• Journal of the Korean Magnetic Resonance Society
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• v.12 no.2
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• pp.81-88
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• 2008

Solid HETCOR (Hetero-Correlation) requires homo-dipolar decoupling between proton spins during the evolution and the mixing period in 2D-NMR. There are two different ways of achieving it with pulse sequences. One is based on the multiple pulse (MP) sequence where thousands of intense radio frequency (rf) pulses are used to remove the homo-dipolar interaction between protons. The other is utilizing the so-called Lee-Goldburg (LG) off-resonance scheme where a continuous rf-irradiation is used. In this report, the advantage of one technique to the other, is analyzed. LG version is evaluated better in S/N and easier in setup procedure with the same experimental time.

• Archives of Pharmacal Research
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• v.19 no.4
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• pp.302-306
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• 1996

The $^1H- and^{13}C-NMR$ spectra of alaternin, aurantio-obtusin, chryso-obtusin, obtusin and 2-glucosyl obtusifolin isolated from the seeds of Cassia tora have been assigned based on HMBC, long-range HETCOR, fully $^1H-coupled {13}^C-NMR$, deuterium isotope experiment, and by comparison with the model compounds.

• 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.

• Journal of the Korean Wood Science and Technology
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• v.34 no.4
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• pp.76-82
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• 2006

The dried ground needles (2.0 kg) of Chamaecyparis pisifera (Sieb. et Zucc.) Endlicher were extracted with acetone-$H_2O$ (7:3, v/v), concentrated, and fractionated with a series of n-hexane, methylene chloride, ethyl acetate and water on a separation funnel. Each fraction was freeze dried, then a portion of ethyl acetate soluble powder was chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-n-hexane mixture as eluents. The isolated compounds were identified by cellulose TLC, $^1H$-, $^{13}C$-NMR, COSY, HETCOR, FAB and EI-MS. (+)-catechin, taxifolin-3-O-${\beta}$-D-xylopyrano-side, quercetin-3-O-${\alpha}$-L-rhamnopyranoside were isolated from the ethyl acetate soluble fraction of Chamaecypairs pisifera needle. Antioxidative tests on the isolated compounds indicated that all of the compounds showed similar values to ${\alpha}$-tocopherol and BHT as controls.

• Proceedings of the Korean Society of Applied Pharmacology
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• 1998.11a
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• pp.89-94
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• 1998

Marine sponges are recognized as a plentiful source of diverse biologically active secondary metabolites. Recently, we have initiated a research to discover antitumor constituents from the marine sponges collected from Korean Waters. Marine sponges collected from the South Sea of Korea were screened for several biological activities including such as brine shrimp lethality and cytotoxicity. Significant brine shrimp lethality was detected in the crude extract of a two-sponge association of Poecillastra sp. and Jaspis sp. A cross-section of this sample showed two layers of morphologically distinct sponges. The thin and dirty yellow outer layer was identified as Poecillastra sp. (Pachastrellidae), the surface of which was very rough. The light-grey inner layer was identified as Jaspis sp. (Jaspidae), the surface of which was smooth. This two-sponge association appears to be consistent as these sponges were always found in associated form regardless of collection site or collection period. Investigation of the bioactive constituents monitored by brine shrimp lethality assay led to the isolation of pectenotoxin II (PTX2) and psammaplin A as causative compounds for the brine shrimp lethality. $^1$H- and $\^$13/C-nmr signals of PTX2 was fully assigned utilizing TOCSY, HETCOR, Long-range HETCOR, and Homonuclear J-resolved 2D experiments. PTX2 displayed very potent and selective cytotoxicities in the 60 cell line panel antitumor assay at the NCI. PTX2 has progressed to acute toxicity determination and in vivo antitumor assay at the NCI (Table 1). However, significant in vitro antitumor activity of PTX2 can not be affirmed in the in vivo assay.

• Natural Product Sciences
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• v.2 no.2
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• pp.106-114
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• 1996

Four polymethoxyfavones were isolated from the leaves of Citrus deliciosa, three of which (nobiletin, 5-O-demethylnobiletin, and tangeritin) are bioactive. The fourth (7,4'-dihydroxy-5,6,8,3'-tetramethoxyflavone) is reported for the first time in the genus Citrus and is a potential chemotaxonomic marker. The structures of these flavones were confirmed by analysing their spectral data and comparison with similar compounds. The previously reported $^{13}C$ NMR assignment of 5-O-demethylnobiletin has been revised on the basis of 2D NMR experiments (HETCOR, COSY, and COLOC). The chemotaxonomic value of the present finding is verified.

• Journal of the Korean Wood Science and Technology
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• v.34 no.3
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• pp.73-83
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• 2006

The dried needles (1.5 kg) of Abies koreana and Abies holophylla were ground, extracted with acetone-$H_2O$ (7:3, v/v), concentrated, and fractionated with a series of hexane, methylene chloride, ethyl acetate and water on a separatory funnel. Each fraction was freeze dried, then a portion of ethyl acetate soluble powder was chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-hexane mixture as eluents. The isolated compounds were identified by cellulose TLC, $^1H$, $^{13}C-NMR$, COSY, HETCOR, FAB and EI-MS. The needles of Abies koreana and Abies holophylla contained a large amount of aromadendrin-7-O-${\beta}$-D-glucopyranoside (compound III), polydatin (compound VI), (-)-rhododendrol-2-O-${\beta}$-D-glucopyranoside (compound VII), in addition to a small amount of (+)-catechin (compound I), kaempferol-3-O-${\beta}$-D-glucopyranoside (compound IV), myricetin-3-O-${\beta}$-D-glucopyranoside (compound V), naringenin-7-O-${\beta}$-D-glucopyranoside (compound II). DPPH analysis was also tested to investigate the antioxidative effects on the isolated compounds and (+)-catechin and polydatin were effective.

• Journal of the Korean Magnetic Resonance Society
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• v.10 no.1
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• pp.115-125
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• 2006

Hippuryl-L-histidyl-L-leucine(HHL) is widely used as a substrate of angiotensin converting enzyme(ACE) cleaving the neurotransmitter angiotensin(I) to the octapeptide angiotensin(II). The structure of the substrate molecules should provide information regarding the geometric requirements of the ACE active site. For the purpose of determination of in vivo reaction, metallo(Cu, Zn)-HHL complexes were synthesized and the degree of complex formation were identified by MALDITOF, ESI mass spectrometric analysis. Tn addition, the pH-dependent species distribution curves were obtained by potentiometric titration. Nitrogen atoms of imidazole ring and oxygen atom of caboxylate groups in the peptide chain were observed to be participated in the metal complex formation. After purification of complexes further structural characterization were made by utilizing UV-Vis, electrochemical methods and NMR. Complete NMR signal assignments were carried out by using 2D-spectrum techniques COSY, TOCSY, NOESY, HETCOR. A complex that two imidazole and carboxylate groups are asymmetrically participating to coordination mode was predicted to the solution-state structure of $Cu(II)-HHL_2$ based on $^{13}C-NMR$ signal assignment and NOE information.

• Bulletin of the Korean Chemical Society
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• v.27 no.1
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• pp.93-98
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• 2006

Two new compounds 1'-(stigmast-11,20(21),25-trien 3$\alpha$,9$\alpha$-diolyl)-3'-(pimara-11,15-dien-3$\alpha$-olyl) glycerol (1) and stigmast-5-en-3$\alpha$,26-diol (2) along with known fatty acids n-hexacosanoic acid (3) and hexadecanoic acid (4), have been isolated from the methanol extract of rice hulls of Oryza sativa. The structures of the compounds were elucidated using 1D and 2D NMR spectral methods, viz; $^1H, ^{13}C, ^{13}C$-DEPT, $^1H-^1H$ COSY, $^1H-^{13}C$ HETCOR, HSQC and HMBC aided by IR, EIMS, FABMS and HRFABMS. Compound (1) showed inhibition to radish germination, growth of shoot and root length.