY,t(3;17(q23;p13,t(5;12(q31;p13,inv(11(p15q12 [11]/46,XY[8

  18. Measurement of the lateral diffusion of dipalmitoylphosphatidylcholine adsorbed on silica beads in the absence and presence of melittin: a 31P two-dimensional exchange solid-state NMR study.

    Picard, F; Paquet, M J; Dufourc, E J; Auger, M.

    1998-01-01

    31P two-dimensional exchange solid-state NMR spectroscopy was used to measure the lateral diffusion, D(L), in the fluid phase of dipalmitoylphosphatidylcholine (DPPC) in the presence and absence of melittin. The use of a spherical solid support with a radius of 320 +/- 20 nm, on which lipids and peptides are adsorbed together, and a novel way of analyzing the two-dimensional exchange patterns afforded a narrow distribution of D(L) centered at a value of (8.8 +/- 0.5) x 10(-8) cm2/s for the pu...

  19. 31P NMR study of improvement in oxidative phosphorylation by vitamins K3 and C in a patient with a defect in electron transport at complex III in skeletal muscle.

    Eleff, S; Kennaway, N G; Buist, N R; Darley-Usmar, V M; Capaldi, R A; Bank, W J; Chance, B

    1984-01-01

    The bioenergetic capacity of skeletal muscle in a 17-year-old patient with a severe defect in complex III of the electron transport chain has been examined by 31P NMR measurements of the molar ratio of phosphocreatine to inorganic phosphate (PCr/Pi). Resting ratios were 1.3-2.5, which can be compared with roughly 8.6 for a young, normal female control at rest. Quantitative evaluation of the activity of oxidative metabolism was afforded by the rate of recovery of PCr/Pi from exercise and was f...

  20. Dynamical decay of 32S* and 31P* formed in 20Ne+12C and 19F+12C reactions, respectively, at E*CN = 60 MeV

    Singh BirBikram

    2015-01-01

    Full Text Available The target-like C-yield in the decay of compound systems 32S* and 31P* formed in 20Ne+12C and 19F+12C reactions at E*CN=60 MeV, is studied for the contribution of fusion-fission (ff decay cross section σff and the deep inelastic (DI orbiting σorb from the compound nucleus (CN and non-compound nucleus nCN processes, respectively. The calculations are performed using the collective clusterization of fragments within the dynamical cluster-decay model (DCM of Gupta and collaborators. Besides studying the competition between ff and DI orbiting phenomenon in the C-yield of these systems, we exclusively investigate the preformation and barrier penetration probabilities P0 and P as a function of angular momentum ℓ values which subsequently affects the contributions of σff and σorb. For calculating the contribution of σff in the C-yield, we have added the contributions from all the minimized intermediate mass fragments (IMFs for Z=6 in the calculated fragmentation potentials for 32S* (IMFs 11,12,13C are minimized and for 31P* (IMFs 12,13C are minimized, while calculating subsequently, P0 and the P for these IMFs. The distribution of preformed clusters/fragments as a function of fragment mass visibly explore the nuclear structure effects for the C-yield in decay of these compound systems, wherein, it is shown to be more favoured in the decay of 31P* in comparison to 32S* decay. The contribution of σorb to the C-yield is calculated from P at different allowed ℓ-values (upto ℓmax and also P≤1 of the outgoing fragments (same as that in the entrance channel, i.e., P0=1. Though preliminary but useful results indicates the competition between the CN and nCN process in the C-yield for the compound system 32S* only while the decay of 31P* is of pure CN origin, as observed in the experimental study. The calculations are in good comparison with the available experimental data.

  1. (1H-1,3-Benzimidazole-5,6-dicarboxylic acid(5-carboxylato-1H-1,3-benzimidazole-6-carboxylic acidsilver(I monohydrate

    Hong Zhai

    2009-11-01

    Full Text Available The title compound, [Ag(C9H5N2O4(C9H6N2O4]·H2O, contains one independent Ag atom, a neutral 1H-benzimidazole-5,6-dicarboxylic acid (bdcH, its monodeprotonated form, i.e. 5-carboxylato-1H-1,3-benzimidazole-6-carboxylic acid (bdc, and one solvent water molecule, the latter being disordered over three sites with site occupancy factors of 0.375 (× 2 and 0.25. In addition, the H atom on one carboxylic acid residue is disordered, being connected to each of the O atoms 50% of the time. The Ag atom is in a virtually linear geometry defined by two N atoms derived from the bdc and bdcH ligands. The three-dimensional supramolecular structure is stablized by extensive O—H...O and N—H...O hydrogen bonds. An intramolecular O—H...O hydrogen bond is also present.

  2. 2-Methyl-6-(6-methyl-1H-benzimidazol-2-ylphenol–2-methyl-6-(5-methyl-1H-benzimidazol-2-ylphenol (3/1

    Suchada Chantrapromma

    2009-12-01

    Full Text Available The title compound, 0.75C15H14N2O·0.25C15H14N2O, is a co-crystal of 2-methyl-6-(6-methyl-1H-benzimidazol-2-ylphenol as the major component and 2-methyl-6-(5-methyl-1H-benzimidazol-2-ylphenol as the minor component. The refined site-occupancy ratio is 0.746 (4/0.254 (4. The conformations of both components are identical except for that of the methyl substituent on the benzene ring of the benzimidazole unit which is positionally disordered over two positions. The molecule is essentially planar, the dihedral angle between the benzimidazole plane and the benzene ring being 3.49 (4°. An intramolecular O—H...N hydrogen bond generates an S(6 ring motif. In the crystal packing, molecules are linked through N—H...O hydrogen bonds into chains along [201]. These chains are stacked approximately along the a-axis direction. The crystal packing is further stabilized by weak N—H...O and O...H...N hydrogen bonds, together with weak intermolecular C—H...π interactions. A π–π interaction with a centroid–centroid distance of 3.6241 (6 Å is also observed between the substituted phenyl ring and that of the benzimidazole system.

  3. 40 CFR 721.9078 - 6-Methoxy-1H-benz[de]isoquinoline-2 [3H]-dione derivative (generic).

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false 6-Methoxy-1H-benz isoquinoline-2... New Uses for Specific Chemical Substances § 721.9078 6-Methoxy-1H-benz isoquinoline-2 -dione... substance identified generically as 6-methoxy-1H-benz isoquinoline-2 -dione derivative (PMN P-00-1205)...

  4. 32 CFR 1630.15 - Class 1-H: Registrant not subject to processing for induction.

    2010-07-01

    ... for induction. 1630.15 Section 1630.15 National Defense Other Regulations Relating to National Defense... induction. In Class 1-H shall be placed any registrant who is not eligible for Class 1-A and is not currently subject to processing for induction....

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

    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. PMID:25241007

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

    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.

  7. Structural analysis of the carbohydrate chains of glycoproteins by 500-MHz 1H-NMR spectroscopy

    This thesis deals with the structural analysis by 500-MHz 1H-NMR spectroscopy of carbohydrate chains obtained from glycoproteins. In the chapters 1 to 6 the structural analysis of N-glycosidically linked carbohydrate chains is described. The chapters 7 to 10 describe the structural analysis of O-glycosidically linked carbohydrate chains. 381 refs.; 44 figs.; 24 tabs.; 7 schemes

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

    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.

  9. 4-Amino-1H-1,2,4-triazol-1-ium nitrate

    Matulková, Irena; Císařová, I.; Němec, A.

    2011-01-01

    Roč. 67, DEC 2011 (2011), O18-U1473. ISSN 1600-5368 Institutional research plan: CEZ:AV0Z40400503 Keywords : ligands * 4-Amino-1H-1,2,4-triazol-1-ium nitrate * complexes Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 0.347, year: 2011

  10. Mutation screen reveals novel variants and expands the phenotypes associated with DYNC1H1.

    Strickland, Alleene V; Schabhüttl, Maria; Offenbacher, Hans; Synofzik, Matthis; Hauser, Natalie S; Brunner-Krainz, Michaela; Gruber-Sedlmayr, Ursula; Moore, Steven A; Windhager, Reinhard; Bender, Benjamin; Harms, Matthew; Klebe, Stephan; Young, Peter; Kennerson, Marina; Garcia, Avencia Sanchez Mejias; Gonzalez, Michael A; Züchner, Stephan; Schule, Rebecca; Shy, Michael E; Auer-Grumbach, Michaela

    2015-09-01

    Dynein, cytoplasmic 1, heavy chain 1 (DYNC1H1) encodes a necessary subunit of the cytoplasmic dynein complex, which traffics cargo along microtubules. Dominant DYNC1H1 mutations are implicated in neural diseases, including spinal muscular atrophy with lower extremity dominance (SMA-LED), intellectual disability with neuronal migration defects, malformations of cortical development, and Charcot-Marie-Tooth disease, type 2O. We hypothesized that additional variants could be found in these and novel motoneuron and related diseases. Therefore, we analyzed our database of 1024 whole exome sequencing samples of motoneuron and related diseases for novel single nucleotide variations. We filtered these results for significant variants, which were further screened using segregation analysis in available family members. Analysis revealed six novel, rare, and highly conserved variants. Three of these are likely pathogenic and encompass a broad phenotypic spectrum with distinct disease clusters. Our findings suggest that DYNC1H1 variants can cause not only lower, but also upper motor neuron disease. It thus adds DYNC1H1 to the growing list of spastic paraplegia related genes in microtubule-dependent motor protein pathways. PMID:26100331

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

    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. 1H NMR determination of urinary betaine in patients with premature vascular disease and mild homocysteinemia.

    Lundberg, P; Dudman, N P; Kuchel, P W; Wilcken, D E

    1995-02-01

    Urinary N,N,N-trimethylglycine (betaine) and N,N-dimethylglycine (DMG) have been identified and quantified for clinical purposes by proton nuclear magnetic resonance (1H NMR) measurement in previous studies. We have assessed these procedures by using both one-dimensional (1-D) and 2-D NMR spectroscopy, together with pH titration of urinary extracts to help assign 1H NMR spectral peaks. The betaine calibration curve linearity was excellent (r = 0.997, P = 0.0001) over the concentration range 0.2-1.2 mmol/L, and CVs for replicate betaine analyses ranged from 7% (n = 10) at the lowest concentration to 1% (n = 9) at the highest. The detection limit for betaine was < 15 mumol/L. Urinary DMG concentrations were substantially lower than those of betaine. Urinary betaine and DMG concentrations measured by 1H NMR spectroscopy from 13 patients with premature vascular disease and 17 normal controls provided clinically pertinent data. We conclude that 1H NMR provides unique advantages as a research tool for determination of urinary betaine and DMG concentrations. PMID:7533065

  13. Scalable synthesis of quaterrylene: solution-phase 1H NMR spectroscopy of its oxidative dication.

    Thamatam, Rajesh; Skraba, Sarah L; Johnson, Richard P

    2013-10-14

    Quaterrylene is prepared in a single reaction and high yield by Scholl-type coupling of perylene, utilizing trifluoromethanesulfonic acid as catalyst and DDQ or molecular oxygen as oxidant. Dissolution in 1 M triflic acid/dichloroethane with sonication yields the aromatic quaterrylene oxidative dication, which is characterized by its (1)H NMR spectrum. PMID:23999880

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

    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

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

    In two trimethylsilyl-substituted 1H-benzimidazole-2(3H)-thiones, noncovalent C—H⋯π interactions between the centroid of the benzmidazole system and the SiMe3 groups form helicoidal arrangements in one, and dimerization results in the formation of Rs 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, C13H22N2SSi2, (2), and 1-trimethylsilyl-1H-benzimidazole-2(3H)-thione, C10H14N2SSi, (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 SiMe3 groups form helicoidal arrangements in (2). Dimerization of (3) results in the formation of R22(8) rings via N—H⋯S interactions, along with parallel π–π interactions between imidazole and benzene rings

  16. Suppression of baseline artifacts in 1H NMR spectroscopy of diluted water solutions

    Suppression of baseline artifacts in 1H NMR spectroscopy of diluted aqueous solutions has been discussed. The time-domain technique capable of eliminating or lowering the baseline distortions in the spectra caused by the ringing of low pas filters has been proposed. Simultaneously, the problem of proper adjusting of the start of data acquisition have been discussed

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

    Wang, Qiang; Li, Xingwei

    2016-05-01

    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. PMID:27082502

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

    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.

  19. Electron spray ionization mass spectrometry and 2D {sup 31}P NMR for monitoring {sup 18}O/{sup 16}O isotope exchange and turnover rates of metabolic oligophosphates

    Nemutlu, Emirhan [Mayo Clinic, Division of Cardiovascular Diseases, Department of Medicine, Rochester, MN (United States); University of Hacettepe, Department of Analytical Chemistry, Faculty of Pharmacy, Ankara (Turkey); Juranic, Nenad; Macura, Slobodan [Mayo Clinic, Department of Biochemistry and Molecular Biology, Rochester, MN (United States); Mayo Clinic, Analytical NMR Core Facility, Rochester, MN (United States); Zhang, Song; Terzic, Andre; Dzeja, Petras P. [Mayo Clinic, Division of Cardiovascular Diseases, Department of Medicine, Rochester, MN (United States); Ward, Lawrence E. [Mayo Clinic, CTSA Metabolomic Core Facility, Rochester, MN (United States); Dutta, Tumpa; Nair, K.S. [Mayo Clinic, CTSA Metabolomic Core Facility, Rochester, MN (United States); Mayo Clinic, Division of Endocrinology and Endocrine Research Unit, Rochester, MN (United States)

    2012-05-15

    A new method was here developed for the determination of {sup 18}O-labeling ratios in metabolic oligophosphates, such as ATP, at different phosphoryl moieties ({alpha}-, {beta}-, and {gamma}-ATP) using sensitive and rapid electrospray ionization mass spectrometry (ESI-MS). The ESI-MS-based method for monitoring of {sup 18}O/{sup 16}O exchange was validated with gas chromatography-mass spectrometry and 2D {sup 31}P NMR correlation spectroscopy, the current standard methods in labeling studies. Significant correlation was found between isotopomer selective 2D {sup 31}P NMR spectroscopy and isotopomer less selective ESI-MS method. Results demonstrate that ESI-MS provides a robust analytical platform for simultaneous determination of levels, {sup 18}O-labeling kinetics and turnover rates of {alpha}-, {beta}-, and {gamma}-phosphoryls in ATP molecule. Such method is advantageous for large scale dynamic phosphometabolomic profiling of metabolic networks and acquiring information on the status of probed cellular energetic system. (orig.)

  20. Multiple Antiferromagnetic Spin Fluctuations and Novel Evolution of Tc in Iron-Based Superconductors LaFe(As1‑xPx)(O1‑yFy) Revealed by 31P-NMR Studies

    Shiota, Takayoshi; Mukuda, Hidekazu; Uekubo, Masahiro; Engetsu, Fuko; Yashima, Mitsuharu; Kitaoka, Yoshio; Lai, Kwing To; Usui, Hidetomo; Kuroki, Kazuhiko; Miyasaka, Shigeki; Tajima, Setsuko

    2016-05-01

    We report on 31P-NMR studies of LaFe(As1‑xPx)(O1‑yFy) over wide compositions for 0 ≤ x ≤ 1 and 0 ≤ y ≤ 0.14, which provide clear evidence that antiferromagnetic spin fluctuations (AFMSFs) are one of the indispensable elements for enhancing Tc. Systematic 31P-NMR measurements revealed two types of AFMSFs in the temperature evolution, that is, one is the AFMSFs that develop rapidly down to Tc with low-energy characteristics, and the other, with relatively higher energy than the former, develops gradually upon cooling from high temperature. The low-energy AFMSFs in low y (electron doping) over a wide x (pnictogen height suppression) range are associated with the two orbitals of dxz/yz, whereas the higher-energy ones for a wide y region around low x originate from the three orbitals of dxy and dxz/yz. We remark that the nonmonotonic variation of Tc as a function of x and y in LaFe(As1‑xPx)(O1‑yFy) is attributed to these multiple AFMSFs originating from degenerated multiple 3d orbitals inherent to Fe-pnictide superconductors.

  1. Antitumor activity of intratumoral injection of pcDNA3.1-p27Kip1mt followed by in vivo electroporation in a malignant Burkitt’s lymphoma cell xenograft

    Supriatno Supriatno

    2012-12-01

    Full Text Available Background: Human malignant Burkitt’s lymphomas are an uncommon type of Non-Hodgkin Lymphoma commonly affects in children. It is a highly aggressive type of B-cell lymphoma. Treatment for this malignant are still limited. However, a new strategy for refractory cancer, gene therapy is watched with keen interest. Recently, a novel method for high-efficiency and region-controlled in vivo gene transfer was developed by combining in vivo electroporation and plasmid cDNA. In the present study, a non-viral gene transfer system, in vivo electroporation in human malignant Burkitt’s lymphoma (Raji cell xenograft was investigated. Purpose: The purpose of this study was to evaluate p27Kip1 gene therapy in Raji cell xenografts using pcDNA3.1-p27Kip1 mutant type (mt and pcDNA3.1 empty vector (neo with the local application of electric pulses. Methods: True experimental study using post-intervention with control group design was performed in this study. Material sample was obtained from integrated research laboratory at faculty of dentistry, Universitas Gadjah Mada, Yogyakarta. The efficiency of transfection of exogenous p27Kip1 gene by electroporation was confirmed by Western bloting analysis. To evaluate the reduction of malignant Burkitt’s lymphoma cell xenografts by this method, the volume of Raji cell xenografts in mice after electroporation with p27Kip1 mt or neo gene was measured. Results: Up-regulation of p27Kip1 protein was detected in pcDNA3.1-p27Kip1 mt. Furthermore, the growth of tumors was markedly suppressed by p27Kip1 mt gene transfection compared with transfection of neo. Conclusion: Injection of pcDNA3.1-p27Kip1 mt gene followed by in vivo electroporation has a high-potentially to suppress the growth of malignant Burkitt’s lymphoma cells. Furthermore, combination system of pcDNA3.1-p27Kip1 mt-injected tumor and electroporation might be used for human oral cancer. Latar belakang: Limfoma Burkitt’s maligna banyak terjadi pada anak-anak dan merupakan jenis yang langka dari limfoma NonHodgkin (NHL. Limfoma Burkitt’s maligna adalah tipe yang sangat agresif dari limfoma sel B. Perawatan penyakit ini masih sangatterbatas, walaupun demikian strategi baru perawatan kanker menggunakan terapi gen menjadi pusat perhatian. Suatu metode baru transfer gen untuk meningkatkan efisiensi dan kontrol area telah dikembangkan dengan mengkombinasi elektroporasi in vivo dan plasmid cDNA. Pada penelitian ini, telah diteliti sistim transfer gen non-virus dengan elektroporasi in vivo terhadap xenograft sel limfoma Burkitt’s maligna (sel Raji. Tujuan: Tujuan dari penelitian ini adalah untuk mengevaluasi terapi gen p27Kip1 terhadap xenograft sel Raji menggunakan pcDNA3.1-p27Kip1 mutant type (mt dan pcDNA3.1 empty vector (neo dengan aplikasi lokal elektroporasi. Metode: Jenis penelitian yang digunakan adalah eksperimen murni memakai rancangan pasca intervensi dengan kelompok kontrol. Sampel dan bahan penelitian didapat dari laboratorium riset terpadu, Fakultas Kedokteran Gigi, Universitas Gadjah Mada, Yogyakarta. Efisiensi transfeksi gen p27Kip1eksogen dengan elektroporasi dilakukan dengan analisis Western bloting. Untuk mengevaluasi hambatan xenograft sel limfoma Burkitt’s maligna dengan metode elektroporasi, dilakukan pengukuran volume xenograft sel Raji pada tikus pasca elektroporasi dan injeksi gen p27Kip1 mt atau neo. Hasil: Peningkatan regulasi protein p27Kip1 terdeteksi pada gen pcDNA3.1-p27Kip1 mt. Selanjutnya, pertumbuhan tumor secara signifikan terhambat oleh transfeksi gen p27Kip1 mt dibandingkan dengan transfeksi neo. Kesimpulan: Injeksi gen pcDNA3.1-p27Kip1 mt disertai elektroporasi in vivo mempunyai potensi yang kuat menghambat pertumbuhan "> sel limfoma Burkitt’s maligna. Kombinasi sistim injeksi tumor menggunakan gen pcDNA3.1-p27Kip1 mt dan elektroporasi kemungkinan dapat digunakan untuk terapi kanker oral.

  2. 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.

    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]. PMID:27375869

  3. 1H-MR spectroscopy study in amyotrophic lateral sclerosis%肌萎缩侧索硬化症的~1H-MR波谱研究

    韩静; 马林; 于生元

    2009-01-01

    Objective To characterize the features of proton magnetic resonance spectroscopy (1H-MRS)on amyotrophic lateral sclerosis(ALS)and its correlations with clinical scale.Methods Fifteen patienta with definite or probable ALS and 15 age and gender matched normal controls were enrolled.1H-MRS was performed on a 3.0 T GE imaging system(GE Medical System,Milwaukee,Wisconsin,USA).TE-averaged point resolved selective spectroscopy was used.N-acetylaspartate(NAA),creatine (Cr).Gh and Glx(glutamate+glutamine)values of subcortical motor area and posterior limb of the intemal capsule were acquired,t teat was used to compare differencea between groups,the correlations between the above valuea and clinical scale were analyzed.Results The motor area and posterior limb of the internal capsule in ALS patients had significantly lower NAA/Cr(1.91±0.34,1.53±0.17)compared with normal subjects(2.23±0.33,1.66±0.07)(t=4.25,2.90,P=0.00,0.01).ALS patients had significantly higher Glu/Cr(0.34±0.05,0.29±0.06)and Glx/Cr(0.40±0.04,0.33±0.06),compared with normal subjects(0.30±0.03,0.25±0.04)and(0.32±0.05,0.26±0.03)(t=2.56,2.40.7.34.5.30,P=0.02,0.03,0.00,0.00).The Norris scale of ALS patients were 57±8,ALSFRS were 29±4.The Norris scale was negatively correlated with Glx/Cr of primary motor cortex by lineal correlation analysis(r=-0.75,P=0.00),while ALSFRS had no correlation with GK/Cr.Conclusions Neuronal loss and Glu+Gln increase can be detected by using proton MRS in ALS patients.(1)H-MRS is an useful tool in reflecting the characteristic changes of metabolite in ALS.%目的 探讨肌萎缩侧索硬化症(ALS)患者的1H-MRS表现及其与临床评分的关系.方法 对15例临床确诊及拟诊为ALS的患者(ALS组)和15名年龄相匹配的健康志愿者(对照组)进行1H-MRS扫描,采用单体素平均TE选择性单点分辨波谱序列(TE-Averaged PRESS).扫描图像经后处理,分别获得以中央前回为中心的运动皮层和内囊后肢处的以下成分波峰:N-

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

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

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

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

    2009-07-15

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

  6. Quantitative analysis of sugars in wood hydrolyzates with 1H NMR during the autohydrolysis of hardwoods.

    Mittal, Ashutosh; Scott, Gary M; Amidon, Thomas E; Kiemle, David J; Stipanovic, Arthur J

    2009-12-01

    The focus of this work was to determine the utility of (1)H NMR spectroscopy in the quantification of sugars resulting from the solubilization of hemicelluloses during the autohydrolysis of hardwoods and the use of this technique to evaluate the kinetics of this process over a range of temperatures and times. Yields of residual xylan, xylooligomers, xylose, glucose, and the degraded products of sugars, i.e., furfural and HMF (5-hydroxymethyl furfural), were determined. The monosaccharide and oligomer contents were quantified with a recently developed high resolution (1)H NMR spectroscopic analysis. This method provided precise measurement of the residual xylan and cellulose remaining in the extracted wood samples and xylose and glucose in the hydrolyzates. NMR was found to exhibit good repeatability and provided carbohydrate compositional results comparable to published methods for sugar maple and aspen woods. PMID:19674893

  7. 1H MAS NMR spectra of hy- droxyl species on diatomite surface

    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.

  8. Localized 1hω particle-hole strength in nuclei

    A cross section enhancement, persisting to high momentum transfer, has been observed around 1hω in excitation energy in spectra from inelastic proton-, alpha- and electron scattering on 90Zr, 116Sn, 196Pt and 208Pb. Data are presented for (p,p') at 201 MeV, (α,α') at 120 MeV and analyzed together with existing data obtained with 133.8 MeV polarized ( vector p,p') on 116Sn and electron-scattering data on 116Sn and 196Pt. Two different interpretations of the observed enhancement are discussed: that of the incoherent sum of all 1hω cross section and alternatively the sum over the isoscalar normal modes of all multipolarities. ((orig.))

  9. Localized 1h{omega} particle-hole strength in nuclei

    Hofstee, M.A. [Rijksuniversiteit Groningen (Netherlands). Kernfysisch Versneller Inst.; Werf, S.Y. van der [Rijksuniversiteit Groningen (Netherlands). Kernfysisch Versneller Inst.; Berg, A.M. van den [Rijksuniversiteit Groningen (Netherlands). Kernfysisch Versneller Inst.; Blasi, N. [Dipartimento di Fisica dell` Universita and INFN, Sezione di Milano, I-20133 Milano (Italy); Bordewijk, J.A. [Rijksuniversiteit Groningen (Netherlands). Kernfysisch Versneller Inst.; Borghols, W.T.A. [National Institute for Nuclear Physics and High-Energy Physics, Section K, P.O. Box 41882, 1009 DB Amsterdam (Netherlands); De Leo, R. [Dipartimento di Fisica dell` Universita and INFN, Sezione di Bari, I-70126 Bari (Italy); Emery, G.T. [Department of Physics, Bowdoin College, Brunswick, ME 04011, USA, and Indiana University Cyclotron Facility, Bloomington, IN 47408 (United States); Fortier, S. [Institut de Physique Nucleaire, Orsay (France); Gales, S. [Institut de Physique Nucleaire, Orsay (France); Harakeh, M.N. [Rijksuniversiteit Groningen (Netherlands). Kernfysisch Versneller Inst.; Heijer, P. den [National Institute for Nuclear Physics and High-Energy Physics, Section K, P.O. Box 41882, 1009 DB Amsterdam (Netherlands); Jager, C.W. de [National Institute for Nuclear Physics and High-Energy Physics, Section K, P.O. Box 41882, 1009 DB Amsterdam (Netherlands); Langevin-Joliot, H. [Institut de Physique Nucleaire, Orsay (France); Micheletti, S. [Dipartimento di Fisica dell` Universita and INFN, Sezione di Milano, I-20133 Milano (Italy); Morlet, M. [Institut de Physique Nucleaire, Orsay (France); Pignanelli, M. [Dipartimento di Fisica dell` Universita and INFN, Sezione di Milano, I-20133 Milano (Italy); Schippers, J.M. [Rijksuniversiteit Groningen (Netherlands). Kernfysisch Versneller Inst.; Vries, R. de [National Institute for Nuclear Physics and High-Energy Physics, Section K, P.O. Box 41882, 1009 DB Amsterdam (Netherlands); Willis, A.

    1995-06-12

    A cross section enhancement, persisting to high momentum transfer, has been observed around 1h{omega} in excitation energy in spectra from inelastic proton-, alpha- and electron scattering on {sup 90}Zr, {sup 116}Sn, {sup 196}Pt and {sup 208}Pb. Data are presented for (p,p`) at 201 MeV, ({alpha},{alpha}`) at 120 MeV and analyzed together with existing data obtained with 133.8 MeV polarized ( vector p,p`) on {sup 116}Sn and electron-scattering data on {sup 116}Sn and {sup 196}Pt. Two different interpretations of the observed enhancement are discussed: that of the incoherent sum of all 1h{omega} cross section and alternatively the sum over the isoscalar normal modes of all multipolarities. ((orig.)).

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

    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)

  11. (1)H-NMR-based discrimination of thermal and vinegar treated ginseng roots.

    Kim, So-Hyun; Hyun, Sun-Hee; Yang, Seung-Ok; Choi, Hyung-Kyoon; Lee, Boo-Yong

    2010-08-01

    To investigate the changes in nonvolatile metabolites of thermal and/or vinegar treated ginseng (TVG), samples prepared using various treatment conditions were analyzed using an (1)H-NMR-based metabolomics technique. The processing conditions of the ginseng in this study were 100, 140, and 180 degrees C with and without vinegar and the duration of exposure to each temperature was 10, 30, and 50 min, respectively. There was a clear separation in the score plots among various treatment conditions. Major compounds contributing to the separation of 50% methanol extracts of TVG with various process conditions were valine, lactate, alanine, arginine, glucose, fructose, and sucrose. As temperature increased, valine, arginine, glucose, fructose, and sucrose concentrations decreased, whereas lactate, glucose, and fructose increased in the vinegar-treated samples compared to non-vinegar-treated samples. The present study suggests the usefulness of an (1)H-NMR-based metabolomics approach to discriminate TVG samples, subjected to different processing conditions. PMID:20722913

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

    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. PMID:26295174

  13. Direct detection of solanesol in tobacco by 1H and 13C magic angle spinning NMR

    1H and 13C NMR have been used to detect solanesol directly in tobacco without destroying or modifying the sample. Magic angle sample spinning was employed to remove the resonance line broadening due to variations of magnetic susceptibility within the sample. 13C line widths of ca . 10 Hz were obtained. The 1H MAS spectrum of tobacco allows the solanesol signals to be resolved from the broad signal of exchangeable protons. 13C spin-lattice relaxation times (T3) and nuclear Overhauser enhancements (NOE) of solanesol in chloroform solution, in intact tobacco, and as nest oil indicate that the polyisoprene chain motion in tobacco is restricted relative to the motion in solution but still sufficient to average out the dipolar couplings between protons and carbons. (author)

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

    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...

  15. Dangling-bond logic gates on a Si(100)-(2 × 1)-H surface

    Atomic-scale Boolean logic gates (LGs) with two inputs and one output (i.e. OR, NOR, AND, NAND) were designed on a Si(100)-(2 × 1)-H surface and connected to the macroscopic scale by metallic nano-pads physisorbed on the Si(100)-(2 × 1)-H surface. The logic inputs are provided by saturating and unsaturating two surface Si dangling bonds, which can, for example, be achieved by adding and extracting two hydrogen atoms per input. Quantum circuit design rules together with semi-empirical elastic-scattering quantum chemistry transport calculations were used to determine the output current intensity of the proposed switches and LGs when they are interconnected to the metallic nano-pads by surface atomic-scale wires. Our calculations demonstrate that the proposed devices can reach ON/OFF ratios of up to 2000 for a running current in the 10 µA range. (paper)

  16. 1H chemical shift imaging characterization of human brain tumor and edema

    Longitudinal (T1) and transverse (T2) relaxation times of metabolites in human brain tumor, peritumoral edema, and unaffected brain tissue were assessed from point resolved spectroscopy (PRESS) 1H chemical shift imaging results at different repetition times (TR=1500 and 5000 ms; T1: n=19) and echo times (TE=135 and 270 ms; T2: n=7). Metabolite T1 and T2 relaxation times in unaffected brain tissue corresponded with those published for healthy volunteers. T2 relaxation times were reduced in tumor (choline, N-acetyl aspartate) and edema (choline, creatine) compared with unaffected brain tissue (p1H chemical shift imaging is most suited in the use of choline elevation as tumor marker. (orig.)

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

    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). PMID:25466103

  18. Preliminary study of 3T 1H MR spectroscopy in bone and soft tissue tumors

    QI Zi-hua; LI Chuan-fu; LI Zhen-feng; ZHANG Kai; WANG Qian; YU De-xin

    2009-01-01

    Background Magnetic resonance spectroscopy (MRS) is one method that can examine noninvasively the alive specimen of the organ, metabolism of the organ and cell, and the biochemistry change. MRS provides the biochemistry information that may be used to diagnose tumors or differentiate the malignant tumor from benign. The objective of this study is to investigate the benign and malignant bone and soft tissue tumors by 1H-MR spectroscopy (1H-MRS) on a 3 Tesla MR scanner, then to assess the usefulness of 'H-MRS in diagnosing bone and soft tissue tumors and distinguishing benign from malignant tumors. Methods Fifty-six patients with bone and soft tissue tumors proved clinically and pathologically were examined with 1H-MRS. 1H-MRS was performed to study malignant musculoskeletal tumors, benign tumors and normal muscle adjacent to lesions to analyze the characteristics, and single-voxel point-resolved spectroscopy sequence was used. Proton brain exam-single voxel of 1H-MRS which directly appeared in the spectrum, was observed to find the peak height of choline compounds (Cho) opposite to the creatine (Cr), and whether there was a Cho peak. Metabolite values were calculated automatically from the area under each metabolite peak by the Functool 3.1 software. Metabolite ratios of Cho/Cr were manually calculated. Then according to the results, it was judged whether there existed benign or malignant tumors. The Kappa statistical test was used to analyze the MRS results, the histopathology data and the surgical situation. Statistics processing was performed using the software package SPSS11.5 for Windows. Results1H-MRS spectra style of bone and soft tissue tumors was different from that of normal muscle, and differences also existed between benign and malignant tumors. Choline level in malignant tumor was markedly higher than that in benign tumors. Cho/Cr in malignant tumor was higher than in benign tumor significantly (P<0.05). The true positive rate of bone and soft tissue

  19. Nonvortical Rashba Spin Structure on a Surface with C_{1h} Symmetry.

    Annese, Emilia; Kuzumaki, Takuya; Müller, Beate; Yamamoto, Yuta; Nakano, Hiroto; Kato, Haruki; Araki, Atsushi; Ohtaka, Minoru; Aoki, Takashi; Ishikawa, Hirotaka; Hayashida, Takashi; Osiecki, Jacek R; Miyamoto, Koji; Takeichi, Yasuo; Harasawa, Ayumi; Yaji, Koichiro; Shirasawa, Tetsuroh; Nittoh, Koh-Ichi; Yang, Wooil; Miki, Kazushi; Oda, Tatsuki; Yeom, Han Woong; Sakamoto, Kazuyuki

    2016-07-01

    A totally anisotropic peculiar Rashba-Bychkov (RB) splitting of electronic bands was found on the Tl/Si(110)-(1×1) surface with C_{1h} symmetry by angle- and spin-resolved photoelectron spectroscopy and first-principles theoretical calculation. The constant energy contour of the upper branch of the RB split band has a warped elliptical shape centered at a k point located between Γ[over ¯] and the edge of the surface Brillouin zone, i.e., at a point without time-reversal symmetry. The spin-polarization vector of this state is in-plane and points almost the same direction along the whole elliptic contour. This novel nonvortical RB spin structure is confirmed as a general phenomenon originating from the C_{1h} symmetry of the surface. PMID:27419582

  20. Nonvortical Rashba Spin Structure on a Surface with C1 h Symmetry

    Annese, Emilia; Kuzumaki, Takuya; Müller, Beate; Yamamoto, Yuta; Nakano, Hiroto; Kato, Haruki; Araki, Atsushi; Ohtaka, Minoru; Aoki, Takashi; Ishikawa, Hirotaka; Hayashida, Takashi; Osiecki, Jacek R.; Miyamoto, Koji; Takeichi, Yasuo; Harasawa, Ayumi; Yaji, Koichiro; Shirasawa, Tetsuroh; Nittoh, Koh-ichi; Yang, Wooil; Miki, Kazushi; Oda, Tatsuki; Yeom, Han Woong; Sakamoto, Kazuyuki

    2016-07-01

    A totally anisotropic peculiar Rashba-Bychkov (RB) splitting of electronic bands was found on the Tl /Si (110 )-(1 ×1 ) surface with C1 h symmetry by angle- and spin-resolved photoelectron spectroscopy and first-principles theoretical calculation. The constant energy contour of the upper branch of the RB split band has a warped elliptical shape centered at a k point located between Γ ¯ and the edge of the surface Brillouin zone, i.e., at a point without time-reversal symmetry. The spin-polarization vector of this state is in-plane and points almost the same direction along the whole elliptic contour. This novel nonvortical RB spin structure is confirmed as a general phenomenon originating from the C1 h symmetry of the surface.

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

    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.

  2. Applications of 1H-NMR relaxometry in experimental liver studies

    Purpose of this study was to investigate applications of proton nuclear magnetic resonance (1H-NMR) relaxometry in experimental medicine. Relaxometry was performed by measurements of spin-lattice (T1) and spin-spin (T2) relaxation time parameters on liver biopsies up to four hours after biopsy excision. Variations of relaxation times due to species and strain, different sample handling and different liver damage models, ethionine fatty liver and paracetamol liver necrosis, were investigated. Cell integrity effects were studied on homogenized liver samples. Relaxation time parameters, especially 'main' components T1A and T2A of biexponential model fit, were identified to react very sensitive after tissue damages as well as to cell viability. Thus, investigation of stored liver grafts was performed in order to evaluate the possibility of a rapid liver graft viability testing method for human liver transplantation surgery by 1H-NMR relaxometry. Another series of measurements was performed to investigate the applicability of isoflurane anesthesia for in vivo NMR experiments. This study proved the good appropriateness of isoflurane for that purpose provided that physiological monitoring and individual adjustment of anesthesia are performed. In these investigations it could be revealed that mainly T1A and T2A are influenced by tissue condition and that different information is inherent in these two parameters, with T2A reflecting tissue viability and changes of tissue conditions very sensitively but rather unspecifically in respect to the damage applied. Based on these results the following future applications of 1H-NMR relaxometry are suggested : (1) model investigations, (2) investigation of given pathologies, (3) investigation of basic requirements for in vivo NMR and (4) application in a liver graft viability testing protocol, which seems to be the most important future application of 1H-NMR relaxometry in medicine. (author)

  3. 23Na and 1H NMR studies on melittin channels activated by tricyclic tranquilizers.

    Tanaka, H.; Matsunaga, K.; Kawazura, H

    1992-01-01

    A dynamic 23Na nuclear magnetic resonance (NMR) technique was applied to the exchange system of Na+ ions present inside and outside large unilamellar vesicles at an equivalent concentration. Addition of melittin to phosphatidylcholine vesicles did not induce any detectable Na+ transport across the membrane but subsequent addition of a trace of chlorpromazine or imipramine did induce Na+ transport. Because the formation of a drug-melittin adduct in a solution was detected by 1H NMR, the activa...

  4. 5,5′-(Butane-1,4-diylbis(1H-tetrazole dihydrate

    Jian-Hua Xin

    2010-12-01

    Full Text Available The title compound, C6H10N8·2H2O, was prepared by the reaction of hexanedinitrile and sodium azide. The di-1H-tetrazole molecule lies on a crystallographic centre of inversion and is linked to the water molecules by N—H...O and O—H...N hydrogen bonds, forming a two-dimensional supramolecular structure in the crystal.

  5. 1H NMR spectroscopic determination of deterioration marker compounds in fats and oils

    Skiera, Christina

    2013-01-01

    In food and pharmaceutical analysis, the classical indices peroxide value (PV), acid value (AV) and p-anisidine value (ANV) still play an important role as quality and authenticity control parameters of fats and oils. These indices are sum parameters for certain deterioration products (PV for hydroperoxides, AV for free fatty acids, ANV for aldehydes) and are obtained using volumetric or UV/VIS spectroscopic analytical approaches. 1H NMR spectroscopy provides a fast and simple alternative to ...

  6. (2-Chlorophenyl-3-methylchromeno[2,3-c]pyrazol-4(1H-one

    Wolfgang Holzer

    2010-03-01

    Full Text Available The title compound was prepared by treatment of 1-(2-chlorophenyl-3-methyl-2-pyrazolin-5-one with 2-chlorobenzoyl chloride / Ca(OH2 in 1,4-dioxane and subsequent cyclization of the thus obtained 4-aroyl-5-hydroxypyrazole with sodium hydride in dry DMF. Detailed spectroscopic data (1H NMR, 13C NMR, 15N NMR, IR, MS are presented.

  7. 3-Methyl-1-phenyl-1H-pyrazol-5-yl 2-Bromo-3-furan-carboxylate

    Karin Schalle

    2009-07-01

    Full Text Available The reaction of 3-methyl-1-phenyl-2-pyrazolin-5-one and 2-bromo-3-furoyl chloride in the presence of Ca(OH2 in 1,4-dioxane gave the title compound. The latter was also obtained in much higher yield upon reaction of the starting materials in the system dichloromethane / triethylamine. Detailed spectroscopic data (1H NMR, 13C NMR, 15N NMR, IR, MS are presented.

  8. 1H MRS spectroscopy in brain tumors - in search of the highest efficacy

    Many thousands of published papers, a lot of communications and daily practice show the outstanding role of proton spectroscopy (1H MRS) in neurooncology. Paradoxically, in several clinical centres (neurosurgery ones) we can observe the lack of full acceptance of the reliability of this method. Presumably, the reason for this attitude lies in non-uniform methodology and quite superficial treatment of spectroscopic results. At the beginning of this paper, we would like to stress that fortunately, there is a certain number of publications which order criteria of tumor's malignancy, its tissue characterisation and the degree of malignancy. In this paper we intend to point out the proper ways of improving reliability of 1H MRS in brain tumor diagnosis. Obviously, the quality of spectroscopic exams is influenced by methodology and manner of result interpretation (e.g. just simple visual inspection of MRS spectra is not sufficient for correct diagnosis). Currently, imaging diagnosis of brain tumors is based on many modalities (DTI, perfusion CT, MR, PET, SPECT) which are sufficiently effective in detection and differentiation of the lesions; in this context, we can say that 1H MRS spectroscopy constitutes the element of multimodal diagnostic approach for brain tumors. Nevertheless, the current papers concerning MR spectroscopy stress its significant role in making therapeutic decision, particularly as an alternative for surgery treatment and solution of the recurrence of tumor or/and extent of the tumor's spreading. Over 15 years of experience with 1H MRS in diagnosis of brain tumors convinced us that these methods have very high diagnostic and decision-making value provided that it is properly applied and interpreted correctly. It is also important to choose the statistic methods that will show the best discriminators (markers) for particular pathologies. Authors' intention is to recommend the best ways to form the right diagnosis considering technological requirements

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

    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)

  10. 1H NMR study of thermotropic phase transition in aqueous polymer solutions

    Spěváček, Jiří; Hanyková, L.

    Poznan : Adam Mickiewicz University, Poznan, 2002 - (Garsztka, M.; Pisula, D.; Wegorowska, W.). s. 237 [Congress AMPERE: Magnetic Resonance and Related Phenomena /31./. 15.07.2002-19.07.2002, Poznan] R&D Projects: GA AV ČR KSK4050111 Grant ostatní: GA UK(CZ) 164/20B Keywords : 1H NMR * thermotropic phase transition * poly(vinyl methyl ether)/D2O solutions Subject RIV: CD - Macromolecular Chemistry

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

    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.

  12. Synthese und pharmakologische Charakterisierung dualer Histamin-H1-/H4-Rezeptorliganden

    Wagner, Eva

    2012-01-01

    Im Rahmen dieses Promotionsprojektes sollten duale H1-/H4-Rezeptor-Antagonisten entwickelt werden. Der im Jahr 2000 entdeckte H4-Rezeptor spielt wie der H1-Rezeptor eine Rolle in der Pathogenese von allergischen Krankheiten[1]. Ausschlaggebend für diese Arbeit waren die Ergebnisse der Neumann-Forschungsgruppe[2]: es wurde gezeigt, dass die kombinierte Gabe von H1-Rezeptorantagonist (Mepyramin) und H4-Rezeptorantagonist (JNJ7777120) zu einem synergistischen Effekt im akuten murinen Asthm...

  13. Metabonomic signature analysis of cervical carcinoma and precancerous lesions in women by 1H NMR spectroscopy

    Hasim, Ayshamgul; ALI, MAYINUER; MAMTIMIN, BATUR; Ma, Jun-Qi; Li, Qiao-Zhi; ABUDULA, ABULIZI

    2012-01-01

    1H nuclear magnetic resonance (NMR)-based metabonomics has been used to characterize the metabolic profiles of cervical intraepithelial neoplasia (CIN) and cervical squamous cell carcinoma (CSCC). Principal component analysis (PCA) and orthogonal partial least-squares discriminant analysis (OPLS-DA) were used to model the systematic variation related to patients with CIN or CSCC with healthy controls. Potential metabolic biomarkers were identified using database comparisons, and the one-way a...

  14. Application of 1H-NMR metabolomic profiling for reef-building corals.

    Emilia M Sogin

    Full Text Available In light of global reef decline new methods to accurately, cheaply, and quickly evaluate coral metabolic states are needed to assess reef health. Metabolomic profiling can describe the response of individuals to disturbance (i.e., shifts in environmental conditions across biological models and is a powerful approach for characterizing and comparing coral metabolism. For the first time, we assess the utility of a proton-nuclear magnetic resonance spectroscopy (1H-NMR-based metabolomics approach in characterizing coral metabolite profiles by 1 investigating technical, intra-, and inter-sample variation, 2 evaluating the ability to recover targeted metabolite spikes, and 3 assessing the potential for this method to differentiate among coral species. Our results indicate 1H-NMR profiling of Porites compressa corals is highly reproducible and exhibits low levels of variability within and among colonies. The spiking experiments validate the sensitivity of our methods and showcase the capacity of orthogonal partial least squares discriminate analysis (OPLS-DA to distinguish between profiles spiked with varying metabolite concentrations (0 mM, 0.1 mM, and 10 mM. Finally, 1H-NMR metabolomics coupled with OPLS-DA, revealed species-specific patterns in metabolite profiles among four reef-building corals (Pocillopora damicornis, Porites lobata, Montipora aequituberculata, and Seriatopora hystrix. Collectively, these data indicate that 1H-NMR metabolomic techniques can profile reef-building coral metabolomes and have the potential to provide an integrated picture of the coral phenotype in response to environmental change.

  15. Application of 1H-NMR Metabolomic Profiling for Reef-Building Corals

    Sogin, Emilia M.; Anderson, Paul; Williams, Philip; Chen, Chii-Shiarng; Gates, Ruth D.

    2014-01-01

    In light of global reef decline new methods to accurately, cheaply, and quickly evaluate coral metabolic states are needed to assess reef health. Metabolomic profiling can describe the response of individuals to disturbance (i.e., shifts in environmental conditions) across biological models and is a powerful approach for characterizing and comparing coral metabolism. For the first time, we assess the utility of a proton-nuclear magnetic resonance spectroscopy (1H-NMR)-based metabolomics approach in characterizing coral metabolite profiles by 1) investigating technical, intra-, and inter-sample variation, 2) evaluating the ability to recover targeted metabolite spikes, and 3) assessing the potential for this method to differentiate among coral species. Our results indicate 1H-NMR profiling of Porites compressa corals is highly reproducible and exhibits low levels of variability within and among colonies. The spiking experiments validate the sensitivity of our methods and showcase the capacity of orthogonal partial least squares discriminate analysis (OPLS-DA) to distinguish between profiles spiked with varying metabolite concentrations (0 mM, 0.1 mM, and 10 mM). Finally, 1H-NMR metabolomics coupled with OPLS-DA, revealed species-specific patterns in metabolite profiles among four reef-building corals (Pocillopora damicornis, Porites lobata, Montipora aequituberculata, and Seriatopora hystrix). Collectively, these data indicate that 1H-NMR metabolomic techniques can profile reef-building coral metabolomes and have the potential to provide an integrated picture of the coral phenotype in response to environmental change. PMID:25354140

  16. Statistical contributrion to the analysis of metabonomic data in 1H-NMR spectroscopy

    Rousseau, Réjane

    2011-01-01

    This thesis provides a complete methodology to lead a metabonomic study from the data acquisition to the discovery of biomarkers. Metabonomics aims to discover biomarkers or the metabolites altered in biological reactions. 1H-NMR spectroscopy is used to generate spectral profiles describing the composition of metabolites in collected biofluid samples. Statistical comparisons of spectra obtained in various biological states permits a quantitative investigation of metabolites changes inherent t...

  17. Multivoxel 1H-MR spectroscopy in obstructive sleep apnea hypopnea syndrome

    Objective: To investigate the clinical value of multivoxel 1H magnetic resonance spectroscopy (1H-MRS) in patients with obstructive sleep apnea hypopnea syndrome (OSAHS). Materials and Methods: 20 patients (case group) with moderate to severe clinically diagnosed OSAHS and 20 age-gender matched healthy volunteers (control group) underwent brain multivoxel 1H-MRS examinations. The ratios of brain metabolites of centrum ovale and basal ganglia were recorded respectively. Related clinical indexes, including sleep apnea and hypopnea index (AHI) and the average night-time oxygen saturation (SpO2), were recorded. Results: In region of centrum ovale, the NAA/Cho and NAA/Cr of the case group decreased and were significantly lower than that of control group (P<0.05). The Cho/Cr of the case group was significantly increased compared to the controls (P<0.05). In region of basal ganglia, the NAA/Cho, NAA/Cr, and Cho/Cr had no significantly difference between the two groups (P>0.05). Lactate peak was not detected in the two groups. In the region of centrum ovale, the AHI showed inverse correlation to the NAA/Cho (P<0.05). The SpO2 showed positive correlations to the NAA/Cho (P<0.05). There was no correlation between clinical indexes and NAA/Cr or Cho/Cr (P>0.05). Conclusion: Multivoxel 1H-MRS could early detect the changes of cerebral metabolism in patients with OSAHS. It provides an objective imaging basis for the clinical diagnosis and treatment. (authors)

  18. 1H and 2H NMR study in paramagnetic solutions of Eu3+ nitrate

    The dependence of the spin-lattice rate(1/T1) of 1H and 2H nuclei for the 2.1 T magnetic field of the concentration (from 0.1 to 2.75 mol) of Eu3+ paramagnetic ions in the range from 263 K to 373 K is presented . Also the NMRD profield for the frecuency range from 0.1 to 500 Mhz is showed

  19. MRI and {sup 1}H MRS findings in Smith-Lemli-Opitz syndrome

    Caruso, P.A. [Department of Radiology, Massachusetts Eye and Ear Infirmary, Boston, MA (United States); Harvard Medical School, Boston, MA (United States); Poussaint, T.Y. [Department of Radiology, Children' s Hospital, 300 Longwood Avenue, MA 02115, Boston (United States); Tzika, A.A.; Astrakas, L.G. [Department of Surgery, Massachusetts General Hospital, Boston, MA (United States); Zurakowski, D. [Department of Biostatistics, Children' s Hospital Boston, Boston, MA (United States); Elias, E.R. [Department of Pediatrics and Genetics, Children' s Hospital, Denver, CO (United States); School of Medicine, University of Colorado, Denver, CO (United States); Bay, C. [Department of Medical Genetics, Children' s Hospital of Pittsburgh, Pittsburgh, PA (United States); Irons, M.B. [Division of Clinical Genetics and Metabolism, Children' s Hospital Boston, Boston, MA (United States)

    2004-01-01

    Smith-Lemli-Opitz syndrome (SLOS) is an autosomal recessive disorder characterized by a defect in cholesterol biosynthesis, associated with mental retardation and multisystem structural abnormalities. This study investigated the prevalence of congenital CNS abnormalities by MRI in a large series of patients with SLOS and the correlation of the clinical and biochemical findings with the results of MRI and {sup 1}H MRS. Eighteen patients were studied; all underwent MRI of the brain, and 16 had {sup 1}H MRS of the cerebral white matter. The ratios choline:NAA, lipid:NAA, and lipid:choline metabolite were found to be correlated with the clinical degree of disease severity, serum total sterol ratios (cholesterol/cholesterol + 7-dehydrocholesterol + 8-dehydrocholesterol) and in two cases with the effect of cholesterol therapy. Abnormal CNS findings were noted in five patients, including callosal abnormalities (n=4), Dandy-Walker variant (n=1), and arachnoid cyst (n=1). Holoprosencephaly was noted in one patient with a prevalence of 6%. Choline:NAA was elevated in seven patients. There was a statistically significant positive correlation between the lipid:choline ratio and the serum cholesterol precursor, 8-dehydrocholesterol. In two patients {sup 1}H MRS demonstrated abnormally elevated lipids prior to cholesterol therapy, which improved on therapy. The use of MRI and {sup 1}H MRS is an effective way to demonstrate brain structural abnormalities in patients with SLOS and may prove to be an effective method for the assessment of the effects of cholesterol replacement therapy in the brain. (orig.)

  20. 2-(2-hydroxyethyl)-1H,3H-benzo[c]pyrrol-1-one

    Urban, Jiří; Fábry, Jan; Zuman, P.; Ludvík, Jiří; Císařová, I.

    2007-01-01

    Roč. 63, - (2007), o4137-o4138. ISSN 1600-5368 R&D Projects: GA MŠk 1P05ME785 Institutional research plan: CEZ:AV0Z40400503; CEZ:AV0Z10100520 Keywords : 2-(2-hydroxyethyl)-1H,3H-benzo[c]pyrrol-1-one * hydrogen bonds * interactions Subject RIV: CG - Electrochemistry Impact factor: 0.508, year: 2007

  1. Cholinergic Dysfunction in Fragile X Syndrome and Potential Intervention: A Preliminary 1H MRS Study

    Kesler, Shelli R.; Lightbody, Amy A.; Reiss, Allan L.

    2009-01-01

    Males with fragile X syndrome are at risk for significant cognitive and behavioral deficits, particularly those involving executive prefrontal systems. Disruption of the cholinergic system secondary to fragile X mental retardation protein deficiency may contribute to the cognitive-behavioral impairments associated with fragile X. We measured choline in the dorsolateral prefrontal cortex of 9 males with fragile X syndrome and 9 age-matched typically developing controls using 1H magnetic resona...

  2. 1 H MR Spectroscopy in Gliomatosis: Is there a Sensitivity Issue?

    Eljamel, M.S.; M. Szewczyk-Bieda; Main, G.; Kanodia, A. K.

    2011-01-01

    Objective. 1H MR spectroscopy (MRS) is widely performed for assessment of brain tumours and is considered a highly sensitive technique capable of differentiating benign from malignant conditions and tumour grading. Method. We present a case of a 69 year old woman who was suspected to have gliomatosis on MRI. Results. MRS performed using single voxel and chemical shift/multivoxel techniques was within normal limits. A repeat scan 6 months later showed progressive disease, and biopsy was perfor...

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

    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

  4. Follow-up gliomas after radiotherapy: {sup 1}H MR spectroscopic imaging for increasing diagnostic accuracy

    Lichy, Matthias Philipp; Plathow, Christian [German Cancer Research Center, Department of Radiology, Heidelberg (Germany); University of Tuebingen, Department of Diagnostic Radiology, Tuebingen (Germany); Schulz-Ertner, Daniela [University of Heidelberg, Department of Radiation Therapy, Heidelberg (Germany); Kauczor, Hans-Ulrich [German Cancer Research Center, Department of Radiology, Heidelberg (Germany); Schlemmer, Heinz-Peter [University of Tuebingen, Department of Diagnostic Radiology, Tuebingen (Germany)

    2005-11-01

    We evaluated the value of magnetic resonance imaging (MRI) and the additional benefit of proton MR spectroscopic imaging ({sup 1}H SI) in patients with a new suspicious lesion after fractionated stereotactic radiotherapy (FSRT) of a glioma. Thirty-four patients with histologically proven astrocytoma WHO II-IV after treatment by FSRT and a new suspect lesion in the follow-up were included in this study. Data were analysed by three independent radiologists with different experience in {sup 1}H SI: Data were verified by clinical follow-up (PT, progressive tumour; nPT, non-progressive tumour) and a kappa analysis was performed. Sensitivity and specificity of T{sub 1} weighted (w) and T{sub 2}w MRI was compared (imaging at radiotherapy and follow-up) using further follow-up controls as gold standard and the additional benefit of {sup 1}H SI (imaging at follow-up) was calculated. Mean interval between last irradiation and detection of a suspicious lesion was 37 {+-} 32 months. Time to clinical evaluation was 13 {+-} 8 months. Interobserver agreement was significantly high in all analyses (kappa always >0.8, P < 0.05). T{sub 2}w imaging proved to be superior to contrast enhanced T{sub 1}w imaging in sensitivity (87.5 vs 81.25%) and specificity (85.7 vs 57.1%). Solitary {sup 1}H SI had similar results as T{sub 2}w (sensitivity 87.5%, specificity 71.4%). Taking all techniques into account, all PT were correctly diagnosed. (orig.)

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

    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)

  6. Metabolic phenotyping by 1H-NMR spectroscopy detects lung cancer via a simple blood sample

    Louis,Evelyne; MESOTTEN, Liesbet; Thomeer, Michiel; Vandeurzen, Kurt; Darquennes, Karen; Vanhove, Karolien; Reekmans, Gunter; Adriaensens, Peter

    2013-01-01

    Introduction: Lung cancer is the leading cause of cancer death worldwide. There is an urgent need of effective methods to detect lung cancer. Accumulating evidence shows that the metabolism of cancer cells differs from that of normal cells. Disturbances in biochemical pathways which occur during the development of cancer provoke changes in the metabolic phenotype. Objective: To determine the metabolic phenotype of lung cancer by 1H-NMR spectroscopy. Methods: Fasting venous blood samples of 78...

  7. Metabolic phenotyping of blood plasma by 1H-NMR spectroscopy to detect lung cancer?

    Louis,Evelyne; MESOTTEN, Liesbet; Thomeer, Michiel; Vanhove, Karolien; Vandeurzen, K.; Sadowska, A.; Reekmans, Gunter; Adriaensens, Peter

    2013-01-01

    Introduction. Lung cancer is the leading cause of cancer death worldwide. An effective method which allows to detect lung cancer is urgently needed. Accumulating evidence shows that the metabolism of cancer cells differs from that of normal cells(1). Disturbances in biochemical pathways which occur during the development of cancer provoke changes in the metabolic phenotype(2). Objective. To determine the metabolic phenotype of lung cancer by means of proton nuclear magnetic resonance (1H-...

  8. {sup 1}H-MR-spectroscopic imaging in patients with Alzheimer`s disease; {sup 1}H-MR-spektroskopische Bildgebung bei Patienten mit klinisch gesichertem Morbus Alzheimer

    Block, W. [Radiogische Klinik der Univ. Bonn (Germany); Traeber, F. [Radiogische Klinik der Univ. Bonn (Germany); Kuhl, C.K. [Radiogische Klinik der Univ. Bonn (Germany); Fric, M. [Psychiatrische Universitaetsklinik, Bonn (Germany); Keller, E. [Radiogische Klinik der Univ. Bonn (Germany); Lamerichs, R. [Philips Medical Systems, Best (Netherlands); Rink, H. [Radiogische Klinik der Univ. Bonn (Germany); Moeller, H.J. [Psychiatrische Universitaetsklinik, Bonn (Germany); Schild, H.H. [Radiogische Klinik der Univ. Bonn (Germany)

    1995-09-01

    To detect regional differences in accompanying metabolic changes, {sup 1}H-Magnetic Resonance Spectroscopic Imaging was performed in 16 patients with Alzheimer`s disease (AD); the clinical diagnosis was based upon DSM-III-R and NINCDS-ADRDA guidelines. In the hippocampal region metabolic maps of the local distribution of N-acetylaspartate (NAA), choline (Cho), creatine compounds (P(Cr)) and lactate were determined. Ratios of Cho/NAA, (P)Cr/NAA and Cho/(P)Cr calculated from selected hippocampal spectra were compared to those from healthy volunteers (n=17). AD patients demonstrated an increase of Cho/NAA and (P)Cr/NAA ratios caused by increased choline compounds and decreased NAA. These alterations were observed in 11/12 cases in the hippocampal and in 7/12 in the temporo-occipital region. Hippocampal Cho/NAA ratios (0.56{+-}0.19) were significantly elevated compared with controls. The observed elevation of choline compounds in the hippocampus supports the hypothesis that alterations in the cholinergic system play an important role in Alzheimer`s disease. The observed reduction of NAA is due to neuronal degeneration. (orig./MG) [Deutsch] Zur Darstellung von regionalen metabolischen Veraenderungen bei Morbus Alzheimer wurden mit dem Verfahren des {sup 1}H-Magnetic-Resonance-Spectroscopic-Imaging 16 Patienten untersucht, deren Diagnose klinisch entsprechend DSM-III-R- und NINCDS-ADRDA-Kriterien gestellt wurde. In Hoehe des Hippocampus wurden transaxiale ``Metabolitenkarten`` der regionalen Verteilung von N-Acetyl-Aspartat (NAA), cholinhaltiger Verbindungen (Cho), Gesamtkreatin (P(Cr)) und Laktat erstellt. Zur Quantifizierung der Unterschiede zum Normalkollektiv (n=17) wurden die Metabolitenquotienten Cho/NAA, (P)Cr/NAA und Cho/(P)Cr, insbesondere aus der Hippocampusregion, ermittelt. Das Krankheitsbild des M. Alzheimer stellte sich durch eine Erhoehung der Quotienten Cho/NAA und Cho/(P)Cr dar, wobei neben einer Cholinerhoehung die Reduktion des Neurotransmitters NAA

  9. 1H MRS study of brain metabolic disorder in patients with chronic liver cirrhosis

    Objective: To study the metabolic alterations in the brain of patients with chronic liver cirrhosis with 1H magnetic resonance spectroscopy (1H MRS) for better understanding the pathophysiology of chronic hepatic encephalopathy (CHE), which will help us in the diagnosis and treatment of this disease. Methods: STEAM 1H MRS and MRI were performed in 30 patients with chronic liver cirrhosis is and 15 healthy volunteers. The height of resonance peaks of different metabolites was measured and the ratios of the other metabolites to Cr were calculated. The authors also studied the correlation between metabolites and the association between globus pallidum signal intensity and the spectroscopic alterations. Results: In patients with severe cirrhosis (in decompensatory period) or CHE, the mean values of mI/Cr and Cho/Cr ratio were significantly lower than those in healthy volunteers or patients with minor cirrhosis (in compensatory period) (P0.05). There was negative correlation between mI/Cr and Glx-α/Cr(r -0.51, n = 44, P1-weighted images, the globus pallidum signal intensity was significantly higher in patients with severe cirrhosis or CHE. mI/Cr, Cho/Cr and Glx-α/Cr correlated significantly with MRI signal changes respectively. Conclusions: Proton MRS can demonstrate brain metabolic changes in patients with chronic liver cirrhosis in vivo noninvasively, thereby helping interpret the pathophysiology of CHE

  10. Improved analysis of 1H-MR spectra in the presence of mobile lipids.

    Auer, D P; Gössl, C; Schirmer, T; Czisch, M

    2001-09-01

    Focal brain lesions can be associated with proton magnetic resonance spectra (1H-MRS)-detectable mobile lipids, reflecting severe tissue degradation and necrosis. However, advanced fitting procedures, such as the LCModel, fail to adequately fit spectra in the presence of lipid resonances. To overcome this, different approaches to generate lipid model spectra were compared using a phantom, real in vivo data, and simulated data. Twenty-six in vivo short-echo time (TE) 1H-MRS from 21 malignant gliomas, four infections, and one ischemia were analyzed to evaluate the performance of the modified LCModel fit. Adding simulated aliphatic resonances at 1.3 and 0.9 ppm improved the overall fitting quality remarkably and allowed good separation of lactate and alanine. Also, a better differentiation of glioblastomas and anaplastic gliomas was achieved. In conclusion, we propose a simple way to efficiently include lipid resonances in the LCModel, allowing a better fit of in vivo short-TE 1H-MRS, and demonstrate the diagnostic potential of quantitative assessment of mobile lipids in brain tumors. PMID:11550257

  11. 1H-MR spectroscopy in anorexia nervosa. Reversible cerebral metabolic changes

    Purpose: By using localized 1H-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 1H-MR spectroscopy (TE=50 ms, TM=30 ms, TR=1500 ms, voxel (2 cm)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: 1H-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.)

  12. Effect of biological factors on successful measurements with skeletal-muscle 1H-MRS

    Isobe, Tomonori; Okamoto, Yoshikazu; Hirano, Yuji; Ando, Hiroki; Takada, Kenta; Sato, Eisuke; Shinoda, Kazuya; Tadano, Kiichi; Takei, Hideyuki; Kamizawa, Satoshi; Mori, Yutaro; Suzuki, Hiroaki

    2016-01-01

    Background Our purpose in this study was to clarify whether differences in subject group attributes could affect data acquisition in proton magnetic resonance spectroscopy (1H-MRS). Methods Subjects without diabetes mellitus (DM) were divided into two groups (group A, in their 20s; group B, 30–60 years old). Subjects with DM formed group C (30–60 years old). The numbers of subjects were 19, 27, and 22 for group A, B, and C respectively. For all subjects, 1H-MRS measurements were taken of the soleus muscle (SOL) and the anterior tibial muscle (AT). We defined the success of the measurements by the detection of intramyocellular lipids. Moreover, we also measured the full width at half maximum of the water peaks for all subjects. Results The success rate was significantly higher for the AT (100%) than for the SOL (81.6%) (P<0.01). For the SOL, the success rate was 100% in group A, 85.2% in group B, and 77.3% in group C. There was a significant difference (P<0.05) between groups A and B, as well as between groups A and C. In all subjects, there was a significant difference (P<0.01) in the full width at half maximum (Hz) of the water peak between the AT and SOL measurements. Conclusion We conclude that differences in the age and DM history of subjects could affect the probability of successful 1H-MRS data acquisition. PMID:27499626

  13. 1H relaxation enhancement induced by nanoparticles in solutions: Influence of magnetic properties and diffusion

    Magnetic nanoparticles that induce nuclear relaxation are the most promising materials to enhance the sensitivity in Magnetic Resonance Imaging. In order to provide a comprehensive understanding of the magnetic field dependence of the relaxation enhancement in solutions, Nuclear Magnetic Resonance 1H spin-lattice relaxation for decalin and toluene solutions of various Fe2O3 nanoparticles was investigated. The relaxation experiments were performed in a frequency range of 10 kHz–20 MHz by applying Field Cycling method, and in the temperature range of 257–298 K, using nanoparticles differing in size and shape: spherical – 5 nm diameter, cubic – 6.5 nm diameter, and cubic – 9 nm diameter. The relaxation dispersion data were interpreted in terms of a theory of nuclear relaxation induced by magnetic crystals in solution. The approach was tested with respect to its applicability depending on the magnetic characteristics of the nanocrystals and the time-scale of translational diffusion of the solvent. The role of Curie relaxation and the contributions to the overall 1H spin-lattice relaxation associated with the electronic spin-lattice and spin-spin relaxation was thoroughly discussed. It was demonstrated that the approach leads to consistent results providing information on the magnetic (electronic) properties of the nanocrystals, i.e., effective electron spin and relaxation times. In addition, features of the 1H spin-lattice relaxation resulting from the electronic properties of the crystals and the solvent diffusion were explained

  14. 1H NMR spectroscopic studies establish that heparanase is a retaining glycosidase

    Highlights: •1H and 13C NMR chemical shifts of fondaparinux were fully assigned by 1D and 2D NMR techniques. •Hydrolysis of fondaparinux by heparanase was monitored by 1H 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 1H 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

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

    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.

  16. Discriminating binding and positioning of amphiphiles to lipid bilayers by 1H NMR

    The binding and positioning in lipid bilayers of three well-known drugs--imipramine, nicotine, and caffeine--have been studied using 1H 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) 1H 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) 1H 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

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

    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.

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

    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.

  19. Fire-related post-traumatic stress disorder: brain 1H-MR spetroscopic findings

    To investigate the MR imaging and 1H-MR spectroscopic findings of acute fire-related post-traumatic stress disorder (PTSD). Sixteen patients (M:F=10:6; mean age, 16 years) with fire-related PTSD underwent MR imagine and 1H-MR spectroscopy, and for control purposes, the procedures were repeated in eight age-matched normal volunteers. In all patients and controls, the regions of interest where data were acquired at MRS were the basal ganglia (BG), frontal periventricular white matter (FWM), and parietal periventricular white matter (PWM). In all patients with PTSD, MR images appeared normal. In contrast, MRS showed that in the BG, NAA/Cr ratios were significantly lower in patients than in volunteers. This decrease did not, however, show close correlation with the severity of the neuropsychiatric symptoms. In patients, neither NAA/Cr ratios in FWM nor PWM, nor Cho/Cr ratios in all three regions, were significantly different from those in the control group. Decreased NAA/Cr ratios in the BG, as seen at 1H-MRS, might be an early sign of acute fire-related PTSD

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

    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.