• Title/Summary/Keyword: 1D%2F2D-NMR

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Solution-State Structure of Native Coenzyme F430 by NMR Methods

  • 원호식;Karl D. Olson;박지석;Ralph S. Wolfe;Dennis R. Hare;Michael F. Summers
    • Bulletin of the Korean Chemical Society
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    • v.16 no.7
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    • pp.649-653
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    • 1995
  • Solution-state structure of native F430 was determined by using NMR methods and NMR-based distance geometry (DG) computations. Structures were generated with loose NOE-derived interproton distance restraints (2.0-2.5 Å, 2.0-3.5 Å and 2.0-4.5 Å for strong, medium, and weak NOE cross-peak intensities, respectively). 2D NOESY back-calculations of structures were subsequently carried out for establishing the consistence between experimental data and DG-model structures. The back-calculated 2D NOESY spectra of resulting DG structures were well consistent with experimental 2D NOESY spectra. Superposition of 20 independent structures with macrocyclic ring atoms and all atoms of F430 afforded pairwise root mean square deviations (RMSD) of 0.025-0.125 Å and 0.64-1.3 Å, respectively. The macrocyclic rings of structures are well converged to a unique conformation with saddle-shaped deformation whereas most of side chains are not converged. The average dihedral angle (N1-N2-N3-N4, 27.78±1.50°) of 20 DG-structures exhibits that the macrocyclic ring conformation is puckered as much as 12,13-diepimeric F430 (28.75±4.07°).

Toxic Evaluation and Chromatographic Analysis of Cucurbitacin D and F from Sorbaria sorbifolia (쉬땅나무(Sorbaria sorbifolia) 성분으로서 cucurbitacin D, F의 독성평가 및 정량)

  • Lee, Sang-Myung;Lee, Cheal-Gyu
    • Analytical Science and Technology
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    • v.14 no.2
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    • pp.191-195
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    • 2001
  • Cucurbitacin D and F, the protostane type triterpenoid of S. sorbifolia, were isolated with chromatograpic method and used as the standard substances for quantitative analysis. The compounds were identified with $^1H$-NMR, FAB-MS and UV spectrophotometer. They were separated on YMC-Pack ODS-AQ(303)[$250{\times}4.6mm$ I.D., $S-5{\mu}m$, 120A] column by HPLC. Cucurbitacin F was detected at 10.73mg/kg in cortex of S. sorbifolia, but cucurbitacin D was not. The compounds were shown to exihibit significant cytotoxicity($ED_{50}$<$0.1{\mu}g/mL$) against several tumor cell lines and acute toxicity(cucurbitacin D: 4.7mg/kg/day, cucurbitacin F: 2.5mg/kg/day) against BDF-1 mouse.

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Complete assignments of $^{1}H$ and $^{13}C NMR$ spectra of Chivosazole F

  • Park, Jung-Rae;Jongheonn Shin;Kim, Jin-Cheol;Ahn, Jong-Woong
    • Journal of the Korean Magnetic Resonance Society
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    • v.5 no.2
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    • pp.91-98
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    • 2001
  • The $^1$H and $^{13}$ C NMR spectra of chivosazole F from Sorangium cellulosum were completely assigned by a combination of ID and 2D NMR techniques. The configurations of double bonds were confirmed from the ROESY spectra. The stereochemistry at asymmetric carboncenters was partially assigned on the basis of the results of NOE analysis.

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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.

NMR Studies on Ferrocytochrome $C_3$ and its Interaction with Ferredoxin I

  • Kim, Andre;Park, Jang-Su
    • Journal of the Korean Magnetic Resonance Society
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    • v.3 no.1
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    • pp.12-26
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    • 1999
  • The 1H NMR signals of the heme methyl, propionate and related chemical groups of cytochrome C3 from Desulfovibrio vulgaris Miyazaki F (D.v. MF) were assigned by means of 1D NOE, 2D DQFCOSY and 2D TOCSY spectra. They were consistent with the assignments of the hemes with the highest and second-lowest redox potentials reported by Gayda et al. [Reference: 15]. The heme assignments were also supported by NOE between the methyl groups of these hemes and the side chain of Val-18, All the results contradicted the heme assignments for D.v. MF cytochrome C3 made on the basis of NMR [Reference: 11]. Based on these assignments, the interaction of cytochrome C3 with ferredoxin I was investigated by NMR. The major interaction site of cytochrome C3 was identified as the heme with the highest redox potential, which is surrounded by the highest density of positive charges. The stoichiometry and association constant were two cytochrome C3 molecules per monomer of ferredoxin I and 108 M-2 (at 53 mM ionic strength and $25^{\circ}C$), respectively.

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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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Effects of Media and Elicitor on Betalain and Phytolaccosides Production in Hairy Root Cultures of Phytolacca esculenta van Houtte (자리공(Phytolacca esculenta van Houtte) 모상근의 Betalain 및 Phytolaccosides 생성에 미치는 배지 및 Elicitor 영향)

  • 양덕조;김용해;윤길영
    • Korean Journal of Plant Tissue Culture
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    • v.25 no.6
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    • pp.507-514
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    • 1998
  • The effects of media and elicitors on betalain, phytolaccoside G and D2 production were examined in the hairy roots of Phytolacca esculenta van Houtte induced by Agrobacterium tumefaciens $A_4$T. Phytolaccoside G and D2 from Phytolacca hairy roots PEH2 were identified by TLC, HPLC, IR, Mass, $^1$H-NMR, and ^(13)C-NMR. Among the culture media tested, SH medium was the best for hairy root growth of hairy roots. White medium was the most suitable medium for betalain production, while MS medium was for phytolaccoside G and D2 production. Although the growth of hairy roots was supped by light (1,000 Lux), the production of betalain, phytolaccoside G and D2 was enhanced by the same light treatment. Addition of elicitors such as NaF, chitosan, and yeast extract to the culture medium increased the content of betalain, phytolaccoside G and D2, suggesting the importance of culture condition for the production of those componds.

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A New Steroidal Glycoside from Allium macrostemon Bunge

  • Kim, Yun Sik;Cha, Joon Min;Kim, Dong Hyun;Lee, Tae Hyun;Lee, Kang Ro
    • Natural Product Sciences
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    • v.24 no.1
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    • pp.54-58
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    • 2018
  • A phytochemical investigation of Allium macrostemon Bunge (Liliaceae) afforded the new pregnane steroidal glycoside, named allimacroside F (1), along with three known glycosides, benzyl-O-${\alpha}-{\text\tiny{L}}$-rhamnopyranosyl-($1{\rightarrow}6$)-${\beta}-{\text\tiny{D}}$-glucopyranoside (2), phenylethyl-O-${\alpha}-{\text\tiny{L}}$-rhamnopyranosyl-($1{\rightarrow}6$)-${\beta}-{\text\tiny{D}}$-glucopyranoside (3), (Z)-3-hexenyl-O-${\alpha}-{\text\tiny{L}}$-rhamnopyranosyl-($1{\rightarrow}6$)-${\beta}-{\text\tiny{D}}$-glucopyranoside (4). The identification and structural elucidation of a new compound (1) was carried out based on spectral data analyses ($^1H-NMR$, $^{13}C-NMR$, $^1H-^1H$ COSY, HSQC, HMBC, and NOESY) and HR-FAB-MS.

Synthesis and Properties of Anionic Tetrakis(pentafluorophenyl)indium(Ⅲ) Complexes (Tetrakis(pentafluorophenyl)indium(Ⅲ) 음이온 착물의 합성과 특성)

  • Choi, Zel Ho
    • Journal of the Korean Chemical Society
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    • v.43 no.1
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    • pp.52-57
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    • 1999
  • The anionic complexes, [ln($C_6F_5)_4$]-, which are thermal and moisture sensitive, have been prepared by the reaction of In($C_6F_5)_3{\cdot}D(D=CH_3CN$, O($C_2H_5)_2$) with the system ($CH_3)_3SiC_6F_5$/CsF, $C_6F_5$MgBr or Cd($C_6F_5)_2$. The stable anionic indium(III) complexes are obtained through cation exchange with PNPCI ([PNP]= bis(triphenylphosphino)ammonium). The pure substance is obtained by column chromatography. These new anionic complexes are unambiguously identifed by NMR-spectroscopy, IR spectroscopy, molecular weight, DTA/TG and elemental analysis.

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Cytotoxic Anthraquinones and Stilbenes from Reynoutria sachalinensis (Fr. Schm.) Nakai

  • Jin, Wenyi;Na, Min-Kyun;Song, Gyu-Yong;Lee, Young-Mi;Bae, Ki-Hwan
    • Korean Journal of Medicinal Crop Science
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    • v.13 no.2
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    • pp.80-84
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    • 2005
  • Five known anthraquinones, physcion (1), I-O-methylemodin (2), emodin (3), $physcion-8-O-{\beta},-D-glucopyranoside$ (5), $emodin-8-O-{\beta},-D-glucopyranoside$ (6) and two known stilbenes, trans-resveratrol (4), $trans-resveratrol-3-O-{\beta},-D-glucopyranoside$ (7) were isolated from MeOH extract of Reynoutria sachalinensis (Polygonaceae). All structures were unambiguously established by 1D and 2D NMR and MS data and the compounds were evaluated for their cytotoxicity against L1210, HL-60, BI6F10 tumor cell lines in MTT assay. Among the compounds, trans-resveratrol (4) exhibited significant cytotoxic activity with $IC_{50}$ values of 9.2, 6.7 and $9.8\;{\mu}g/ml$, against the test cell lines respectively, but compounds 1-3 exhibited the moderate cytotoxic activity.