• Proceedings of the Korean Society of Applied Pharmacology
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• 2007.11a
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• pp.19-27
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• 2007

An important potential of metabolomics-based approach is the possibility to develop fingerprints of diseases or cellular responses to classes of compounds with known common biological effect. Such fingerprints have the potential to allow classification of disease states or compounds, to provide mechanistic information on cellular perturbations and pathways and to identify biomarkers specific for disease severity and drug efficacy. Metabolic profiles of biological fluids contain a vast array of endogenous metabolites. Changes in those profiles resulting from perturbations of the system can be observed using analytical techniques, such as NMR and MS. $^1H$ NMR was used to generate a molecular fingerprint of serum or urinary sample, and then pattern recognition technique was applied to identity molecular signatures associated with the specific diseases or drug efficiency. Several metabolites that differentiate disease samples from the control were thoroughly characterized by NMR spectroscopy. We investigated the metabolic changes in human normal and clinical samples using $^1H$ NMR. Spectral data were applied to targeted profiling and spectral binning method, and then multivariate statistical data analysis (MVDA) was used to examine in detail the modulation of small molecule candidate biomarkers. We show that targeted profiling produces robust models, generates accurate metabolite concentration data, and provides data that can be used to help understand metabolic differences between healthy and disease population. Such metabolic signatures could provide diagnostic markers for a disease state or biomarkers for drug response phenotypes.

• Bulletin of the Korean Chemical Society
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• v.9 no.3
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• pp.176-179
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• 1988

3-Methoxy-4-cyano-2,9-dioxabicyclo[4.3.0]non-3-e ne (1) was prepared by (4 + 2) cycloaddition reaction of methyl ${\alpha}$-cyanoacrylate with 2,3-dihydrofuran. Compound 1 was ring-open polymerized by cationic catalyst such as boron trifluoride etherate to obtain alternating head-to-head (H-H) copolymer (2) of methyl $\alpha$ -cyanoacrylate and 2,3-dihydrofuran. For comparison, head-to-tail (H-T) copolymer (3) was also prepared by free radical copolymerization of the corresponding monomers. The H-H copolymer exhibited minor differences in its $^1H$-NMR and IR spectra, but in the $^{13}C$-NMR spectra significant differences were observed between the H-H and H-T copolymers. All of the H-H and H-T copolymers were soluble in common solvents and the inherent viscosities were in the range 0.2-0.3 dl/g.

• The Korean Journal of Food And Nutrition
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• v.27 no.3
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• pp.532-537
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• 2014

Cortex Phellodendri (CP) is derived from the dried bark of Phellodendron amurense. It has been widely used as a drug in traditional Korea medicine for treating diarrhea, jaundice, swelling pains in the knees and feet, urinary tract infections, and infections of the body surface. Many analytical methods have been used to study oriental herbal medicines, such as thin-layer chromatography, column liquid chromatography, and high performance liquid chromatography (HPLC). In this study, preparative centrifugal partition chromatography (CPC) was successfully carried out in order to separate pure compounds from a CP methanol extract. The optimum two-phase CPC solvent system was composed of n-butanol: acetic acid: water (4:1:5 v/v/v). The flow rate of the mobile phase was 3 mL/min in ascending mode with rotation at 1,000 rpm. The CPC-separated fraction and purification procedures were carried out by preparatory HPLC. The $^1H$ NMR spectrum revealed that the resonances at ${\delta}$ 4.10 and 4.20 ppm corresponded to three protons ($-OCH_3$), whereas those at ${\delta}$ 6.10 ppm corresponded to two protons ($-OCH_2O-$). Further, two aromatic protons (H-11 and H-12) conveys a doublet-doublet pattern. The H-11 doublet and H-12 doublet appear at ${\delta}$ 7.98 and 8.11, respectively. The $^{13}C$ NMR. spectrum showed a tetrasubstituted with a methylenedioxy group at C2 and C3, and two methoxy groups at C9 and C10. The chemical structure of the berberine was identified by $^1H$, $^{13}C$-nuclear magnetic resonance and electrospray ionization-mass spectroscopy spectral data analysis.

• Microbiology and Biotechnology Letters
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• v.33 no.2
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• pp.123-129
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• 2005

Isolation and identification of pathogens from slaughter and meat processing plant were investigated. Antimicrobial activity of Amaranthus lividus against isolated pathogens such as Aeromonas sobria, Escherichia coli, Escherichia coli O157, Listeria monocytogenes, Salmonella spp., and Staphylococcus aureus was investigated. Among the chloroform, ethyl acetate and buthanol fraction of amaranthus lividus showed inhibitory effect against Aeromonas sobria CLFM1 and Escherichia coli CLFM2. Antimicrobial substance in chloroform fraction was isolated by silica gel adsorption column chromatography, sephadex LH-20 column chromatography and silica gel partition column chromatography. The antimicrobial compound of amaranthus lividus was identified as diethyl phtalate by HPLC, GC-MS, H-NMR and C-NMR.

• Journal of the Korean Wood Science and Technology
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• v.41 no.6
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• pp.566-575
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• 2013

The fruits of Taxus cuspidata were collected, divided into seeds and fruits, and extracted with 95% EtOH. The extracts were evaporated under the reduced vacuum pressure, concentrated, then successively fractionated with a series of n-hexane, dichloromethane, ethyl acetate and water on a separatory funnel to get some freeze dried samples. A portion of the EtOAc (arils:1.65 g, seeds:1.04 g) and $H_2O$ (arils:7 g, seeds:10 g) soluble samples were chromatographed on a Sephadex column using MeOH-$H_2O$ (1:1, 1:3, 1:5, v/v), EtOH-hexane (3:1, v/v) mixture and 100% $H_2O$ as eluting solvents to isolate pure compounds from the fractions. The isolates were developed by cellulose TLC using t-BuOH-HOAc-$H_2O$ (TBA; 3:1:1, v/v/v) and 6% aqueous HOAc. Visualization was done under ultraviolet light and by spraying the vanillin-HCl-EtOH reagent (4.8:12:480, v/v/v). followed by heating. The structures of the isolates were characterized by $^1H$- and $^{13}C$-NMR, DEPT, 2D-NMR, LC/MS and EI-MS spectra. In addition to the NMR and MS spectra, acid hydrolysis and permethylation were used to determine the correct structure of the isolated sugar compound. Their structures were elucidated as (+)-catechin (1), (-)-epicatechin (2), (+)-gallocatechin (3), (-)-epigallocatechin (4) and ${\beta}$-D-fructofuranose-($2{\rightarrow}4$)-O-${\beta}$-D-glucopyranose($1{\rightarrow}4$)-O-${\alpha}$-D-glucopyranose ($1{\rightarrow}2$)-O-${\beta}$-D-fructofuranose (5) on the basis of the above experimental evidences.

• Journal of the Korean Chemical Society
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• v.24 no.1
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• pp.44-52
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• 1980

Ionic dissociation rates of $\alpha$-chlorobenzyl ethyl ether in each solvent of toluene-$d_8$ and carbon tetrachloride were measured by the method of dynamic NMR spectroscopy. The spin system of these 1H NMR spectra was $AB_3$. The theoretical spectrum was calculated by computer simulation of dynamic NMR spectra, which agreed very well with observed spectra. From this computer simulation, the ionic dissociation rate constant k was obtained, and by Eyring plot with it, slope and intercept length was gained, from which kinetic parameters were calculated.The easiness of ionic dissociation depended upon solvent polarity. Activation enthalpy was 4.7 kcal/mole in toluene-$d_8$, 10.7 kcal/mole in carbon tetrachloride, and activation entropy was -35. 8 e.u. in toluene-$d_8$, -14.4 e.u. in carbon tetrachloride. It was understood that though the ${\Delta}H^{neq}$ value was small, this ionic dissociation had an easier procession in nonpolar solvents with increasing temperatures. Considering that the ionic dissociation could be thought as the first step of $S_N1$ mechanism, attention might be paid to the results that the value of ${\Delta}S^{neq}$ had a large negative value in comparison with a small ${\Delta}H^{neq}$.

• Bulletin of the Korean Chemical Society
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• v.32 no.9
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• pp.3382-3388
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• 2011

Reaction of barbituric acid (BA), 1,3-dimethyl barbituric acid (DMBA) and 2-thiobarbituric acid (TBA) with cyanogen bromide and aldehydes in the presence of L-(+)-tartaric acid afforded a new route for the synthesis of stable heterocyclic 5-aryl-1H,1'H-spiro[furo[2,3-d]pyrimidine-6,5'-pyrimidine]2,2',4,4',6'(3H,3'H,5H)-pentaones which is a dimeric form of barbiturate (uracil and thiouracil derivative). In the reaction of 1,3-diethyl thiobarbituric acid (DETBA) the Knoevenagel condensation and then Michael adducts were obtained under the same condition. Structure elucidation is carried out by $^1H$ NMR, $^{13}C$ NMR, FT-IR and Mass analyses. Mechanism of the formation is discussed.

• Journal of the Korean Magnetic Resonance Society
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• v.23 no.4
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• pp.93-97
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• 2019

Black ginger (Kaempferia parviflora) is a short-lived ginger plant with dark purple colored root and is known to be effective in treating diabetes and obesity. To find out the difference in the characteristics of the black ginger according to the variety of production, 1D proton NMR experiments were performed on 4 types of black gingers from different regions. The NMR spectra of all black ginger showed the characteristic peaks of the polymethoxy flavone compounds, and the chemical shifts and intensity of peaks showed slight differences depending of the type of black ginger implying the difference in molecular environment. These initial NMR experiments can be applied to the identification of the diversity of black ginger in physiological function according to the climate of regions using SNIF-NMR (Site-specific Natural Isotope Fractionation studied by NMR).

• 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.46 no.2
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• pp.69-73
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• 2003

A novel antifungal antibiotic for azole-resistant Candida albicans was purified from the culture broth of Bacillus subtilis LAM 97-44 by butanol extraction, Diaion HP-20 and Dowex-50 adsorption chromatography, silica gel flash chromatography followed by HPLC and designated LAM-44A. LAM-44A was stable for 60 min at $100^{\circ}C$, and pH range from 2 to 10. MIC values were observed at $0.5-3.5\;{\mu}g/ml$ against various Candida albicans strains. The antibiotic showed no cytotoxicity for S180, MKN-45, P388, HeLa and 373 at the concentration of 1 mg/ml. LAM-f4A was colorless powder soluble in water, methanol, ethanol, butanol and negative to ninhydrin reaction. The antibiotic had maximum absorption at 273 nm in methanol, and melting point was $202^{\circ}C$. The molecular weight and formula were determined to be 282 and $C_{14}H_{34}O_5$ by $^1H-NMR,\;^{13}C-NMR$, IR spectrum and elemental analysis.