• YAKHAK HOEJI
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• v.57 no.4
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• pp.272-281
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• 2013

In this study, we developed and validated the HPLC method using the isolated components from Erycibae caulis. Their structures were elucidated by spectroscopic methods including UV, $^1H$-NMR, $^{13}C$-NMR, FAB-Mass and ESI-Mass as Compound 1 (crypto-chlorogenic acid), Compound 2 (scopolin), Compound 3 (neochlorogenic acid) and Compound 4 (3,4-di-O-caffeoylquinic acid). Major three compounds and scopoletin were decided as representative components of Erycibae caulis. We established HPLC analytical method by using the representative components and 20 commercial samples which were collected considering to various cultivated area. The HPLC fingerprinting was successfully achieved with an AKZO NOBEL Kromasil 100-5C18 column. The mobile phase consisted of 0.5% acetic acid in water (A) and methanol (B) using gradient method of 85(A) to 50(A) for 35min. The fingerprints of chromatograms were recorded at an optimized wavelength of 330 nm. This developed analytical method was validated with specificity, selectivity, accuracy and precision. And it is suggested that scopolin, scopoletin, neochlorogenic acid, 3,4-di-O-caffeoylquinic acid were more than 0.162%, 0.133%, 0.057%, 0.044%, respectively. In addition, principal component analysis (PCA) was performed on the analytical data of 20 different Erycibae caulis samples in order to classify samples collected from different regions. We hope that this assay can be readily utilized as quality control method for Erycibae caulis.

• Journal of Digital Convergence
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• v.13 no.5
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• pp.337-344
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• 2015

Medicinal plants containing wellness-fusion-complex compound are increasingly being pursued as suitable alternative sources of various biological properties. In this study, inhibitory effect of Quintinia acutifolia, which is a New Zealand plant, on P388 murine lymphocytic leukemia cells using MTT [3-(4,5-dimethylthiazol-2-yl)- 2,5-diphenyl-tetrazolium bromide] assay. Based on $^1H-NMR$, $^{13}C-NMR$ spectral data and other spectral analysis, 2,3,2'',3''-tetrahydroochanaflavone (1) and 2'',3''-dihydroochana-flavone (3) inhibited the leukemia cells were purified from the plants. 2,3,2'',3''-tetrahydroochanaflavone (1) and 2'',3''-dihydroochana-flavone (3) are biflavonoids possessing two basic flavonoids and actively inhibited growth of P388 murine lymphocytic leukemia cells with a 50% inhibitory concentration ($IC_{50}$) of $8.2{\mu}g/mL$ and $3.1{\mu}g/mL$, respectively. Specially, 2'',3''-dihydroochana-flavone (3) possessed unconjugated flavonone system, which isn't consist of a pair with B ring of 2,3,2'',3''-tetrahydroochanaflavone (1). Therefore, the two compounds could be considered as a candidate for development of anticancer drugs and need to much studies in the future.

• Bulletin of the Korean Chemical Society
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• v.14 no.2
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• pp.266-271
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• 1993

The reaction of $(CO_5$)M=C(OMe)Tol (M=Cr, Mo, W and $Tol=p-C_6H_4Me)$ and $BBr_3$ followed by treatment with tetramethylethylenediamine (TMEDA) yields a mixture of two diastereomers, trans, $cis-Br(CO)_2(tmeda)M{\equiv}$CTol [M=Cr(1a), Mo(2a), W(3a)] and cis, $trans-Br(CO)_2(tmeda)M{\equiv}$CTol [M=Cr(1b), Mo(2b), W(3b)], respectively. These compounds have been isolated as crystalline solids and characterized by spectroscopic (infrared, mass, $^1H$ and $^{13}C-NMR)$ data. The trans, cis-Br(CO)2(tmeda)Cr${\equiv}$CTol (1a), has been examine via a single crystal X-ray diffraction study : $BrCrO_2N_2C_{16}H_{23}$, Mr=407.27, triclinic, $P{\bar{1}},\;a=12.792(2),\;b=13.400(5),\;c= 11.645(4)\;{\AA},\;{\alpha}=101.26(2)^{\circ},\;{\beta}=103.04(2)^{\circ},\;{\gamma}=91.88(2)^{\circ},\;{\nu}=1907(1){\AA}^3,\;Z=2,\;{\rho}(calcd)=1.418\;gcm^{-3},\;{\lambda}(MoK{\alpha})=0.71069\;{\AA},\;{\mu}=26.25 cm^{-1},\;F(000)=831.97,\;T=295K,\;R=0.0977$ for 1332 significant reflections $[F_0>5{\sigma}(F_0)]$. There are two essentially equivalent molecules in the crystallographic asymmetric unit. Each molecule is octahedral with the bromide ligand trans to the alkylidyne carbon, the two cis-carbonyl ligands, and the bidentate TMEDA ligand.

• Journal of the Korean Chemical Society
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• v.55 no.4
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• pp.612-619
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• 2011

Lanthanide(III) complexes of 1,2-diphenyl-4-butyl-3,5-pyrazolidinedione(phenylbutazone, PB) have been synthesized and characterized by elemental analyses, molar conductance measurements, IR, UV-Vis. and NMR spectra. The spectral data reveal that the PB acts as a bidentate and mono-ionic ligand coordinating through both the carbonyl oxygens of the pyrazolidinedione ring. The molar conductance data suggest that the complexes are non-electrolytes. The thermal behaviour of the complexes was studied by TG and DTG in air atmosphere and the results provide information about dehydration, thermal stability and thermal decomposition. The final products are found to be the corresponding metal oxides. The thermodynamic parameters and kinetic parameters were evaluated for the dehydration and decomposition stages. The negative entropy values of the decomposition stages indicate that the activated complexes have a more ordered structure than the reactants and that the reactions are slower than normal. Based on these studies, the complexes have been formulated as $[Ln(PB)_3]{\cdot}5H_2O$(Ln=La and Ce) and $[Ln(PB)_3(H_2O)_2]{\cdot}2H_2O$(Ln=Pr, Nd and Sm).

• Natural Product Sciences
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• v.21 no.1
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• pp.49-53
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• 2015

Eight isoflavonoid compounds were isolated from the EtOAc fraction of Maackia amurensis which had shown the highest anti-Helicobacter pylori activity among the fractions, using medium pressure liquid chromatography and recrystallization. Based on the spectroscopic data including $^1H$-NMR, $^{13}C$-NMR, HMBC and MS data, the chemical structures of the isolates were determined to be (-)-medicarpin (1), afromosin (2), formononetin (3), tectorigenin (4), prunetin (5), wistin (6), tectoridin (7) and ononin (8). Anti-H. pylori activity of each compound was evaluated with broth dilution assay. As a result, (-)-medicarpin (1), tectorigenin (4) and wistin (6) showed anti-H. pylori activity. (-)-Medicarpin (1) exhibited the most potent growth inhibitory activity against H. pylori with the minimal inhibitory concentration $(MIC)_{90}$ of $25{\mu}M$, and tectorigenin (4) with $MIC_{90}$ of $100{\mu}M$ ranked the second. This is the first study to show the anti-H. pylori activity of M. amurensis, and it is suggested that the stem bark of M. amurensis or the EtOAc fraction or the isolated compounds can be a new natural source for the treatment of H. pylori infection.

• Journal of Microbiology and Biotechnology
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• v.13 no.5
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• pp.778-782
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• 2003

In the course of screening anti-influenza agents from natural products, four neuraminidase inhibitors were isolated from the methanol extract of mushroom Microphorus affinis by purification using solvent partition, silica gel column chromatography, Sephadex LH-20, and semi-preparative HPLC. The chemical structures of these compounds were identified as ${\alpha}-lupeol$, methyl linoleate, methyl palmitate, and methyl oleate by means of spectral data including GC-MS, $^1H-,\;and\;^{13}C-NMR\;with\;IC_{50}$ values of 5.65, 7.07, 7.12, and $7.52\;\mu\textrm{M}$, respectively. They did not inhibit other glycosidases such as glucosidase, mannosidase, and galactosidase, indicating that they were relatively specific inhibitors of neuraminidase. The relationship between the fatty acid structure and inhibitory activity was investigated. The result showed that, in the case of an aliphatic linear hydrocarbon skeleton, at least one carboxyl (presumably any carbonyl) moiety and sixteen carbons were the necessary requirements for potent inhibition, whereas saturated, unsaturated, free, and ester forms did not have any significant effect on the activity.

• Korean Journal of Pharmacognosy
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• v.51 no.2
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• pp.139-145
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• 2020

The leaves of Diospyros kaki Thunb. were used to treat heart disease and hypotension in traditionally East Asia. The purpose of this study is to simultaneously quantitiative analyze the content of flavonoids in leaves of D. kaki. The isolated flavonoids from the leaves of D. kaki, and the structure of the isolated flavonoids were analyzed based on ¹H and ¹³C NMR spectrum compared to literature data. Simultaneous quantitative analysis of the isolated flavonoids was validated using high performance liquid chromatography (HPLC). Results showed that the calibration curves of the flavonoid compounds were confirmed that they have a large linearity with a correlation coefficient (R²) of 0.99. In the intra-day and inter-day analysis, accuracy and precision of five compounds were measured that accuracy was 94.39 to 114.47% and precision was less than 3.00%. Content analysis showed hyperoside (1.30 ± 0.09%), astragalin (0.81 ± 0.06%), trifoline (1.58 ± 0.07%), quercetin (0.13 ± 0.02%) and kaempferol (1.33 ± 0.25%).

• Proceedings of the Materials Research Society of Korea Conference
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• 2009.11a
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• pp.36.2-36.2
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• 2009

Low dielectric materials have been great attention in the semiconductor industry to develop high performance interlayer dielectrics with low k for Cu interconnect technology. In our study, the dielectric properties of SiOC /SiO2 thin film derived from polyphenylcarbosilane were investigated as a potential interlayer dielectrics for Cu interconnect technology. Polyphenylcarbosilane was synthesized from thermal rearrangement of polymethylphenylsilane around $350^{\circ}C{\sim}430^{\circ}C$. Characterization of synthesized polyphenylcarbosilane was performed with 29Si, 13C, 1H NMR, FT-IR, TG, XRD, GPC and GC analysis. From FT-IR data, the band at 1035 cm-1 is very strong and assigned to CH2 bending vibration in Si-CH2-Si group, indicating the formation of the polyphenylcarbosilane. Number average of molecular weight (Mn) of the polyphenylcarbosilane synthesized at $400^{\circ}C$ for 6hwas 2, 500 and is easily soluble in organic solvent. SiOC/SiO2 thin film was fabricated on ton-type silicon wafer by spin coating using 30wt % polyphenylcarbosilane incyclohexane. Curing of the film was performed in the air up to $400^{\circ}C$ for 2h. The thickness of the film is ranged from $1{\mu}m$ to $1.7{\mu}m$. The dielectric constant was determined from the capacitance data obtained from metal/polyphenylcarbosilane/conductive Si MIM capacitors and show a dielectric constant as low as 2.5 without added porosity. The SiOC /SiO2 thin film derived from polyphenylcarbosilane shows promising application as an interlayer dielectrics for Cu interconnect technology.

• Journal of Soil and Groundwater Environment
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• v.9 no.4
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• pp.42-51
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• 2004

Peat humin(p-Humin), humic acid(p-HA) and fulvic acid(p-FA) were isolated from Canadian Sphagnum peat moss by dissolution in 0.1M NaOH followed by acid precipitation. After purification cycles, they are characterized for their elemental compositions and, acid/base properties. Functionalities and carbon structures of the humic fractions were also characterized using FT-IR and solid state $^{13}C$-NMR spectroscopy. Those results are compared with one another and with soil humic substances from literatures. Main purpose of this study was to present a chemical and spectroscopic characterization data of humic substance from peat moss needed to evaluate its environmental applicability. The relative proportions of the p-Humin, p-HA and p-FA in the peat moss was $76\%,\;18\%,\;and\;3\%$, respectively, based on the total organic matter content ($957{\pm}32\;g/kg$). Elemental composition of p-Humin were found to be $C_{1.00}H_{1.52}O_{0.79}N_{0.01}$ and had higher H/C and (N+O)/C ratio compared to those of p-HA($C_{1.00}H_{1.09}O_{0.51}N_{0.02}$) and p-FA($C_{1.00}H_{1.08}O_{0.65}N_{0.01}$). Based on the analysis of pH titration data, there are two different types of acidic functional groups in the peat moss and its humic fractions and their proton exchange capacities(PEC, meq/g) were in the order p-FA(4.91) >p-HA(4.09) >p-Humin(2.38). IR spectroscopic results showed that the functionalities of the peat moss humic molecules are similar to those of soil humic substances, and carboxylic acid(-COOH) is main function group providing metal binding sites for Cd(II) sorption. Spectral features obtained from $^{13}C$-NMR indicated that peat moss humic molecules have rather lower degree of humification, and that important structural differences exist between p-Humin and soluble humic fractions(p-HA and p-FA).

• Journal of Life Science
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• v.25 no.11
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• pp.1298-1303
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• 2015

Machilus thunbergii (Lauraceae) is an evergreen tree cultivated in Korea and Japan. M. thunbergii has long been used as a traditional medicine in Korea, China, and Japan to treat various diseases, including edema, abdominal pain, and abdominal distension. In this study, dried stem bark of M. thunbergii extracted in methanol and extract was partitioned into n-hexane, CHCl₃, and BuOH. The CHCl₃-soluble extracts chromatographed on silica gel column using a CHCl₃/acetone and n-hexane/EtOAc mixture to afford Compound 1 and 2. Two dibenzylbutane lignans, macelignan (1) and meso-dihydroguaiaretic acid (2), were isolated from the CHCl₃-soluble extract of M. thunbergii stem bark. The structures of 1 and 2 were determined by ¹H- and ¹³C-NMR spectroscopic data analyses and a comparison with literature data. The tyrosinase inhibitory activity of the isolated compounds was evaluated. Among these compounds, Compound 2 strongly inhibited the monophenolase (IC₅₀=10.2 μM) activity of tyrosinase. A kinetic analysis showed that Compound 2 was a competitive inhibitor. The apparent inhibition constant (K_i) for Compound 2 binding to free enzyme was 4.8 μM. Based on these results, it can be concluded that meso-dihydroguaiaretic acid (2) is a potential candidate for the treatment of melanin biosynthesis-related skin diseases.