• Applied Biological Chemistry
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• v.38 no.2
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• pp.184-189
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• 1995

(20S)- and (20R)-Ginsenoside $Rh_2$ were prepared from crude ginseng saponin by chemical treatments. The $^1H-$ and $^{13}C-NMR$ signals of these compounds were fully assigned by various NMR techniques such as DEPT, $^1H-^1H$ COSY, HMQC, HMBC and NOESY.

• Bulletin of the Korean Chemical Society
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• v.30 no.1
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• pp.149-152
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• 2009

Hydrotalcites are anionic clays that are quite prevalent in nature and their importance is growing more and more because of their very wide range of potential applications and uses. Understanding the structural and compositional changes that occur on the molecular scale during the thermal decomposition of hydrotalcite compounds is essential for the basic prediction and comprehensive understanding of the behavior and technical application of these materials. In this study, several hydrotalcite compounds calcined at different temperatures for applications in a chlorine resistant textile were prepared and 27-Aluminm solid-state nuclear magnetic resonance (NMR) spectroscopy was used as a tool to study their local structure and behavior. The changes in the Al coordination of the hydrotalcite compounds were investigated with one dimensional (1D) solid-state magic angle spinning (MAS) NMR spectroscopy. The two broad resonances arising from the structurally different Al coordinations of these compounds were clearly resolved by two dimensional (2D) triple quantum magic angle spinning (3QMAS) NMR spectroscopy.

• Food Science of Animal Resources
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• v.39 no.1
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• pp.1-12
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• 2019

The objective of this study was to establish an optimized 1D $^1H$ quantitative nuclear magnetic resonance (qNMR) analytical method for analyzing polar metabolites in meat. Three extraction solutions [0.6 M perchloric acid, 10 mM phosphate buffer, water/methanol (1:1)], three reconstitution buffers [20 mM 3-morpholinopropane-1-sulfonic acid, 2-[4-(2-hydroxyethyl)piperazin-1-yl]ethanesulfonic acid, phosphate buffer], and two pulse programs (zg30, noesypr1d) were evaluated. Extraction with 0.6 M perchloric acid and 20 mM phosphate resulted in a stable baseline and no additional overlap for quantifying polar metabolites in chicken breast. In qNMR analysis, zg30 pulse program (without water-suppression) showed smaller relative standard deviation (RSD) and faster running time than noesypr1d (water-suppression). High-performance liquid chromatography was compared with qNMR analyses to validate accuracy. The zg30 pulse program showed good accuracy and lower RSD. The optimized qNMR method was able to apply for beef and pork samples. Thus, an optimized 1D $^1H$ qNMR method for meat metabolomics was established.

• Journal of the Korean Magnetic Resonance Society
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• v.8 no.2
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• pp.115-126
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• 2004

Four secondary metabolites from an unidentified tunicate were isolated by treatment with trichloroethyl chloroformate(TECF) or acetic anhydride in pyridine. Their structures were determined by an extensive NMR analysis and the configuration of diacetyl derivatives(3a, 4a) was assigned by comparing with NMR data of a similar compound. Three new naturally occurring compounds (1, 3, 4) showed potent brine shrimp lethality and antifungal effect against Candia albicans.

• 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°).

• Applied Biological Chemistry
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• v.43 no.2
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• pp.136-140
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• 2000

Two steroidal saponins were isolated from MeOH extract of the rhizomes of Asparagus oligoclonos. Using the spectroscopic techniques of $^1H,\;^{13}C$ NMR and 2D NMR, they were identified as $3-O-[{\beta}-D-glucopyranosyl-(1{\rightarrow}2)-{\beta}-D-glucopyranosyl]-(25S)-spirostan-3{\beta}-ol$ and $3-O-{{\beta}-D-glucopyranosyl-(1{\rightarrow}2)-[{\beta}-D-xylopyranosyl-(1{\rightarrow}4)]-{\beta}-D-glucopyranosyl}-(25S)-spirostan-3{\beta}-ol$, respectively. They were first isolated from A. oligoclonos. The in vitro antibacterial activities as well as antibacterial spectrums against 20 bacteria strains were investigated with MIC test. Both saponins inhibited the growth of 10 bacteria strains at the concentration of$100\;{\mu}g/ml$.

• Journal of Microbiology and Biotechnology
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• v.18 no.2
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• pp.314-321
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• 2008

Acaricidal effects of materials derived from Diospyros kaki roots against Dermatophagoides farinae and D. pteronyssinus were assessed using impregnated fabric disk bioassay and compared with that of the commercial benzyl benzoate. The observed responses varied according to dosage and mite species. The $LD_{50}$ values of the chloroform extract of Diospyros kaki roots were 1.66 and $0.96{\mu}g/cm^2$ against D. farinae and D. pteronyssinus. The chloroform extract of Diospyros kaki roots was approximately 15.2 more toxic than benzyl benzoate against D. farinae, and 7.6 times more toxic against D. pteronyssinus. Purification of the biologically active constituent from D. kaki roots was done by using 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 spectra, and identified as plumbagin. The acaricidal activity of plumbagin and its derivatives (naphthazarin, dichlon, 2,3-dibromo-1,4-naphthoquinone, and 2-bromo-1,4-naphthoquinone) was examined. On the basis of $LD_{50}$ values, the most toxic compound against D. farinae was naphthazarin $(0.011{\mu}g/cm^2)$ followed by plumbagin $(0.019{\mu}g/cm^2),$ 2-bromo-1,4-naphthoquinone $(0.079{\mu}g/cm^2)$, dichlon $(0.422{\mu}g/cm^2)$, and benzyl benzoate $(9.14{\mu}g/cm^2)$. Additionally, the skin color of the dust mites was changed from colorless-transparent to dark brown-black by the treatment of plumbagin. Similar results have been exhibited in its derivatives (naphthazarin, dichlon, and 2-bromo-1,4-naphthoquinone). In contrast, little or no discoloration was observed for benzyl benzoate. From this point of view, plumbagin and its derivatives can be very useful for the potential control agents, lead compounds, and indicator of house dust mites.

• Journal of the Korean Magnetic Resonance Society
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• v.3 no.1
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• pp.44-51
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• 1999

An enzyme derived conformational changes of cobalamine is thought to be important in the homolytic cleavage of Co-C bond which is the first step of catalytic Cl-cycle of coenzyme B12-dependent enzymes. Modern 2D-NMR and NMR-based distance geometric studies were carried out to determine the 3D structure of corrin ring. Homonuclear and heteronuclear correlation NMR experiments were performed for complete 1H-NMR signal assignments. Distances between numerous proton pairs were deduced based on the NOE cross peak intensities and subsequently used as input into the distance geometry program for the 3D structure determination. The detailed 3D structure from the present NMR-based analysis was compared with the result from X-ray crystallographic study, which revealed greater conformational changes occur in benzimidazole group and sugar ring than in macrocyclic corrin and tetrapyrrole. In addition, the distance geometry used in this study was found to be quite useful for NMR-based structure determination of medium-sized molecules that give poor NOE effects arising from their intermediate tumbling rate ($\omega$$\tau$c 1.0).

• Journal of the Korean Magnetic Resonance Society
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• v.11 no.1
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• pp.1-9
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• 2007

An unequal site exchanging system induced by restricted rotation of 9-methyl group in 1,8-dichloro-9-triptycene has been studied by spin-lattice relaxation and 2D-EXSY experiments. The exchange rate obtained from relaxation studies is very well coincident to the result of line shape analysis, and the difference of the relaxation times ($T_1$) in two different sites has an important role to analyze 2D-EXSY experimental data.

• Bulletin of the Korean Chemical Society
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• v.20 no.10
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• pp.1145-1148
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• 1999

1H NMR spectra of methyl-, ethyl-, propyl-, isopropyl-, butyl-, N-methylethyl-, N-methylpropyl-, and N-methylisopropylamine coordinated to the paramagnetic 11-tungstocobalto(II)silicate anion (SiW11Co) in dimethylsulfoxide-d6 or dimethylformamide-d7 are reported. For these complexes the ligand exchange is slow on the NMR time scale and pure 1H NMR signals have been observed at room temperature. No complex is detected in D2O. From the pseudocontact shifts of the CH2 and CH3 groups in ethylamine the energy of the gauche conformers with respect to the anti conformer is estimated. Two diastereotopic protons in the CH2 group of N-methylethylamine have quite different chemical shifts especially at low temperatures (e.g. 48.5 vs. 19.4 ppm at -10℃). This may be attributed mainly to the different positions of the two protons in the most stable (gauche) conformer.