• Bulletin of the Korean Chemical Society
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• v.30 no.5
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• pp.1039-1042
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• 2009

RNA polymerase II C-terminal domain phosphatase 1 containing ubiquitin like domain (UBLCP1) has been identified as a regulatory molecule of RNA polymerase II. UBLCP1 consists of ubiquitin like domain (UBL) and phosphatase domain homologous with UDP and CTD phosphatase. UBLCP1 was cloned into the E.coli expression vectors, pET32a and pGEX 4T-1 with TEV protease cleavage site and purified using both affinity and gel-filtration chromatography. Domains of UBLCP1 protein were successfully purified as 7 mg/500 mL (UBLCP1, 36.78 KDa), 32 mg/500 mL (UBL, 9 KDa) and 8 mg/500 mL (phosphatase domain, 25 KDa) yielded in LB medium, respectively. Isotope-labeled samples including triple-labeled ($^2H/^{15}N/^{13}C$) UBLCP1 were also prepared for hetero-nuclear NMR experiments. $^{15}N-^{1}H$ 2D-HSQC spectra of UBLCP1 suggest that both UBL and phosphatase domain are properly folded and structurally independent each other. These data will promise us further structural investigation of UBLCP1 by NMR spectroscopy and/or X-ray crystallography.

• Biomolecules & Therapeutics
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• v.17 no.2
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• pp.133-137
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• 2009

The root of Astragalus membranaceus is a traditional folk medicine that has been used for many therapeutic purposes in Asia. It reportedly acts as an immunostimulant, tonic, hepatoprotective, diuretic, antidiabetic, analgesic, expectorant, sedative, and anticancer drug. In this study, metabolomic profiling was applied to the roots of A. membranaceus of different ages using NMR coupled with two multivariate statistical analysis methods: such as principal components analysis (PCA) and canonical discriminant analysis (CDA). This allowed various metabolites to be assigned in NMR spectra, including $\gamma$-aminobutyric acid (GABA), aspartic acid, succinic acid, glutamic acid, glutamine, N-acetyl aspartic acid, acetic acid, arginine, alanine, threonine, lactic acid, and valine. The score plot from PCA and also CDA allowed a clear separation between samples according to age.

• Journal of the Korean Magnetic Resonance Society
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• v.14 no.2
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• pp.127-133
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• 2010

Redox-dependent conformational change of human 8-kDa Dynein light chain (LC8) plays important role in regulating NF-${\kappa}B$ signaling pathway. In this study we characterized the structural states of the oxidized and reduced forms of LC8 by using NMR spectroscopy. The $^1H-^{15}N$ 2D HSQC spectra of oxidized LC8 indicated that no significant change in tertiary structure of LC8 occurred upon oxidation. The chemical shift perturbations of LC8 upon oxidation suggest a redox-dependent quaternary structural change.

• Korean Journal of Medicinal Crop Science
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• v.12 no.3
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• pp.203-208
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• 2004

Salidroside was isolated and purified from R. sachalinensis A. Bor. roots. Purified salidroside was obtained from repeated silicagel column chromatography and preparative HPLC, and identified by $^1H-NMR,\;^{13}C-NMR\;and\;^1H-^1H$ COSY spectra analyzer. Callus induction and cell suspension from R. sachalinensis leaf segments were established on 1/2MS solid medium and in $2B_5$ liquid medium containing 0.5 mg/l NAA and 1 mg/l, BA in the dark condition, respectively. The contents of salidroside for suspension culture were ranging from 0.12% to 0.41% in comparison with 0.17% for natural roots.

• Applied Biological Chemistry
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• v.48 no.3
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• pp.267-272
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• 2005

trans-Cinnamaldehyde, a major component of Cinnamomum cassia, was quantitatively analyzed using the $^1H-NMR$ spectrometry. Applicability of this method was confirmed through observing the variation of chemical shift in the $^1H-NMR$ spectrum of t-cinnamaldehyde and the integration value according to various sample concentrations or running temperatures. When the $^1H-NMR$ spectrometry was run for t-cinnamaldehyde (7.1429 mg/ml) at 19, 25, 30, 40 and $50^{\circ}C$, the chemical shifts of the doublet methine signal due to an aldehyde group were observed at 9.7202, 9.7184, 9.7169, 9.7142 and 9.7124 ppm, respectively, to imply that the running temperature had no significant variation in the chemical shift of the signal. The integration values of the signal were $1.37\;(19^{\circ}C),\;1.37\;(25^{\circ}C),\;1.37\;(30^{\circ}C),\;1.37(40^{\circ}C)$ and $1.37(50^{\circ}C)$, respectively, to also indicate running temperature gave no effect on the integration value. When the sample solutions with various concentrations such as 0.4464, 0.8929, 1.7857, 3.5714, 7.1429 and 14.286 mg/ml were respectively measured for the $^1H-NMR$ at $25^{\circ}C$, the chemical shifts of the aldehyde group were observed at 9.7206, 9.7201, 9.7196, 9.7192, 9.7185 and 9.7174 ppm. Even though the signal was slightly shifted to the high field in proportion to the increase of sample concentration, the alteration was not significant enough to applicate this method. The calibration curve for integration values of the doublet methine signal due to the aldehyde group vs the sample concentration was linear and showed very high regression rate ($r^2=1.0000$). Meantime, the $^1H-NMR$ spectra (7.1429 mg/ml $CDCl_3,\;25^{\circ}C$) of t-cinnamaldehyde and t-2-methoxycinnamaldehyde, another constituent of Cinnamomum cassia, showed the chemical shifts of the aldehyde group as ${\delta}_H$ 9.7174 (9.7078, 9.7270) for the former compound and ${\delta}_H$ 9.6936 (9.6839, 9.7032) for the latter one. The difference of the chemical shift between two compounds was big enough to be distinguished using the NMR spectrometer with 0.45 Hz of resolution. The contents of cinnamaldehyde in Cinnamomum cassia, which were respectively extracted with n-hexane, $CHCl_3$, and EtOAc, were determiend as 94.2 \;mg/g (0.94%), 137.6 mg/g (1.38%) and 140.1 mg/g(1.40%) t-cinnamaldehyde in each extract, respectively, by using the above method.

• Journal of Plant Biotechnology
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• v.33 no.4
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• pp.283-288
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• 2006

Discrimination of 5 rice cultivars (Sangjubyeo , Dongjinbyeo Simbaekbyeo , Hwamanbyeo , and Simbaek-hetero ) using metabolic profiling was carried out. Whole cell extracts from each cultivar were subjected to $^1H$ NMR spectroscopy. When spectral data were analyzed by principal component analysis, 5 cultivars were clustered into 3 groups: SJ, DJ + SB, and HM + SH. Thecultivars showed great difference in carbohydrate region of $^1H$ NMR spectra, suggesting that qualitative and quantitative differences in carbohydrate compounds play a major role in discrimination of the cultivars. In addition, it was readily possible to determine relative quantification of major carbohydrates including sucrose, glucose, maltose from spectral data of the cultivars. SJ showed 2 to 4 times higher content of maltose than the other rice cultivars. Overall results indicate that metabolic discrimination of rice cultivars using $^1H$ NMR spectroscopy combined by multivariate statistical analysis can be used for rapid discrimination of numerous rice cultivars and simple quantitative analysis system of major carbohydrate compounds in rice grains.

• Journal of the Korean Chemical Society
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• v.68 no.2
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• pp.74-81
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• 2024

A sulfonic acid-water-silanol system in SO₃H-functionalized MCM-41 was investigated using solid-state nuclear magnetic resonance techniques. The proton exchange rate between a water molecule and a silanol group in the S-PE-MCM-41 was determined by analyzing the 1D proton spectra, the proton EXSY spectrum, and ²H spin-lattice relaxation data under various hydration levels. Two kinds of water-bounding sites were found in the S-PE-MCM-41: weakly and strongly bound sites. Over several hours, water molecules bound to the weakly bound sites at the low hydration level migrated to the strongly bound sites. At high temperature, the S-PE-MCM-41 easily lost water molecules weakly bound to the silanol, while the strongly bound water molecules survived. Water molecules that participated in the hydration of the phenethyl sulfonate were involved in the hydrogenbonded silanol mechanism of proton conductivity. This phenomenon contributes higher proton conductivity to the S-PE-MCM-41 by the cooperation of sulfonyl and silanol groups in the proton transfer process, even at higher temperature.

• Bulletin of the Korean Chemical Society
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• v.20 no.6
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• pp.683-688
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• 1999

In deuterium NMR spectra of phosphatidylethanolamine bilayers with an extremely high content of saturated fatty acids, each C1 deuteron of the glycerol backbone gave rise to a doublet. This suggests the presence of two backbone conformations, the exchange between which is slow on an NMR time scale. The origin of the two conformations has been investigated in this work using saturated 1,2-diacyl-sn-glycero-3-phosphoethanolamine specifically deuterated in the glycerol backbone. The results showed that the two conformations originate from different domains, which have different fatty acid compositions. The differential scanning calorimetry of the bilayers suggested that the size of the domain is not large enough to show an independent phase transition. Thus, the formation of microdomains in the phosphatidylethanolamine bilayers has been concluded. Conformational difference in different domains was shown to be restricted to the C1 position of the glycerol backbone. The microdomains of phosphatidylethanolamine were retained even in the presence of other phospholipids.

• Bulletin of the Korean Chemical Society
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• v.34 no.10
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• pp.2959-2962
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• 2013

As the concentration of aqueous $CD_3OH$ solutions was decreased, the OD peaks in $^2H$ NMR spectra grew relative to the $CD_3$ peaks. Isotope impurity for OH groups of $CD_3OH$ and deuterium naturally present in water contributed to the OD peaks. Using these peak area data, the site-specific isotope populations of isotope enriched chemicals were measured. In addition, the method using both $^1H$ and $^2H$ NMR spectroscopy was demonstrated with neat $CD_3OH$ to measure the site-specific isotope populations. The results indicate that although it represents only ~0.015% of hydrogen isotopes, the deuterium naturally present in solvents cannot be ignored, especially when the concentration of deuterium-enriched solutes is varied. Proton/deuteron exchange between methyl and methyl/hydroxyl groups was confirmed to be negligible, while that among hydroxyl groups was detectable.

• Bulletin of the Korean Chemical Society
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• v.25 no.12
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• pp.1757-1763
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• 2004

A new series of nickel(II), cobalt(II)/(III) and copper(II) complexes of 14, 15 and 16-membered of macrocyclic ligands have been prepared and characterized by elemental analyses, IR, UV-VIS and $^1H-NMR$ spectra, magnetic susceptibilities, conductivities, DTA and ESR measurements. Molar conductances in DMF solution indicate that, the complexes are nonelectrolytes except (9-12) complexes. The electronic spectra show that, all complexes are square planar or distorted octahedral geometry. The ESR spectra of solid complexes (4), (8) and (11) show square planar of axial type symmetry $(d_{x2-y2})$ with considerable covalent bond character. However, complex (12) shows a spectrum of octahedral geometry with $d_{z2}$ ground state. Complex (12) shows exploitation in reducing the amount of electron adducts formed in DNA during irradiation with low radiation products.