Analysis of 1H and 13C{1H} NMR Spectral Parameters of Diphenylchloroarsine, Diphenylcyanoarsine, and 10-Chloro- 5,10-Dihydrophenarsazine: Identification of the Compounds through Reference to Simulated Spectra

1997 ◽  
Vol 51 (5) ◽  
pp. 733-737 ◽  
Author(s):  
Markku Mesilaakso ◽  
Eeva-Liisa Tolppa ◽  
Paula Nousiainen
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
1H Nmr ◽  
Nmr Spectra ◽  
Spectral Parameters ◽  
H Nmr ◽  
Iterative Analysis ◽  
Simulation Of Spectra ◽  
Nuclear Magnetic

The 1H and 13C{1H} nuclear magnetic resonance (NMR) spectra of diphenylchloroarsine, diphenylcyanoarsine, and 10-chloro-5,10-dihydrophenarsazine were recorded from samples prepared in CDCl3, CD2Cl2, and (CD3)2CO. Spectra were analyzed, and detailed 1H NMR spectral parameters were determined by iterative analysis. Simulation of spectra and their use as reference spectra for identification of the compounds under different conditions are discussed.

Identification of Polychlorinated Pyrenes and Pyrene-Addition Products Using Proton Nuclear Magnetic Resonance Techniques

1987 ◽  
Vol 41 (7) ◽  
pp. 1194-1199 ◽  
Author(s):  
David L. Ashley ◽  
Elizabeth R. Barnhart ◽  
Donald G. Patterson ◽  
Robert H. Hill
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Nmr Spectra ◽  
Chemical Shifts ◽  
Proton Nuclear Magnetic Resonance ◽  
Relaxation Rates ◽  
Spectral Parameters ◽  
Normal Orientation ◽  
Nmr Techniques ◽  
Nuclear Magnetic

Nuclear magnetic resonance (NMR) techniques are used to determine the chlorination pattern on a number of chlorinated pyrenes and pyrene-addition products. Determining chemical shifts, couplings, and longitudinal relaxation rates makes the unequivocal assignment of these molecules possible. Chlorination under the conditions described here were found to follow the normal orientation rules for pyrene. Spectral parameters obtained from these molecules are consistent enough to allow further application to unknown compounds. This should simplify assigning NMR spectra to other chlorinated pyrene standards.

scholarly journals Nuclear Magnetic Resonance Studies on Aromatic Compounds. Part II. 13C and 1H NMR Spectra of 1-Hydroxy-4-sulfo-2-naphthoic Acid.

1977 ◽  
Vol 31a ◽  
pp. 700-702 ◽  
Author(s):  
Lauri H. Lajunen ◽  
Kauko Räisänen ◽  
Signe Kjelstrup Ratkje ◽  
Michel Pouchard ◽  
Paul Hagenmuller ◽  
...  
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
1H Nmr ◽  
Aromatic Compounds ◽  
Nmr Spectra ◽  
1H Nmr Spectra ◽  
Magnetic Resonance Studies ◽  
Naphthoic Acid ◽  
Nuclear Magnetic

scholarly journals Nuclear Magnetic Resonance-based Metabolomics of Blood Plasma from Dairy Calves Infected with the Main Causal Agents of Bovine Respiratory Disease (BRD)

2021 ◽  
Author(s):  
Mariana Santos-Rivera ◽  
Nicholas C. Fitzkee ◽  
Rebecca A. Hill ◽  
Richard E. Baird ◽  
Ellianna Blair ◽  
...  
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Blood Plasma ◽  
Respiratory Disease ◽  
Nmr Spectra ◽  
Bovine Respiratory Disease ◽  
Dairy Calves ◽  
Proton Nuclear Magnetic Resonance ◽  
H Nmr ◽  
Nuclear Magnetic

Abstract Each year, Bovine Respiratory Disease (BRD) results in significant economic loss in the cattle sector, and novel metabolic profiling and early diagnosis techniques represent a promising tool for developing effective measures for disease management. Here, proton - Nuclear Magnetic Resonance (1H - NMR) spectra were used to characterize metabolites from blood plasma collected from dairy calves intentionally infected with the main BRD causal agents, bovine respiratory syncytial virus (BRSV) and Mannheimia haemolytica (MH), to generate a well-defined metabolomic profile under controlled conditions. In response to infection, 42 metabolites (BRSV = 27, MH = 24) changed in concentration compared to the Baseline (non-infected) state. Fuel substrates and products exhibited a particularly strong effect, reflecting imbalances that occur during the immune response. Glucose levels decreased only during bacterial infection, suggesting that the clinical signs of bacterial BRD are more energetically taxing than those of viral BRD. Furthermore, 1H - NMR spectra from Baseline and Infected samples were discriminated with an accuracy, sensitivity, and specificity ≥ 95% using chemometrics to model the changes associated with disease, suggesting that metabolic profiles can be used for further development and validation of diagnostic tools.

scholarly journals Antifungal Effects on Metabolite Profiles of Medically Important Yeast Species Measured by Nuclear Magnetic Resonance Spectroscopy

2006 ◽  
Vol 50 (12) ◽  
pp. 4018-4026 ◽  
Author(s):  
Muireann Coen ◽  
Jennifer Bodkin ◽  
Damla Power ◽  
William A. Bubb ◽  
Uwe Himmelreich ◽  
...  
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Nmr Spectra ◽  
Yeast Species ◽  
Antifungal Drugs ◽  
Resonance Spectroscopy ◽  
H Nmr ◽  
Broth Microdilution Method ◽  
Antifungal Effects ◽  
Nuclear Magnetic

ABSTRACT Drug-induced inhibition of fungal growth is used in the diagnostic laboratory to predict therapeutic efficacy but is relatively slow, and determination of endpoints can be problematic. Nuclear magnetic resonance (NMR) spectroscopy identifies the metabolic complement of microorganisms while monitoring utilization of constituents of the incubation medium. This technique may provide a rapid and objective indicator of antifungal effects. We evaluated the effects of caspofungin, amphotericin B (AMB), and voriconazole on metabolic profiles of yeast species cultured in RPMI-2% glucose-morpholinepropanesulfonic acid buffer in microtiter plates in a proof-of-principle study. 1H NMR spectra were obtained using Bruker NMR spectrometers at 1H frequencies of 600 and 360 MHz. Metabolites were identified by two-dimensional correlation NMR spectra, and relative peak integrals were calculated from one-dimensional 1H NMR spectra. MICs were determined by a modification of the Clinical and Laboratory Standards Institute broth microdilution method M27-A. Utilization of glucose and branched-chain and aromatic amino acid substrates was accompanied by fungal production of acetate, acetaldehyde, ethanol, formate, fumarate, glycerol, lactate, pyruvate, and succinate. Clear-cut metabolic endpoints indicating a greater than 50% reduction in substrate utilization and fungal metabolite production which correlated with MICs were noted at 16 and 24 h for all three drugs. At 8 h, reductions of greater than 50% for selected metabolites were noted for caspofungin and AMB. Direct NMR-based observation of metabolic alterations in yeast cultures reveals changes in key metabolic pathways and should be evaluated formally as a rapid technique for determining susceptibility to antifungal drugs.

Phosphorus nuclear magnetic resonance of fast- and slow-twitch muscle

1985 ◽  
Vol 248 (3) ◽  
pp. C279-C287 ◽  
Author(s):  
R. A. Meyer ◽  
T. R. Brown ◽  
M. J. Kushmerick
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Nmr Spectra ◽  
H Nmr ◽  
Slow Twitch Muscle ◽  
Creatine Kinase Equilibrium ◽  
Slow Twitch ◽  
Twitch Characteristics ◽  
Fast Twitch ◽  
Nuclear Magnetic

Phosphorus nuclear magnetic resonance (NMR) spectra were obtained at 109.3 MHz from isolated, arterially perfused cat biceps brachi (greater than 75% fast-twitch, glycolytic fibers) and soleus (greater than 92% slow-twitch, oxidative) muscles at 30 degrees C. The perfused muscles were stable with respect to O2 consumption, twitch characteristics, and ATP and phosphocreatine (PC) levels for up to 10 h. NMR spectra showed a higher PC/Pi ratio in the biceps (11) than in the soleus (1.7). Relatively higher Pi levels were observed in extracts of clamp-frozen muscles than in the intact muscles. This difference could be accounted for by artifactual hydrolysis of PC during muscle freezing. Based on the NMR and chemical data, the free cytosolic ADP level, calculated from the creatine kinase equilibrium, was 14 microM in the soleus and less than 1 microM in the biceps. Intracellular Pi concentration was 10 mM in the soleus and 3 mM in the biceps. Intracellular pH, estimated from the chemical shift of phosphate or 2-deoxyglucose 6-phosphate, was 7.0 in both muscles (perfusate pH 7.2). Both extracellular space and pH measurements were obtained from NMR spectra of muscles perfused with 10 mM sodium phenylphosphonate added to the perfusate. These results document larger differences in the phosphate metabolites in the two types of mammalian muscles than previously reported.

scholarly journals Comparison of HPLC and NMR for Quantification of The Main Volatile Fatty Acids in Rumen Digesta

2021 ◽  
Author(s):  
Mengyuan Wang ◽  
Haiying Wang ◽  
Huiru Zheng ◽  
Dusan Uhrin ◽  
Richard J. Dewhurst ◽  
...  
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Correlation Analysis ◽  
Nmr Spectra ◽  
Rumen Fluid ◽  
Line Broadening ◽  
H Nmr ◽  
First Choice ◽  
Pre Treatment ◽  
Nuclear Magnetic

Abstract BackgroundAccurate quantification of volatile fatty acid (VFA) concentrations in rumen fluid are essential for research on rumen metabolism. HPLC analysis of VFAs has the advantages of relatively simple sample preparation, no derivatization and high sensitivity, but it can only be used to quantify metabolites when standards are used. 1H Nuclear magnetic resonance (1H-NMR) targeted metabolomics could provide more metabolism information by detecting the proton fingerprint of biochemical mixtures and chemometric analysis of metabolite concentration. This study comprehensively investigated the pros and cons of High-performance liquid chromatography (HPLC) and 1H Nuclear magnetic resonance (1H-NMR) analysis methods for ruminal VFA. We also investigated the performance of several commonly used data pre-treatments for the two sets of data using correlation analysis, principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA). Our work aimed primarily to verify the repeatability, precision, and limits of the methods. It provided insights into the methods used for metabolite data pre-treatment before downstream analysis. ResultsThe molar proportion and reliability analysis demonstrated that the two approaches produce highly consistent VFA concentrations. In the pre-processing of NMR spectra, line broadening and shim correction may reduce estimated concentrations of metabolites. We identified differences in results using different spectral clusters and the chemical shifts of the spectral clusters as quantitative references for VFAs were provided. Different data pre-treatment strategies tested with both HPLC and NMR significantly affected the results of downstream data analysis. “Normalized by sum” pre-treatment can eliminate the large number of positive correlations between NMR-based VFA, which is helpful for correlation analysis between metabolites. To make the differences between samples based on metabolites comparable, scaling should be used. ConclusionsRegarding the quantitative processing steps of NMR spectroscopy and subsequent data pre-treatments, the study provided the following practical suggestions. In the pre-processing of NMR spectra, line broadening and shim correction are recommended to use with caution. A “Combine” strategy should be the first choice when calculating the correlation between metabolites or between samples, but it is not applicable in PCA and PLS-DA analysis. However, the PCA and PLS-DA suggest that except for “Normalize by sum”, pre-treatments should be used with caution.

Nuclear Magnetic Resonance Studies of Substituted 4-Hydroxy-5-phosphinyl-2-imidazolidinones

1982 ◽  
Vol 36 (4) ◽  
pp. 466-471 ◽  
Author(s):  
John A. Mikroyannidis ◽  
Alexandros K. Tsolis
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Nmr Spectroscopy ◽  
Magnetic Resonance ◽  
Nmr Spectra ◽  
Parent Compound ◽  
Proton Nuclear Magnetic Resonance ◽  
Magnetic Resonance Studies ◽  
Aqueous Sodium ◽  
H Nmr ◽  
Nuclear Magnetic

The proton nuclear magnetic resonance (NMR) spectra of some substituted 4-hydroxy-5-phosphinyl-2-imidazolidinones have been studied. The predominance of the cis stereoisomer of these compounds has been also established by 1H NMR spectroscopy. The spectral effects produced by the introduction of the phosphinyl group on the parent compound and by reaction of the substituted 4-hydroxy-5-phosphinyl-2-imidazolidinones with aqueous sodium deuteroxide are discussed. In addition, it has been established by 1H NMR that the product obtained from the reaction of 2-hydroxy-2-(diethoxyphosphinyl)ethanal with N-methylurea was a mixture of 18.2% 1-methyl- and of 81.8% 3-methyl-4-hydroxy-5-diethoxyphosphinyl-2-imidazolidinone.

scholarly journals P052 Nuclear magnetic resonance metabolomic profiling of IBD patients under anti-TNF treatment. Are the pathways network deregulated?

2020 ◽  
Vol 14 (Supplement_1) ◽  
pp. S160-S160
Author(s):  
S Notararigo ◽  
M Martin-Pastor ◽  
J E Dominguez Munoz ◽  
M Barreiro-de Acosta
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Nmr Spectra ◽  
Mononuclear Cells ◽  
High Rate ◽  
Resonance Spectroscopy ◽  
Serum Samples ◽  
Spectral Window ◽  
Metabolomic Study ◽  
Nuclear Magnetic

Abstract Background The deregulation of immune system cell response implies loss of T-cell apoptosis, high rate of proinflammatory cytokines production and subsequent exacerbate activation of TNF-α pathway. The use of biologic antibody decrease inflammation rate and symptoms, but it remains unclear if it has a direct effect on the pathways activation/inactivation on peripheral blood mononuclear cells (PBMCs). The aim of this study is evaluate the role of nuclear magnetic resonance spectroscopy (NMR) applied to the metabolomic study of serum samples isolated from fresh blood from inflammatory bowel disease (IBD) patients under IFX treatment to understand the activated/inactivated pathways of PBMCs. Methods A case–control study was performed. Inclusion criteria were IBD patients under IFX treatment. Blood samples were obtained in Crohn’s disease (CD) and ulcerative colitis (UC) patients before IFX and in healthy controls (CTRL). CD patients were divided into subgroups according to the gut affected, in Ileocolic (IC), ileum and colon. NMR samples of the serum were collected and measured according to Standard Operation Procedures. Three types of NMR spectra were measured for each serum sample (1Hnoepresat, 1Hcpmgpresat and 1HDfilterpresat). The signal in each NMR spectrum was integrated in a series of equidistant little portion of the spectrum called buckets of a constant width of 0.04 ppm, covering the complete 1H NMR spectral window from −5 to 14 ppm. Buckets in regions depleted from signal at the two extremes of the spectrum were discarded as well as those in the proximity of the water peak at ca. 4.7 ppm which was affected by the presaturation. The vectors corresponding to a number of samples of two or more groups can be rapidly analysed using Multivariant Statistical Analysis methods. Results Twenty-two IBD patients (12 CD and nine UC) were included, 10 CTRL were also included. The metabolomic analyses of the NMR spectra of the serum of the different patients and control groups by the fingerprinting and targeting profiling strategies provided OPLS-DA statistical models (Figure 1) that permitted the successful classification of certain groups of samples which are summarised in Table 1. Conclusion The results of this pilot NMR metabolomic study of serum samples of IBD found a series of spectral fingerprints that are able to discriminate between groups of patients CTRL and CD, which underlines its potential use for the diagnosis of the disease.

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