• Proceedings of the Korean Society of Applied Pharmacology
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• 1994.04a
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• pp.263-263
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• 1994

Annexin I is a member of the in family of calcium dependent phospholipid banding proteins and is an in vitro phospholipase $A_2$ (PLA$_2$) inhibitor. The mechanism of PLA$_2$ inhibition by annexin I is still ambiguous. The structure of annexin I was studied at the atomic level by using nuclear magnetic resonance (NMR), circular dichrotsm (CD) and fluorescence spectroscopy. Recombinant human annexin I and N-terminally truncated annexin I (1-31 deleted: d-annexin I) were purified and their NMR spectra were compared. The NMR spectra of the two were similar. When $Ca^{2+}$ ion added to annexin I ad d-annexin I, peak broadening occurred, but no significant spectroscopic change was observed. When porcine pancreatic PLA$_2$ was added to deuterium labeled annexin I, an interaction of annexin I with PLA$_2$ was observed as indicated by the disappearance and shift of several peaks in the NMR spectrum. This result supports a protein-protein interaction mechanism for PLA$_2$ inhibition by annexin I.I.

• 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.

• Archives of Pharmacal Research
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• v.13 no.3
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• pp.246-251
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• 1990

Intermolecular interaction between barbiturates and membrane components such as phospholipid and cholesterol were investigated on $^1$H-NMR spectra and infrared spectra. According to previous reports, barbiturates interacted with phospholipid through intermolecular hydrogen bonds. We also investigated thi observation using dipalmitoyl-phosphatidylcholine (DPPC) as phospholipid in deuterochloroform, and characterized quantitatively. Also, the observed drug could interact with cholesterol which is one of the major components of biomembranes through hydrogen bonds. It was the carbonyl groups of barbiturate and the hydroxyl group of cholesterol that formed hydrogen bond complex. In addition to spectroscopic studies, we investigated the direct effect of phenobarbital on lipid multibilayer vesicles, whose compositions were varied, by calorimetric method. Phenobarbital caused a reduction in the temperature of phase transition of vesicles. These studies may provided a basis for interpreting the mode of action of barbiturates.

• Bulletin of the Korean Chemical Society
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• v.20 no.10
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• pp.1205-1208
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• 1999

27Al NMR chemical shielding, quadrupolar coupling, and dipolar coupling interactions for corundum (α-Al2O3) are determined from the single-crystal 27 Al NMR spectra according to the rotation about three orthogonal axis. 27 Al NMR parameters obtained in this work with high accuracy are as follows: δiso = 7.4(4) ppm, QCC = 2.30(4) MHz, h = 0.08(3), and R = 2.0(3) kHz. This work appears to be the first NMR measurement of an aluminum-aluminum dipolar coupling interaction in α-Al2O3 crystals.

• Korean Journal of Agricultural Science
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• v.35 no.1
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• pp.11-17
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• 2008

This study was conducted to isolate polyacetylenes from the Acanthopanax senticosus and to identify the chemical structure of the polyacetylenes by UV, IR, $^1H$-NMR and $^{13}C$-NMR. One of the liposoluble materials was extracted with petroleum ether. Polyacetylene compounds were collected through solvent fractionation at silica gel column chromatograph. The HPLC was used for the semi-preparative separation IR spectra of fraction 5 showed triple bonds at $2256cm^{-1}$ and double bond at $1654cm^{-1}$, respectively, $^1H$-NMR spectra of Fraction 5 showed the double bond at 5.35-5.48 ppm. Triple bond at 64.0. 71.2, 74.2, 80.2 ppm and double bond at 121.89, 133.0 ppm were observed in the $^{13}C$-NMR spectra.

• Applied Chemistry for Engineering
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• v.23 no.6
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• pp.539-545
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• 2012

3-(2-benzotriazolovinyl)thiophene (BVT) was synthesized by the connection of the thiophene with the electron-withdrawing group, benzotriazole, through the vinylene. Its structure was confirmed by FT-IR, $^1H$-NMR, $^{13}C$-NMR and 2D hetero-cosy spectroscopy. Both BVT and 3-octylthiophene (OT) were copolymerized and showed an average molecular weight of 12000 (PDI 2.67) and 15000 (PDI 2.55), respectively. The copolymers were dissolved in the organic solvent such as chloroform, THF, TCE, etc. The mole ratios of BVT and OT in the synthesized copolymers were confirmed as 1 : 1.8 and 1 : 2.8 from $^1H$-NMR spectra. The UV-vis maximum absorption of copolymers appeared at the wavelength of 470 nm and 465 nm and the photoluminescence at ${\lambda}_{max}$ = 662 nm and 641 nm correspond to red-orange light. The band gaps of copolymers at 1.96 eV and 2.02 eV were found to be higher than those of poly(3-octylthiophene). The HOMO energy levels of the copolymers decreased overall in comparison with those of poly(3-octylthiophene), but the overall LUMO energy level increased.

• Journal of the Korean Magnetic Resonance Society
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• v.25 no.4
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• pp.58-63
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• 2021

Apolipoprotein B-100 (apo B-100), the main protein component that makes up LDL (Low density lipoprotein), consists of 4,536 amino acids and serves to combine with the LDL receptor. The oxidized LDL peptides by malondialdehyde (MDA) or acetylation in vivo act as immunoglobulin (Ig) antigens and peptide groups were classified into 7 peptide groups with subsequent 20 amino acids (P1-P302). The biomimetic peptide P143 (IALDD AKINF NEKLS QLQTY) out of C-group peptides carrying the highest value of IgG antigens were selected for structural studies that may provide antigen specificity. Experimental results show that P143 has β-sheet in Ile[1]-Asn[9] and α-helice in Gln[16]-Tyr[20] structure. Homonuclear 2D-NMR (COSY, TOCSY, NOESY) experiments were carried out for NMR signal assignments and structure determination for P143. On the basis of these completely assigned NMR spectra and proton distance information, distance geometry (DG) and molecular dynamic (MD) were carried out to determine the structures of P143. The proposed structure was selected by comparisons between experimental NOE spectra and back-calculated 2D NOE results from determined structure showing acceptable agreement. The total Root-Mean-Square-Deviation (RMSD) value of P143 obtained upon superposition of all atoms were in the set range. The solution state P143 has a mixed structure of pseudo α-helix and β-turn(Phe[10] to Glu[12]). These results are well consistent with calculated structure from experimental data of NOE spectra. Structural studies based on NMR may contribute to the prevent oxidation studies of atherosclerosis and observed conformational characteristics of apo B-100 in LDL using monoclonal antibodies.

• Analytical Science and Technology
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• v.7 no.2
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• pp.213-224
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• 1994

Several isotopomers of cyclooctanone were prepared by selective deuterium substitution. Intrinsic isotope effects on $^{13}C$ NMR chemical shifts of these isotopomers were investigated systematically at low temperature. These istope effects were discussed in relation to the preferred boat-chair conformation of cyclooctanone. Deuterium isotope effects on NMR chemical shifts have been known for a long time. Especially in a conformationally mobile molecule, isotope perturbation could affect NMR signals through a combination of isotope effects on equilibria and intrinsic effects. The distinction between intrinsic and nonintrinsic effects is quite difficult at ambient temperature due to involvement of both equilibrium and intrinsic isotope effects. However if equilibria between possible conformers of cyclooctanone are slowed down enough on the NMR time scale by lowering temperature, it should be possible to measure intrinsic isotope shifts from the separated signals at low temperature. $^{13}C$ NMR has been successfully utilized in the study on molecular conformation in solution when one deals with stable conformers or molecules were rapid interconversion occurs at ambient temperature. The study of dynamic processes in general requires analysis of spectra at several temperature. Anet et al. did $^1H$ NMR study of cyclooctanone at low temperature to freeze out a stable conformation, but were not able initially to deduce which conformation was stable because of the complexity of alkyl region in the $^1H$ NMR spectrum. They also reported the $^1H$ and $^{13}C$ NMR spectra of the $C_9-C_{16}$ cycloalkanones with changing temperature from $-80^{\circ}C$ to $-170^{\circ}C$, but they did not report a variable temperature $^{13}C$ NMR study of cyclooctanone. For the analysis of the intrinsic isotope effect with relation to cylooctanone conformation, $^{13}C$ NMR spectra are obtained in the present work at low temperatures (up to $-150^{\circ}C$) in order to find the chemical shifts at the temperature at which the dynamic process can be "frozen-out" on the NMR time scale and cyclooctanone can be observed as a stable conformation. Both the ring inversion and pseudorotational processes must be "frozen-out" in order to see separate resonances for all eight carbons in cyclooctanone. In contrast to $^1H$ spectra, slowing down just the ring inversion process has no apparent effects on the $^{13}C$ spectra because exchange of environments within the pairs of methylene carbons can still occur by the pseudorotational process. Several isotopomers of cyclooctanone were prepared by selective deuterium substitution (fig. 1) : complete deuterium labeling at C-2 and C-8 positions gave cyclooctanone-2, 2, 8, $8-D_4$ : complete labeling at C-2 and C-7 positions afforded the 2, 2, 7, $7-D_4$ isotopomer : di-deuteration at C-3 gave the 3, $3-D_2$ isotopomer : mono-deuteration provided cyclooctanone-2-D, 4-D and 5-D isotopomers : and partial deuteration on the C-2 and C-8 position, with a chiral and difunctional case catalyst, gave the trans-2, $8-D_2$ isotopomer. These isotopomer were investigated systematically in relation with cyclooctanone conformation and intrinsic isotope effects on $^{13}C$ NMR chemical shifts at low temperature. The determination of the intrinsic effects could help in the analysis of the more complex effects at higher temperature. For quantitative analysis of intrinsic isotope effects, the $^{13}C$ NMR spectrum has been obtained for a mixture of the labeled and unlabeled compounds because the signal separations are very small.

• 한국신재생에너지학회:학술대회논문집
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• 2005.06a
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• pp.615-617
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• 2005

[ $^{13}C$ ] NMR spectra were obtained for pure $CH_4$ hydrate in order to identify hydrate structure and cage occupancy of guest molecule. The NMR technique can provide both qualitative and quantitative hydrate characteristics. The moles of methane captured into pure $CH_4$ hydrate per mole of water were found to be similar to the full occupancy value. The overall results drawn from this study can be usefully applied to storage and transportation of natural gas.

• Journal of the Korean Chemical Society
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• v.50 no.3
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• pp.183-189
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• 2006

A series of substituted styryl 4-methoxy-1-naphthyl ketones [(2E)-1-(4-methoxy-1-naphthyl)-3-phenyl-2-propen-1-ones] were synthesized using facile method of microwave assisted condensation reaction. The yield of chalcones is more than 90%. They are characterized by their physical constants, micro analysis, infrared (KBr, 4000-400 cm？1) and NMR both 1H and 13C spectral data. From infrared spectra, the s-cis and s-trans stretching vibrations of carbonyl group, from NMR spectra the ethylenic proton and carbon chemical shifts (ppm) are assigned. These spectral data are correlated with various Hammett substituent constants. From the results of statistical analysis the effect of substituents on CO, ？ and ？ proton and carbons are explained.