• Title/Summary/Keyword: 2-D NMR

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Color Alteration and Acaricidal Activity of Juglone Isolated from Caesalpinia sappan Heartwoods Against Dermatophagoides spp.

  • Lee, Chi-Hoon;Lee, Hoi-Seon
    • Journal of Microbiology and Biotechnology
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    • v.16 no.10
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    • pp.1591-1596
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    • 2006
  • Acaricidal effects of materials derived from Caesalpinia sappan heartwoods against Dermatophagoides farinae and D. pteronyssinus were assessed and compared with those evidenced by commercial benzyl benzoate and DEET. The observed responses varied according to dosage and mite species. The $LD_{50}$ values of the methanol extracts derived from C. sappan heartwoods were 6.13 and $5.44{\mu}g/cm^3$ against D. farinae and D. pteronyssinus, respectively. Furthermore, the ethyl acetate fraction derived from the methanol extract was approximately 8.71 more toxic than DEET against D. farinae, and 4.73 times more toxic against D. pteronyssinus. The biologically active constituent from the ethyl acetate fraction of C. sappan heartwood extract was purified via silica gel chromatography and high-performance liquid chromatography. The structure of the acaricidal component was analyzed by $GC-MS,\;^1H-NMR,\;^{13}C-NMR,\;^1H-^{13}C\;COSY-NMR$, and DEPT-NMR spectroscopy, and identified as juglone (5-hydroxy-l,4-naphthoquinone). Based on the $LD_{50}$ values of juglone and its derivatives, the most toxic compound against D. farinae was juglone ($0.076{\mu}g/cm^3$), followed by benzyl benzoate ($9.143{\mu}g/cm^3$) and 2methyl-l,4-naphthoquinone ($40.0{\mu}g/cm^3$). These results indicate that the acaricidal activity of C. sappan heartwoods is likely to be the result of the effects of juglone. Additionally, juglone treatment was shown to effect a change in the color of the cuticles of house dust mites, from colorless-transparent to dark brownish-black. Accordingly, as a naturally occurring acaricidal agent, C. sappan heartwood-derived juglone should prove to be quite 'useful as a potential control agent, lead compound, and house dust mite indicator.

Solution State Structure of pA1, the Mimotopic Peptide of Apolipoprotein A-I, by NMR Spectroscopy

  • Kim, Hyo-Joon;Won, Ho-Shik
    • Bulletin of the Korean Chemical Society
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    • v.32 no.9
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    • pp.3425-3428
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    • 2011
  • Apolipoprotein A-I (Apo A-I) is a major component for high density lipoproteins (HDL). A number of mimetic peptides of Apo A-I were screened from the phase-displayed random peptide library by utilizing monoclonal antibodies (A12). Mimetic peptide for A12 epitope against Apo A-I was selected as CPFARLPVEHHDVVGL (pA1). From the BLAST search, the mimetic peptide pA1 had 40% homology with Apo A-I. As a result of the structural determination of this mimotope using homo/hetero nuclear 2D-NMR techniques and NMR-based distance geometry (DG)/molecular dynamic (MD) computations, DG structure had low penalty value of 0.3-0.7 ${\AA}^2$ and the total RMSD was 0.6-1.6 ${\AA}$. The mimotope pA1 exhibited characteristic conformation including a ${\beta}$-turn from Pro[7] to His[11].

In Vivo $^{13}C$-NMR Spectroscopic Study of Polyhydroxyalkanoic Acid Degradation Kinetics in Bacteria

  • Oh, Jung-Sook;Choi, Mun-Hwan;Yoon, Sung-Chul
    • Journal of Microbiology and Biotechnology
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    • v.15 no.6
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    • pp.1330-1336
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    • 2005
  • Polyhydroxyalkanoic acid (PHA) inclusion bodies were analyzed in situ by $^{13}C$-nuclear magnetic resonance ($^{13}C$-NMR) spectroscopy. The PHA inclusion bodies studied were composed of poly(3-hydroxybutyrate) or poly(3hydroxybutyrate-co-4-hydroxybutyrate), which was accumulated in Hydrogenophaga pseudoflava, and medium-chain-length PHA (MCL-PHA), which was accumulated in Pseudomonas fluorescens BM07 from octanoic acid or 11-phenoxyundecanoic acid (11-POU). The quantification of the $^{13}C$-NMR signals was conducted against a standard compound, sodium 2,2-dimethyl-2-silapentane-5-sulfonate (DSS). The chemical shift values for the in vivo NMR spectral peaks agreed well with those for the corresponding purified PHA polymers. The intracellular degradation of the PHA inclusions by intracellular PHA depolymerase(s) was monitored by in vivo NMR spectroscopy and analyzed in terms of first-order reaction kinetics. The H. pseudoflava cells were washed for the degradation experiment, transferred to a degradation medium without a carbon source, but containing 1.0 g/l ammonium sulfate, and cultivated at $35^{\circ}C$ for 72 h. The in vivo NMR spectra were obtained at $70^{\circ}C$ for the short-chain-length PHA cells whereas the spectra for the aliphatic and aromatic MCL-PHA cells were obtained at $50^{\circ}C\;and\;80^{\circ}C$, respectively. For the H. pseudoflava cells, the in vivo NMR kinetics analysis of the PHA degradation resulted in a first-order degradation rate constant of 0.075/h ($r^{2}$=0.94) for the initial 24 h of degradation, which was close to the 0.050/h determined when using a gas chromatographic analysis of chloroform extracts of sulfuric acid/methanol reaction mixtures of dried whole cells. Accordingly, it is suggested that in vivo $^{13}C$-NMR spectroscopy is an important tool for studying intracellular PHA degradation in terms of kinetics.

Scalaran-type sesterterpenes from a Marine Sponge Smenospongia species showing the AMPK activation

  • Hwang, Buyng-Su;Rho, Jung-Rae
    • Journal of the Korean Magnetic Resonance Society
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    • v.16 no.1
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    • pp.1-10
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    • 2012
  • A new scalaran class sesterterpenoid with five known ones was isolated from a marine sponge Smenospongia species collected from the Gageo island, Korea. Chemical structure of all of compounds was determined on the basis of a combination of extensive 1D and 2D NMR experiments and MS data. The new compound exhibited a new functional group on a common scalaran sesterterpene skeleton, identified as 12-deacetoxy-23-deacetoxyscalarin. The compound 1 moderately showed the effect of the activation of AMP-activated protein kinase (AMPK) in L6 myoblast cell.

Partial Assignment of Heme Groups of Cytochrome $c_3$ of Desulfovibrio vulgaris Miyazaki F by $^{1}H$-NMR

  • Jang-Su Park;Shin Won Kang
    • Bulletin of the Korean Chemical Society
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    • v.14 no.5
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    • pp.588-592
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    • 1993
  • The $^1H-NMR$ signals of the heme methyl, propionate and related chemical groups of cytochrome $c_3$ from Desulfovibrio vulgaris Miyazaki F (D.v. MF) were site-specifically assigned by means of 1D-NOE, 2D-DQFCOSY and 2D-TOCSY spectra. They were consistent with the site-specific assignments of the hemes with the highest and second-lowest redox potentials reported by Fan et al. (Biochemistry, 29, 2257-2263 1990). The site-specific heme assignments were also supported by NOE between the methyl groups of these hemes and the side chain of Val-18.

Extractives from the barks of Querus acutissima and Quercus variabilis (상수리나무(Querus acutissima)와 굴참나무(Querus vcariabilis) 수피의 추출성분)

  • 김진규;이상극;함연호;배영수
    • Journal of Korea Foresty Energy
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    • v.21 no.1
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    • pp.41-48
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    • 2002
  • The barks of oak trees (Quercus acutissima and Quercus variabilis) were collected, extracted with acetone-$H_2O$ (7:3, v/v), fractionated with hexane, $CH^2C1^2$ EtOAc and -$H_2O$, then freeze dried to give dark brown powder. The EtOAc soluble mixtures of the trees were chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-hexane mixture as eluents. The structures of isolated compounds were characterized by $^1H$, $^13C$ and 2D-NMR spectroscopy and molecular weights were determined by FAB-MS spectra. The isolated compounds from Quercus acutissima were (+)-catechin, (+)-gallocatechin, gallic acid and taxifolin-3-O-$\beta$-D-glucopyranoside and the compounds from Quercus variahilis (+)-catechin, caffeic acid and taxifolin-3-O-$\beta$-D-glucopyranoside.

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($^{11}$B NMR study of vortex dynamics in LuNi$_2$B$_2$C

  • Lee, K.H.;Seo, S.W.;Kim, D.H.;Khang, K.H.;Seo, H.S.;Hwang, C.S.;Cho, B.K.;Lee, Moo-Hee
    • 한국초전도학회:학술대회논문집
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    • v.10
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    • pp.107-110
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    • 2000
  • ($^{11}$B NMR measurements have been performed on single crystals of LuNi$_2$B$_2$C superconductor to investigate vortex lattice structures and dynamical behavior. The spectrum in the superconducting state is significantly broadened by local field inhomogeneity due to the vortex lattice and the peak point of the spectrum shifts toward low magnetic field due to the imperfect field penetration. The linewidth of the spectrum reflecting local field variation is much smaller than expected for conventional vortex lattices and shows peculiar increase at low temperature. Furthermore, the transverse relaxation rate, 1/T$_2$, probing the slow motion of vortices, exhibits a single peak as temperature decreases. These prominent results highlight significant fluctuation of vortices even for this low T$_c$, and nearly isotropic 3D superconductor.

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Mite-Control Activities of Active Constituents Isolated from Pelargonium graveolens Against House Dust Mites

  • Jeon, Ju-Hyun;Kim, Hyung-Wook;Kim, Min-Gi;Lee, Hoi-Seon
    • Journal of Microbiology and Biotechnology
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    • v.18 no.10
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    • pp.1666-1671
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    • 2008
  • The mite-control activities of materials obtained from Pelargonium graveolens oil against Dermatophagoides farinae and D. pteronyssinus were examined using an impregnated fabric disk bioassay and were compared with those shown by commercial benzyl benzoate and N,N-diethyl-m-toluamide (DEET). Purification of the biologically active constituents from P. graveolens oil was done by silica gel chromatography and high performance liquid chromatography. The structures of the active components were analyzed by EI/MS, $^{1}H$-NMR, $^{13}C$-NMR, $^{1}H-^{13}C$ COSY-NMR, and DEPT-NMR spectra, and were identified as geraniol ($C_{10}H_{18}O$, MW 154.25, trans-3,7-dimethyl-2,6-octadien-l-ol) and $\beta$-citronellol ($C_{10}H_{20}O$, MW 156.27, 3,7-dimethyl-6-octen-l-o1). Based on the $LD_{50}$ values, the most toxic compound was geraniol (0.26${\mu}g/cm^{2}$), followed by $\beta$-citronellol (0.28${\mu}g/cm^{2}$), benzyl benzoate (10.03${\mu}g/cm^{2}$), and DEET (37.12${\mu}g/cm^{2}$) against D. farillae. In the case of D. pteronyssinus, geraniol (0.28${\mu}g/cm^{2}$) was the most toxic, followed by $\beta$-citronellol (0.29${\mu}g/cm^{2}$), benzyl benzoate (9.58${\mu}g/cm^{2}$), and DEET (18.23${\mu}g/cm^{2}$). These results suggest that D. farinae and D. pteronyssinus may be controlled more effectively by the application of geraniol and $\beta$-citronellol than benzyl benzoate and DEET. Furthermore, geraniol and $\beta$-citronellol isolated from P. graveolens could be useful for managing populations of D. farinae and D. pterollyssinus.

19F NMR Study of Fluorinated YBa2Cu3O7-x

  • Lee, Cheol-Eui;D. White;P. K. Davies;S. J. Noh
    • Journal of Magnetics
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    • v.2 no.2
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    • pp.35-37
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    • 1997
  • A sample of YBa2Cu3O7-x fluorinated by a high temperature (400$^{\circ}C$) gas exchange technique has been investigated by means of 19F NMR (nuclear magneti resonance) measurements in both superconducting and normal state. As a result, behaviors characteristic of the superconductor, including a peculiarity in the spin-lattice relaxation rate (1/T1) around 250 K, were observed.

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