The NMR Spectral Measurement Database: A System for Organizing and Accessing NMR Spectra of Therapeutic Proteins

The Nuclear Magnetic Resonance Spectral Measurement Database (NMR-SMDB) was developed for the purpose of organizing and searching NMR spectral data of protein therapeutics, linking spectra to corresponding sample information and enabling quick access to full datasets and entire studies. In addition to supporting internal research at the National Institute of Standards and Technology (NIST), the system could facilitate data access to stakeholders outside of NIST, and future versions of the database software itself could be installed by others for their own data storage and retrieval.

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

Journal of Crohn s and Colitis ◽

10.1093/ecco-jcc/jjz203.181 ◽

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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The metal nuclear magnetic resonance spectra of some tin(II) and lead(II) complexes with polydentate phosphines

Canadian Journal of Chemistry ◽

10.1139/v83-307 ◽

1983 ◽

Vol 61 (8) ◽

pp. 1795-1799 ◽

Cited By ~ 13

Author(s):

Philip A. W. Dean

Keyword(s):

Nuclear Magnetic Resonance ◽

Magnetic Resonance ◽

Nmr Spectra ◽

Narrow Range ◽

Chemical Shifts ◽

Nuclear Magnetic Resonance Spectra ◽

Magnetic Resonance Spectra ◽

Nuclear Magnetic

The previously reported 1:1 complexes formed in MeNO2, between M(SbF6)2 (M = Sn or Pb) and Ph2P(CH2)2PPh2, PhP[(CH2)2PPh2]2, MeC(CH2PPh2)3, P[(CH2)2PPh2]3, and [Formula: see text] have been studied by metal (119Sn or 207Pb) nmr. The metal chemical shifts span the comparatively narrow range of −586 to −792 ppm and 60 to −269 ppm, relative to the resonance of MMe4, for 119Sn and 207Pb nmr, respectively. The implications of these data regarding the denticity of the ligand in M(P[(CH2)2PPh2]3)2+ are discussed, and a comparison with the metal nmr spectra of related stannous and plumbous complexes is made.

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A Metabolomic Approach to Beer Characterization

Molecules ◽

10.3390/molecules26051472 ◽

2021 ◽

Vol 26 (5) ◽

pp. 1472

Author(s):

Nicola Cavallini ◽

Francesco Savorani ◽

Rasmus Bro ◽

Marina Cocchi

Keyword(s):

Nuclear Magnetic Resonance ◽

Nmr Spectroscopy ◽

Magnetic Resonance ◽

Analytical Methods ◽

Nmr Spectra ◽

Full Spectrum ◽

The Past ◽

Beer Consumption ◽

Metabolomic Approach ◽

Chemometric Tools

The consumers’ interest towards beer consumption has been on the rise during the past decade: new approaches and ingredients get tested, expanding the traditional recipe for brewing beer. As a consequence, the field of “beeromics” has also been constantly growing, as well as the demand for quick and exhaustive analytical methods. In this study, we propose a combination of nuclear magnetic resonance (NMR) spectroscopy and chemometrics to characterize beer. 1H-NMR spectra were collected and then analyzed using chemometric tools. An interval-based approach was applied to extract chemical features from the spectra to build a dataset of resolved relative concentrations. One aim of this work was to compare the results obtained using the full spectrum and the resolved approach: with a reasonable amount of time needed to obtain the resolved dataset, we show that the resolved information is comparable with the full spectrum information, but interpretability is greatly improved.

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Synthesis and antimicrobial activities of some (E)-N'-1-(substituted benzylidene)benzohydrazides

International Journal of Advanced Chemistry ◽

10.14419/ijac.v5i1.7155 ◽

2017 ◽

Vol 5 (1) ◽

pp. 17 ◽

Cited By ~ 2

Author(s):

V. Manikandan ◽

S. Balaji ◽

R. Senbagam ◽

R. Vijayakumar ◽

M. Rajarajan ◽

...

Keyword(s):

Nuclear Magnetic Resonance ◽

Fourier Transform ◽

Magnetic Resonance ◽

Spectral Data ◽

Ultra Violet ◽

Antimicrobial Activities ◽

Antibacterial And Antifungal Activities ◽

Ft Ir ◽

Fourier Transform Ir ◽

Antibacterial And Antifungal

About ten substituted (E)-N'-1-(substituted benzylidene) benzohydrazides have been synthesized. They are analyzed by their analytical, ultra violet (UV), Fourier transform-IR (FT-IR) and nuclear magnetic resonance (NMR) spectral data and evaluated by antimicrobial activities such antibacterial and antifungal activities.

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Elucidating Tricin-Lignin Structures: Assigning Correlations in HSQC Spectra of Monocot Lignins

Polymers ◽

10.3390/polym10080916 ◽

2018 ◽

Vol 10 (8) ◽

pp. 916 ◽

Cited By ~ 14

Author(s):

Wu Lan ◽

Fengxia Yue ◽

Jorge Rencoret ◽

José del Río ◽

Wout Boerjan ◽

...

Keyword(s):

Nuclear Magnetic Resonance ◽

Magnetic Resonance ◽

Chemical Shift ◽

Nmr Spectra ◽

Model Compounds ◽

Heteronuclear Correlation ◽

Nmr Methods ◽

Nuclear Magnetic ◽

Lignin Structure

Tricin [5,7-dihydroxy-2-(4-hydroxy-3,5-dimethoxyphenyl)-4H-chromen-4-one] is a flavone that has been found to be incorporated in grass lignin polymers via 4′–O–β coupling. Herein, we investigated the tricin-lignin structure using nuclear magnetic resonance (NMR) methods by comparing the 1H–13C heteronuclear correlation (HSQC) NMR spectra of the isolated lignin with a series of dimeric and trimeric tricin-4′–O–β-ether model compounds. Results showed that the tricin moiety significantly affects the chemical shift of the Cβ/Hβ of 4′–O–β unit, producing peaks at around δC/δH 82.5–83.5/4.15–4.45, that differ from the Cβ/Hβ correlations from normal 4–O–β units formed solely by monolignols, and that have to date been unassigned.

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A 19F nuclear magnetic resonance study of the conjugate Brönsted-Lewis superacid HSO3F-SbF5. Part 1

Canadian Journal of Chemistry ◽

10.1139/v99-182 ◽

1999 ◽

Vol 77 (11) ◽

pp. 1869-1886 ◽

Cited By ~ 7

Author(s):

Dingliang Zhang ◽

Markus Heubes ◽

Gerhard Hägele ◽

Friedhelm Aubke

Keyword(s):

Nuclear Magnetic Resonance ◽

Magnetic Resonance ◽

Nmr Spectra ◽

Nuclear Magnetic Resonance Study ◽

Magnetic Resonance Study ◽

Formation Reaction ◽

H Nmr ◽

Acid Conjugate ◽

Nmr Methods ◽

Cis And Trans

The Brönsted-Lewis superacid HSO3F-SbF5 or "magic acid" is re-investigated by modern 19F NMR methods over a wide concentration range. The system is found to be considerably more complex than had been assumed previously. A total of 13 different anions are identified of which only five have previously been identified in magic acid. With increasing SbF5 contents the concentration of monomeric anions like [SbF6]-, [SbF5(SO3F)]-, cis- and trans-[SbF4(SO3F)2]-, and mer-[SbF3(SO3F)3]- gradually decreases. Except for [Sb2F11]-, which is present in very small concentrations only, the formation of oligomers involves exclusively μ-fluorosulfato bridges. In addition to donor (SO3F)- and acceptor (SbF5) complex formation to give [SbF5(SO3F)]- and possibly ligand redistribution, the solvolysis of SbF5 or SbF4(SO3F) in HSO3F appears to be the principal formation reaction for polyfluorosulfatofluoroantimonate(V) anions. In glass (NMR tubes) the solvolysis product HF is converted to the oxonium ion [H3O]+, which has previously been identified by 1H NMR and structurally characterized as [H3O][Sb2F11] by us.Key words: magic acid, conjugate superacid, fluorosulfuric acid, 19F NMR spectra.

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Study of the biologically active acyclic ureas by nuclear magnetic resonance

Bulletin of the Karaganda University Chemistry series ◽

10.31489/2020ch4/60-74 ◽

2020 ◽

Vol 100 (4) ◽

pp. 60-74

Author(s):

А.А. Bakibaev ◽

◽

М.Zh. Sadvakassova ◽

V.S. Malkov ◽

R.Sh. Еrkasov ◽

...

Keyword(s):

Nuclear Magnetic Resonance ◽

Magnetic Resonance ◽

Functional Groups ◽

13C Nmr ◽

Nmr Spectra ◽

Chemical Shifts ◽

Biologically Active ◽

Resonance Spectroscopy ◽

13C Nmr Spectra ◽

Nuclear Magnetic

A wide variety of acyclic ureas comprising alkyl, arylalkyl, acyl, and aryl functional groups are investigated by nuclear magnetic resonance spectroscopy. In general, spectral characteristics of more than 130 substances based on acyclic ureas dissolved in deuterated dimethyl sulfoxide at room temperature are studied. The re-sults obtained based on the studies of 1H and 13C NMR spectra of urea and its N-alkyl-, N-arylalkyl-, N-aryl- and 1,3-diaryl derivatives are presented, and the effect of these functional groups on the chemical shifts in carbonyl and amide moieties in acyclic urea derivatives is discussed. An introduction of any type of substitu-ent (electron-withdrawing or electron-donating) into urea molecule is stated to result in a strong upfield shift in 13C NMR spectra relatively to unsubstituted urea. A strong sensitivity of NH protons to the presence of acyl and aryl groups in nuclear magnetic resonance spectra is pointed out. In some cases, qualitative depend-encies between the chemical shifts in the NMR spectra and the structure of the studied acyclic ureas are re-vealed. A summary of the results on chemical shifts in the NMR spectra of the investigated substances allows determining the ranges of chemical shift variations of the key protons and carbon atoms in acyclic ureas. The literature describing the synthesis procedures are provided. The results obtained significantly expand the methods of reliable identification of biologically active acyclic ureas and their metabolites that makes it promising to use NMR spectroscopy both in biochemistry and in clinical practice.

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Peak Estimation of Univariate Spectraby the Best L1 Piecewise Monotonic Approximation Method

WSEAS TRANSACTIONS ON SYSTEMS AND CONTROL ◽

10.37394/23203.2020.15.48 ◽

2020 ◽

Vol 15 ◽

Keyword(s):

Nuclear Magnetic Resonance ◽

Magnetic Resonance ◽

Least Squares ◽

Approximation Method ◽

Nmr Spectra ◽

Inorganic Compound ◽

Piecewise Monotonic ◽

Inherent Problem ◽

New Algorithms ◽

Nuclear Magnetic

We consider applications of the best L1 piecewise monotonic approximation method for the peak estimation of three sets of up to 2500 measurements of Raman, Infrared and Nuclear Magnetic Resonance (NMR)spectra. Peak estimation is an inherent problem of spectroscopy. The location of peaks and their intensities arethe signature of a sample of an organic or an inorganic compound. The diversity and the complexity of our measurements makes it a difficult test of the effectiveness of the method. We find that the method identifies efficientlypeaks and we compare to the results obtained by the analogous least squares calculations. These results havemany similarities and occasionally considerable differences due to both properties of the norms employed in theoptimization calculations and nature of the spectra. Our results may be helpful to subject analysts as part of theinformation on which decisions will be made for estimating peaks in sequences of spectra and to the developmentof new algorithms that are particularly suitable for peak estimation calculations.

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Determination and Identification of Chondroitin Sulfate from Tilapia Byproducts

Advanced Materials Research ◽

10.4028/www.scientific.net/amr.690-693.1318 ◽

2013 ◽

Vol 690-693 ◽

pp. 1318-1321 ◽

Cited By ~ 2

Author(s):

Zhen Hua Duan ◽

Chang Yu Cheng ◽

Yang Hai ◽

Ju Lan Wang

Keyword(s):

Nuclear Magnetic Resonance ◽

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Magnetic Resonance ◽

Chondroitin Sulfate ◽

Infrared Spectra ◽

Oreochromis Niloticus ◽

High Performance ◽

Nmr Spectra ◽

Ir And Nmr Spectra

In order to probe the structure of chondroitin sulfate (CS) from tilapia fish, the CS was extracted from tilapia (Oreochromis niloticus) byproducts with the combination of ultrasonic and microwave, some means including high performance liquid chromatography (HPLC), infrared spectra (IR) and nuclear magnetic resonance (NMR) were used in this paper. The data of HPLC exhibited that the obtained chondroitin sulfate is of highly purity (98.78%). IR and NMR spectra indicated that the sample consisted of both chondroitin-4-sulfate and chondroitin-6-sulfate, and the proportion of chondroitin-6-sulfate was higher than chondroitin-4-sulfate.

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Synthesis of plantamajoside, a bioactive dihydroxyphenylethyl glycoside from Plantago major L.

Holzforschung ◽

10.1515/hf.2006.081 ◽

2006 ◽

Vol 60 (5) ◽

pp. 492-497 ◽

Cited By ~ 2

Author(s):

Toshinari Kawada ◽

Yuko Yoneda ◽

Ryuji Asano ◽

Ippei Kan-no ◽

Walther Schmid

Keyword(s):

Nuclear Magnetic Resonance ◽

Magnetic Resonance ◽

Total Synthesis ◽

Caffeic Acid ◽

Spectral Data ◽

Natural Compound ◽

Plantago Major ◽

Target Compound ◽

Sugar Esters ◽

Nuclear Magnetic

Abstract The first total synthesis of plantamajoside (1), 2-(3′,4′-dihydroxylphenyl)ethyl-4-O-caffeoyl-3-O-(β-D-glucopyranosyl)-β-D-glucopyranoside, which is one of the dihydroxyphenylethyl glycosides (caffeic acid sugar esters), is described. Key intermediate 2, 2-[3′,4′-bis(O-benzyl)phenyl]ethyl 2,6-di-O-acetyl-4-O-[3′,4′-bis(O-benzyl)caffeoyl]-β-D-glucopyranoside was glycosylated with trichloroacetoimidoyl 2,3,4,6-tetra-O-acetyl-α-D-glycopyranoside (3) to afford plantamajoside derivative 4a, 2-[3′,4′-bis(O-benzyl)phenyl]ethyl 2,6-di-O-acetyl-4-O-[3′,4′-bis(O-benzyl)caffeoyl]-3-O-(2,3,4,6-tetra-O-acetyl-β-D-glucopyranosyl)-β-D-glucopyranoside, in 39% yield. Plantamajoside derivative 4a was successfully converted into the target compound, plantamajoside (1), through a series of de-protective procedures. 1H- and 13C nuclear magnetic resonance (NMR) spectral data of the synthesized plantamajoside (1) were identical to those of the natural compound.

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