• Title/Summary/Keyword: $^{13}C$-NMR spectroscopy

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The Chemical Constituents from Unidentified Sponge (해면의 화학적 성분 연구)

  • Park, Seon Gu;Paul J. Scheuer
    • Journal of the Korean Chemical Society
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    • v.38 no.2
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    • pp.169-173
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    • 1994
  • The previously reported cytotoxic metabolites, against the KB cell line, xestoquinone, halenaquinol sulfate and $halenaquinol^{5,6}$ were isolated from the unidentified sponge collected in October 1992, Manado Bay, Sulawesi in Indonesia. Their structure were elucidated by $^1H-,\;^{13}C$-NMR, $^1H-,\;^{13}C$(1 bond) Heteronuclear Multiple Quantum Coherence Spectroscopy$(HMQC)^1$, $^1H-,\;^{13}C$C(2 and 3 bond) Heteronuclear multiple Bond Correlation Spectroscopy$(HMBC)^2$, Electron Impact Mass Spectroscopy(EI ms), Ultraviolet Spectroscopy(UV), and Infrared Spectroscopy(IR)

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The Chemical Constituents from the Sponge Spongia sp. (해면 Spongia sp.의 화학적 성분 연구)

  • Park, Sun-Ku;Oh, Chang-Sok;Scheuer, Paul-J.
    • Journal of the Korean Chemical Society
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    • v.39 no.4
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    • pp.301-305
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    • 1995
  • The cytotoxic metabolites, against the KB cell line, halenaquinone, epispongiatriol and aldisin were isolated from the sponge Spongia sp. collected in September 1992, Manado Bay, Sulawesi in Indonesia. Their structures were elucidated by 1H, 13C NMR, 1H 13C(1 bond) Heteronuclear Multiple Quantum Coherence Spectroscopy (HMQC), 1H 13C(2 and 3 bond) Heteronuclear Multiple Bond Correlation Spectroscopy (HMBC), Electron Impact Mass Spectroscopy (EI ms) and Infrared Spectroscopy (IR).

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Characterization of Kraft Lignin by 13C-Nuclear Magnetic Resonance Spectroscopy (13C-NMR에 의한 크라프트 리그닌의 특성)

  • Lee, Beom-Goo;Hwang, Byung-Ho
    • Journal of the Korean Wood Science and Technology
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    • v.17 no.4
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    • pp.44-56
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    • 1989
  • To recover much residual lignin from the black liquor of kraft pulp. the black liquor was extracted and purified with many organic solvents. Many kinds of lignins were isolated from each fraction obtained and the characteristics of these lignins investigated by $^{13}C$-NMR spectroscopy. If M$\ddot{o}$rck's method was compared with Kirk's method. M$\ddot{o}$rck's method was better than Kirk's method because the particular signals of each lignin occur more in the former than m the latter. Especially the $^{13}C$-NMR spectrum of the MCS fraction identifies with those of other researchers. The experiment that the kraft lignin from Pinus densiflora S. et Z. found in Korea was investigated by $^{13}C$-NMR spectroscopy was performed first in Korea.

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Characterization and Synthesis of Titanium (IV) Isopropoxide Derivatives (Titanium(IV) isoproxide 유도체의 합성 및 특성연구)

  • Jung, Mie-Won
    • Analytical Science and Technology
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    • v.12 no.6
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    • pp.509-514
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    • 1999
  • The systematic modification of titanium(IV) isopropoxide with acetic acid as a organic additive was done and identifided by FT-IR, $^1H$, $^{13}C$ NMR and UV-Vis spectroscopy. The structure was cbanged after hydrolysis-condensation reaction and drying process. The hydrolysis-condensation rates of modified Ti alkoxide with acetic acid were investigated by $^1H$ NMR spectroscopy. This modified Ti(IV) alkoxide was less reactive toward hydrolysis-condensation reaction than $Ti(OPr^i)_4$, which can be attributed to the stable ligand structure between Ti alkoxide and ligand. The structural change on obtained from gel powders with heat treatment was also observed by FT-IR spectroscopy.

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13C-NMR Spectroscopy of Urea-Formaldehyde Resin Adhesives with Different Formaldehyde/Urea Mole Ratios

  • Park, Byung-Dae;Lee, Sang M.;Park, Jong-Young
    • Journal of the Korean Wood Science and Technology
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    • v.36 no.2
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    • pp.63-72
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    • 2008
  • As a part of abating formaldehyde emission of urea-formaldehyde (UF) resin adhesive, this study was conducted to investigate chemical structures of UF resin adhesives with different formaldehyde/urea (F/U) mole ratios, using carbon-13 nuclear magnetic resonance ($^{13}C$-NMR) spectroscopy. UF resin adhesives were synthesized at four different F/U mole ratios such as 1.6, 1.4, 1.2, and 1.0 for the analysis. The analysis $^{13}C$-NMR spectroscopy showed that UF resin adhesives with higher F/U mole ratios (i.e., 1.6 and 1.4) had two distinctive peaks, indicating the presence of dimethylene ether linkages and methylene glycols, a dissolved form of free formaldehyde. But, these peaks were not detected at the UF resins with lower F/U mole ratios (i.e., 1.2 and 1.0). These chemical structures present at the UF resins with higher F/U mole ratios indicated that UF resin adhesive with higher F/U mole ratio had a greater contribution to the formaldehyde emission than that of lower F/U mole ratio. Uronic species were detected for all UF resins regardless of F/U mole ratios.

The Application of NMR Techniques to the Structural Confirmation of O-Substituted 3,4-Dihydroxyphenylacetic Acid Derivatives

  • Lee, Sueg-Geun;Choi, Joong-Kwon;Park, No-Sang;Hong, Mi-Sook;Ha, Deok-Chan
    • Bulletin of the Korean Chemical Society
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    • v.13 no.1
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    • pp.87-91
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    • 1992
  • The structures of the compounds, 1, 2, 3, and 4, which were precursors of analgesics, were confirmed by modern NMR techniques. The complete $^{13}C-NMR$ assignments of these systems were established by applying COLOC (COrrelated spectroscopy for LOng range Couplings), HETCOR (HETeronuclear CORrelated spectroscopy), RCT (Relay Coherence Transfer), and NOE difference spectroscopy. The limitation of COLOC approach which has been widely used recently is discussed.

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.

Isolation and Structure Determination of Two Furanosesquiterpenes from the Soft Coral Sinularia lochmodes (산호로부터 2개의 푸란노세스키테르펜의 분리와 구조 결정)

  • Park, Seon Gu;Paul J. Scheuer
    • Journal of the Korean Chemical Society
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    • v.38 no.10
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    • pp.749-752
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    • 1994
  • Two furanosesquiterpenes, (5'E)-5-(2',6'-dimethylocta-5',7'-dienyl) furan-3-carboxylic acid (1) and (1'E,5'E)-5-(2',6'-dimethylocta-l',5',7'-trienyl) furan-3-carboxylic acid (2), were isolated from soft coral Sinularia lochmodes collected from Palikir pass at Pohnpei Micronesia, June, 1990 in Hawaii. Their structures were elucidated by $^1H$, $^{13}C$ NMR, Homo-COSY, $^1H$-$^{13}C$ (1 bond) Heteronuclear Multiple Quantum Coherence Spectroscopy (HMQC), $^1H$-$^{13}C$ (2 and 3 bond) Heteronuclear Multiple Bond Coherence Spectroscopy (HMBC), Electron Impact Mass Spectroscopy (EI-ms), and Infrared Spectroscopy (IR).

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Structural Analysis of Petroleum Fractions by Near-Infrared and $^{13}C$-NMR Spectroscopy (근적외선과 $^{13}C$-핵자기 공명 분광학에 의한 석유유분 구조분석)

  • Choi, Ju-Hwan;Kim, Hai-Dong;Choi, Young-Sang
    • Analytical Science and Technology
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    • v.9 no.2
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    • pp.168-178
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    • 1996
  • Molecular structures of petroleum fractions(diesel fuel, bunker-C oil, lubricant base stocks) have been analyzed and compared in terms of the compositions (aromatics, naphtherucs, paraffinics), aromatics(benzene-nuclear and bonded alkyl groups), C2(methylene) carbon atoms % $C_{\alpha}$ and $C_{\beta}$ carbon stom % in alkyl groups and paraffins(branched and normal) by near-infrared and $^{13}C$-NMR spectroscopy.

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