• Journal of the Korean Magnetic Resonance Society
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• v.24 no.4
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• pp.96-103
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• 2020

A new NMR method to monitor solvent-localized NMR signals in the two-phase liquid system is suggested. This method based on intermolecular single-quantum coherence (iSQC). Here, we exploited the feature of the local action of distant dipolar field (DDF) effect in order to filter out specific NMR signals dissolved in different solvents. This solvent specific iSQC spectroscopy was carried out on a model two-phase liquid system (D-glucose in water/palmitic acid in chloroform), and showed solvent-localized NMR signals. We believe our approaches might be useful in metabolic analysis such as two-phase liquid extraction scheme for labile chemical species.

• Food Science and Biotechnology
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• v.17 no.1
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• pp.102-105
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• 2008

The freezing patterns of commercial frozen foods were characterized by using proton nuclear magnetic resonance ($^1H$ NMR) relaxometry and differential scanning calorimetry (DSC). The liquid-like components like unfrozen water were investigated as a function of temperature (10 to $-40^{\circ}C$) and then compared with the unfrozen water content measured by DSC. The formation of ice crystals and the reduction of water in the foods during freezing were readily observed as a loss of the NMR signal intensity. The proton NMR relaxation measurement showed that the decreasing pattern of the liquid-like components varied depending on the samples even though they exhibited the same onset temperature of ice formation at around $0^{\circ}C$. When compared with the unfrozen water content obtained by the DSC, the NMR and DSC results could be closely correlated at the temperature above $-20^{\circ}C$. However, the distinct divergence in the values between 2 methods was observed with further decreasing temperatures probably due to the solid glass formation which was not detected by DSC.

• Applied Chemistry for Engineering
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• v.4 no.4
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• pp.770-775
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• 1993

Chemical structure of poly(ethylene terephthalate-co-1, 4-cyclohexylene dimethylene terephthalate), P(ET-CT) copolyesters was investigated by High Resolution NMR analysis. The copolymer composition and isomeric ratio were determined by methylene resonance peaks which were separated into three peaks corresponding to ET, trans CT and cis CT units, respectively. The copolymer sequence distribution was evaluated from the carbon resonance peaks connected to carbonyl groups in benzene, indicating died distribution. According to statistics model, these copolyesters are almost random copolymers. The copolymer sequence distribution could be simulated and its averaged length was calculated by random copolymer statistics.

• Bulletin of the Korean Chemical Society
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• v.25 no.2
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• pp.198-202
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• 2004

Hydrogen bond is an important factor in the structures of carbohydrates. Because of great strength, short range, and strong angular dependence, hydrogen bonding is an important factor stabilizing the structure of carbohydrate. In this study, conformational properties and the hydrogen bonds in GlcNAc( ${\beta}$1,3)Gal(${\beta}$)OMe in DMSO are investigated through NMR spectroscopy and molecular dynamics simulation. Lowest energy structure in the adiabatic energy map was utilized as an initial structure for the molecular dynamics simulations in DMSO. NOEs, temperature coefficients, SIMPLE NMR data, and molecular dynamics simulations proved that there is a strong intramolecular hydrogen bond between O7' and HO3' in GlcNAc( ${\beta}$1,3)Gal(${\beta}$)OMe in DMSO. In aqueous solution, water molecule makes intermolecular hydrogen bonds with the disaccharides and there was no intramolecular hydrogen bonds in water. Since DMSO molecule is too big to be inserted deep into GlcNAc(${\beta}$1,3)Gal(${\beta}$)OMe, DMSO can not make strong intermolecular hydrogen bonding with carbohydrate and increases the ability of O7' in GlcNAc(${\beta}$1,3)Gal(${\beta}$)OMe to participate in intramolecular hydrogen bonding. Molecular dynamics simulation in conjunction with NMR experiments proves to be efficient way to investigate the intramolecular hydrogen bonding existed in carbohydrate.

• Analytical Science and Technology
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• v.17 no.5
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• pp.388-392
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• 2004

Structural studies of membrane proteins, importantly involving interpretation of genomics information, many signaling pathway and major drug target for drug discovery, are having difficulty in characterizing the function using conventional solution nmr spectroscopy and x-ray crystallography because phospholipid bilayers hindered fast tumbling and crystallization. Here, we studied the structure of the pf1 coat protein in oriented phospholipid bilayers by home-built solid-state NMR probe. Bacteriophage pf1 was purified from Paeudomonas Aeruginosa and coat protein of bacteriophage pf1 was isolated from DNA and other proteins.

• Journal of the Korean Magnetic Resonance Society
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• v.10 no.1
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• pp.74-88
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• 2006

Since the first commercial NMR spectrometer came out in 1953 from Varian, much of the hardware development has been improved and matured through commercial equipments. Many of magnetic resonance laboratories however still build and use home-built spectrometers, which are satisfactory even with the consideration of educational purpose only. The home-built NMR spectrometer could be further advantageous and could be often an only option for investigating new ideas with demanding experimental conditions or new hardware support. A solid state NMR spectrometer was designed with extra interest in stochastic experiment and built for an 8.93 T superconducting magnet from Oxford instrument. Super-heterodyned system was implemented for the transmitter and receiver parts. Intermediate frequency (IF) for the heterodyne system was chosen to 70 MHz for the first and the second channels, with additional 120 MHz for the third channel for maximum NMR frequency capability. We will show overall schematics, and discuss the designs with detailed diagrams, then demonstrate the applicability of home-built spectrometer with stochastic-excitation in solid state NMR and in applications to quadrupolar nuclear Spins.

• Journal of the Korean Magnetic Resonance Society
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• v.15 no.1
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• pp.54-68
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• 2011

$^1H$ nuclear magnetic resonance (NMR) spectroscopy of biological samples has been proven to be an effective and nondestructive approach to probe drug toxicity within an organism. In this study, ketoprofen toxicity was investigated using $^1H$-NMR spectroscopy coupled with multivariate statistical analysis. Histopathologic test of ketoprofen-induced acute gastrointestinal damage in rats demonstrated a significant dose-dependent effect. Furthermore, principal component analysis (PCA) derived from $^1H$-NMR spectra of urinary samples showed clear separation between the vehicle-treated control and ketoprofen-treated groups. Moreover, PCA derived from endogenous metabolite concentrations through targeted profiling revealed a dose-dependent metabolic shift between the vehicle-treated control, low-dose ketoprofen-treated (10 mg/kg body weight), and high-dose ketoprofen-treated (50 mg/kg) groups coinciding with their gastric damage scores after ketoprofen administration. The resultant metabolic profiles demonstrated that the ketoprofen-induced gastric damage exhibited energy metabolism perturbations that increased urinary levels of citrate, cis-aconitate, succinate, and phosphocreatine. In addition, ketoprofen administration induced an enhancement of xenobiotic activity in fatty oxidation, which caused increase levels of N-isovalerylglycine, adipate, phenylacetylglycine, dimethylamine, betaine, hippurate, 3-indoxylsulfate, N,N-dimethylglycine, trimethyl-N-oxide, and glycine. These findings demonstrate that $^1H$-NMR-based urinary metabolic profiling can be used for noninvasive and rapid way to diagnose adverse drug effects and is suitable for explaining the possible biological pathways perturbed by nonsteroidal anti-inflammatory drug toxicity.

• Analytical Science and Technology
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• v.7 no.2
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• pp.187-191
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• 1994

A reactive intermediate 1,2-dihydropyridine derivative 2 has been prepared and isolated from the reaction of pyridine with $^tBuLi$ and trimethylchlorosilane in nonpolar condition at low temperature 2 has characterized by $^1H-NMR$ fine structure analysis with SPINX3. The mechanistic information of formation of 2 was obtained from synthesized 2,5-disubstituted pyridine derivatives 3 and 4.

• Journal of the Korean Magnetic Resonance Society
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• v.14 no.1
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• pp.38-44
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• 2010

In liquids NMR, $^{1}H$ is the most widely observed nucleus, which is not the case in solids NMR. The reason is due to the strong homo-dipolar interactions between the hydrogen atoms which mask the useful chemical shift information. Therefore we must remove the strong homo-dipolar interactions in order to get structural information, which can be investigated by the isotropic chemical shift. There are two ways of obtaining it. One is the ultra-fast MAS of ca. 70 kHz spinning speed, which has become available only recently. The other way is devising a pulse sequence which can remove the strong homo-dipolar interaction. In the latter way, MAS with a moderate spinning rate of a few kHz, is enough to remove the chemical shift anisotropy. In this report, 1D-CRAMPS and 2D MASFSLG techniques are utilized and their results will be compared. This kind of highresolution $^{1}H$ NMR for solids, should become a valuable analytical tool in the understanding and the developing of a new class of hydrogen storage materials. Here ammonium borane $-NH_{3}BH_{3}$, whose hydrogen content is high, is used as a sample.

• Proceedings of the Polymer Society of Korea Conference
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• 2006.10a
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• pp.339-339
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• 2006

In this study, the microvoids in glassy polymers were investigated by Xe sorption and $^{129}Xe$ NMR measurements. Xe sorption isotherms of glassy polymers have been successfully interpreted by the dual-mode sorption model. $^{129}Xe$ NMR chemical shift of the $^{129}Xe$ in the samples show nonlinear low-field shift with increasing sorption amount of Xe because of a fast exchange of Xe atoms between Henry and Langmuir sites, whereas it has showed linear shift against sorption amount of Xe into the Langmuir site. From this Xe-density dependence of the $^{129}Xe$ NMR chemical shift, it has been able to estimate mean size of the microvoids in glassy polymer. It is confirmed that there is correlation between ${C_H}'$ and volume or number of microvoids. From these findings, it is demonstrated that $^{129}Xe$ NMR spectroscopy is a powerful technique to determine the mean size and number of microvoids in glassy polymers.