• Title/Summary/Keyword: $^{13}$C NMR

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1H, 15N and 13C resonance assignment and secondary structure prediction of ss-DNA binding protein 12RNP2 precursor, HP0827 from Helicobacter pylori

  • Jang, Sun-Bok;Ma, Chao;Chandan, Pathak Chinar;Kim, Do-Hee;Lee, Bong-Jin
    • Journal of the Korean Magnetic Resonance Society
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    • v.15 no.1
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    • pp.69-79
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    • 2011
  • HP0827 has two RNP motif which is a very common protein domain involved in recognition of a wide range of ssRNA/DNA.We acquired 3D NMR spectra of HP0827 which shows well dispersed and homogeneous signals which allows us to assign 98% of all $^1H_N$, $^{15}N$, $^{13}C_{\alpha}$, $^{13}C_{\beta}$ and $^{13}C$=O resonances and 90% of all sidechain resonances. The sequence-specific backbone resonance assignment of HP0827 can be used to gain deeper insights into the nucleic acids binding specificity of HP0827 in the future study. Here, we report secondary structure prediction of HP0827 derived from NMR data. Additionally, ssRNA/DNA binding assay studies was also conducted. This study might provide a clue for exact function of HP0827 based on structure and sequence.

NMR Studies on the Structure of Human Annexin I

  • Han, Hee-Yong;Bang, Keun-Su;Na, Doe-Sun;Lee, Bong-Jin
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1996.04a
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    • pp.182-182
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    • 1996
  • Annexin I is a member of the annexin family of calcium dependent phospholipid binding proteins and has anti-inflammatory activity by inhibiting phospholipase A$_2$ (PLA$_2$). Recent X-ray crystallographic study of annexin I identified six Ca$\^$2+/ binding bites, which was different types (type II, III) from the well-known EF-hand motif (type I). In this work, the structure of annexin I was studied at atomic level by using $^1$H, $\^$15/N and $\^$l3/C NMR(nuclear magnetic resonance) spectroscopy, and the effect of Ca$\^$2+/ binding on the structure of annexin I was studied, and compared with that of Mg$\^$2+/ binding, When Ca$\^$2+/ was added to annexin I, NMR peak change was occured in high- and low-field regions of $^1$H-NMR spectra. NMR peak change by Ca$\^$2+/ binding was different from that by Mg$\^$2+/ binding. Because annexin I is a larger protein with 35 kDa molecular weight, site-specific (amide-$\^$15/N, carbonyl-$\^$l3/C) labeling technique was also used. We were able to detect methionine, tyrosine and phenylalanine peaks respectively in $\^$13/C-NMR spectra, and each residue was able to be assigned by the method of doubly labeling annexin I with [$\^$13/C] carbonyl-amino acid and [$\^$15/N] amide-amino acid. In $\^$l3/C-NMR spectra of [$\^$13/C] carbonyl-Met labeled annexin I, we observed that methionine residues spatially located near Ca$\^$2+/ binding Sites Were Significantly effected by Ca$\^$2+/ binding. From UV spectroscopic data on the effect of Ca$\^$2+/ binding, we knew that Ca$\^$2+/ binding sites of annexin I have cooperativity in Ca$\^$2+/ binding. The interaction of annexin I with PLA$_2$ also could be detected by using heteronuclear NMR spctroscopy. Consequently, we expect that the anti-inflammatory action mechanism of annexin I may be a specific protein-protein interaction. The residues involved in the interaction with PLA$_2$ can be identified as active site by assigning NMR peaks effected by PLA$_2$ binding.

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Easy-to-execute 'One-pot' Synthesis of 1,2,4,5-Tetrazines Catalyzed by Activated Fly Ash (활성화된 비산회 촉매를 이용하여 간단히 수행된 1,2,4,5-Tetrazines의 One-pot 합성)

  • Gopalakrishnan, M.;Thanusu, J.;Kanagarajan, V.
    • Journal of the Korean Chemical Society
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    • v.51 no.6
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    • pp.520-525
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    • 2007
  • Three-component coupling of thiourea/urea, various structurally diverse aromatic aldehydes and ammonium acetate is catalyzed by activated fly ash in dry media under microwave irradiation to give 6-aryl-1,2,4,5-tetrazinan- 3-thiones/ones in good yields. The structure of 6-aryl-1,2,4,5-tetrazinan-3-thiones/ones have been elucidated on the basis of their melting points, elemental analysis, MS, IR, 1H NMR, D2O exchange, 13C NMR and two dimensional NMR spectral studies including Homonuclear Correlation (HOMOCOR) and Heteronuclear Single Quantum Correlation (HSQC) spectra.

Comparison of Metal Cleaning Effect on Pt Particles Supported on Carbon and Pt Black Observed by NMR, CV, and TEM

  • Han, Kee-Sung;Han, Oc-Hee
    • Journal of the Korean Magnetic Resonance Society
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    • v.6 no.1
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    • pp.38-44
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    • 2002
  • 60% Pt on Vulcan XC-72 with similar Pt sizes to fuel cell grade Pt black was investigated by $\^$13/C nuclear magnetic resonance spectroscopy (NMR), cyclic voltammery (CV), transmission electron microscopy (TEM). Experiments were carried out on electrochemically cleaned samples as well as as-received. The TEM and CV results showed that the average particle sizes were changed by cleaning. However, the chemical shift ($\delta$$\_$G/) of $\^$13/C of $\^$13/CO absorbed on Pt surfaces did not show any appreciable variation with particle size change as did in Pt black. These results indicate that a combination of different analytic techniques is essential to understand the properties of the metal particle catalysts and that the presence of carbon black support strongly influences the NMR data, probably through metal-support interaction.

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$^{13}C$nmr Studies on the Interaction of Lithium Salts to Formamide, Acetamide and Propionamide Systems (Formamide, Acetamide 및 Propionamide계에 대한 리튬염의 상호작용에 관한 $^{13}C$ nmr 연구)

  • Dae-Ho Shin;Jo W. Lee;Young Sang Choi
    • Journal of the Korean Chemical Society
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    • v.26 no.5
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    • pp.291-295
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    • 1982
  • $^{13}C$resonances of carbonyl and various alkyl groups in amides are found to shift down-field on the interaction with lithium salts and it is shown that lithium ion binds directly to the carbonyl group in amides. The magnitudes of the $^{13}C$ chemical shifts of various amides depend not only on the size of alkyl groups in amides but also on the interaction with anion. The change of $^{13}C$chemical shift of amide in LiCl is smaller than that in$LiClO_4$ due to the difference of the charge density of the anion.

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Phenolic Compounds from Frullania nisquallensis

  • Kim, Youn-Chul;Kingston, David G.I.
    • Korean Journal of Pharmacognosy
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    • v.26 no.3
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    • pp.248-252
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    • 1995
  • Five phenolic compounds were isolated from the MeCOEt extract of Frullania nisquallensis (Jubulaceae), namely methyl 2,4-dihydroxy-3,6-dimethylbenzoate, methyl 2,4-dihydroxy-6-methylbenzoate, acacetin, betuletol, and pectolinaringenin. Revised ${13}^C-NMR$ data of methyl 2,4-dihydroxy-6-methylbenzoate and betuletol are reported.

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$^{13}C$ NMR Studies of the Chelate Ring Opening-Closing Process in (Nitrilotriacetato)vanadate(V) dioxovandate(V) Ion

  • Lee, Man-Ho;Schaumburg, Kjeld
    • Bulletin of the Korean Chemical Society
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    • v.11 no.5
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    • pp.399-402
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    • 1990
  • Activation parameters of the exchange between two types of glycinate groups in (nitrilotriacetato)dioxovanadate(V) ion, $[VO_2(NTA)]^{2-}$, have been determined as the results of $^{13}C$ NMR measurements over a range of temperatures between 277 and 306$^{\circ}K$. The exchange mechanism is proposed on the basis of the chelate ring opening-closing process, assuming rupture of the metal-oxygen (glycinate) bond trans to V = O bond to give a five-coordinated intermediate.

Panaxyne epoxide, A New Cytotoxic Polyyne from Panax ginseng Root against L210 Cells

  • Kim, Shin-Il;Kang, Kyu-Sang;Lee, You-Hui
    • Archives of Pharmacal Research
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    • v.12 no.1
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    • pp.48-51
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    • 1989
  • A new polyacetylene compound with cytotoxic activity against L1210 cells having diyne-ene and epoxy moiety, named panaxyne epoxide, was isolated from Panax ginseng C.A. Meyer. The chemical structure of the polyacetylene was determined to be tetradeca-13-ene-1,3-diyne-6,7-epoxide by UV, IR, $^1H-NMR,\;^{l3}$C-NMR and mass spectra.

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Characterization of Humic Acid in the Chemical Oxidation Technology(II) - Characteristics by Ozonation - (화학적 산화법에 의한 부식산의 분해처리 기술에 관한 연구(II) - 오존처리에 따른 분해특성 분석 -)

  • Rhee, Dong Seok;Jung, Young-Rim
    • Analytical Science and Technology
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    • v.13 no.2
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    • pp.241-249
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    • 2000
  • In this paper, ozonation of humic acid in water was characterized using $UV_{254}$ absorbance, TOC, Ultra Filtration and $^{13}C-NMR$. Also, carbonyl compounds in ozonated water were analyzed by GC/MS using PFBOA method. Ozonation by-products of water containing humic acid were determined as formaldehyde, acetaldehyde, acetone, glyoxal and methylglyoxal. Results of $UV_{254}$ absorbance and TOC with ozonation time at humic acid 20, 100ppm represent that decrease rate of 80% within ozonation time is 20 min and TOC removal rate of 40-50% within ozonation time is 30 min. Results for $^{13}C-NMR$ and Ultra Filtration, humic acid of high molecular weight by ozonation are oxidated and decomposed so that it was conversed low molecular weight such as aldehydes, carboxylic acid.

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Developing 500 MHz NB 19F-13C Double Resonance Solid-State NMR Probe for in-situ Analysis of Liquid Crystal Display Panels

  • Choi, Sung-Sub;Jung, Ji-Ho;Park, Yu-Geun;Park, Tae-Joon;Park, Gregory Hyung-Jin;Kim, Yong-Ae
    • Bulletin of the Korean Chemical Society
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    • v.33 no.5
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    • pp.1577-1580
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    • 2012
  • The orientational and dynamic behavior of liquid crystal molecules on the alignment layer surfaces of liquid crystal display (LCD) devices is crucial to their performance, but there are only a few methods of experimentally elucidating the interactions between the liquid crystals and the alignment layers. Inspired by the natural and technical similarities between membrane proteins in lipid bilayers and liquid crystals in LCDs, we employed solid-state NMR methodologies originally developed for the study of membrane proteins in lipid bilayers for the in-situ analysis of liquid crystal display panels. In this article, we present a home-built 500 MHz narrowbore (NB) The orientational and dynamic behavior of liquid crystal molecules on the alignment layer surfaces of liquid crystal display (LCD) devices is crucial to their performance, but there are only a few methods of experimentally elucidating the interactions between the liquid crystals and the alignment layers. Inspired by the natural and technical similarities between membrane proteins in lipid bilayers and liquid crystals in LCDs, we employed solid-state NMR methodologies originally developed for the study of membrane proteins in lipid bilayers for the in-situ analysis of liquid crystal display panels. In this article, we present a home-built 500 MHz narrowbore (NB) $^{19}F-^{13}C$ double resonance solid-state NMR probe with a flat-square coil and the first application of this probe for the in-situ analysis of LCD panel samples. double resonance solid-state NMR probe with a flat-square coil and the first application of this probe for the in-situ analysis of LCD panel samples.