• Journal of the Korean Chemical Society
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• v.40 no.1
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• pp.28-36
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• 1996

The pentanuclear complexes have been obtained by the reactions of molybdenum(VI) and tungsten(VI) polynuclear complexes with molybdenum(O) and tungsten(O) dinitrosyl mononuclear complexes, and methylthioamidoxime. The prepared complexes (n-Bu4N)2[Mo4O12Mo(NO)2{CH3SCH2C(NH2)NHO}2{CH3SCH2C(NH)NO}2](1), (n-Bu4N)2[W4O12Mo(NO)2{CH3SCH2C(NH2)NHO}2{CH3SCH2C(NH)NO}2](2), (n-Bu4N)2[Mo4O12W (NO)2{CH3SCH2C(NH2)NHO}2{CH3SCH2C(NH)NO}2] (3) have been characterized by elemental analysis, infrared, UV-visible and 1H NMR spectra. The complexes are elucidated the cis-{M(NO)2}2+(M = Mo, W) unit and a slight delocalization by spectroscopy. The structure of (n-Bu4N)2[W4O12Mo(NO) 2{CH3SCH2C(NH2)NHO}2{CH3SCH2C(NH)NO}2] was determined by X-ray single crystal diffraction. Crystal data are follows: Monoclinic, $P21}a$, a = 22.14(2) $\AA$, b = 14.93(1) $\AA$, c = 23.20(1) $\AA$, $\beta$ = 111.08(6) $\AA$, V = 7155(9) $\AA$, Z = 4, final R = 0.072 for 6191(I > $3\sigma(I)).$ The structure of complex forms two dinuclear [W2O5{CH3SCH2C(NH2)NHO}{CH3SCH2C(NH)NO}] and a central {Mo(NO)2} 2+ core. The geometric structure of the {Mo(NO)2} 2+unit is the formally cistype and C2v symmetry.

• Journal of Ginseng Research
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• v.43 no.2
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• pp.186-195
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• 2019

Background: Notoginseng stem-leaf (NGL) ginsenosides have not been well used. To improve their utilization, the biotransformation of NGL ginsenosides was studied using ginsenosidase type-I from Aspergillus niger g.848. Methods: NGL ginsenosides were reacted with a crude enzyme in the RAT-5D bioreactor, and the dynamic changes of multi-ginsenosides of NGL were recognized by HPLC. The reaction products were separated using a silica gel column and identified by HPLC and NMR. Results: All the NGL ginsenosides are protopanaxadiol-type ginsenosides; the main ginsenoside contents are 27.1% Rb3, 15.7% C-Mx1, 13.8% Rc, 11.1% Fc, 7.10% Fa, 6.44% C-Mc, 5.08% Rb2, and 4.31% Rb1. In the reaction of NGL ginsenosides with crude enzyme, the main reaction of Rb3 and C-Mx1 occurred through Rb3${\rightarrow}$C-Mx1${\rightarrow}$C-Mx; when reacted for 1 h, Rb3 decreased from 27.1% to 9.82 %, C-Mx1 increased from 15.5% to 32.3%, C-Mx was produced to 6.46%, finally into C-Mx and a small amount of C-K. When reacted for 1.5 h, all the Rb1, Rd, and Gyp17 were completely reacted, and the reaction intermediate F2 was produced to 8.25%, finally into C-K. The main reaction of Rc (13.8%) occurred through Rc${\rightarrow}$C-Mc1${\rightarrow}$C-Mc${\rightarrow}$C-K. The enzyme barely hydrolyzed the terminal xyloside on 3-O- or 20-O-sugar-moiety of the substrate; therefore, 9.43 g C-Mx, 6.85 g C-K, 4.50 g R7, and 4.71 g Fc (hardly separating from the substrate) were obtained from 50 g NGL ginsenosides by the crude enzyme reaction. Conclusion: Four monomer ginsenosides were successfully produced and separated from NGL ginsenosides by the enzyme reaction.

• Analytical Science and Technology
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• v.29 no.1
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• pp.1-9
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• 2016

It is believed that traditional Korean medicines can be managed more scientifically through the development of logical criteria to verify their region of cultivation, and that this could contribute to the advancement of the traditional herbal medicine industry. This study attempted to determine such criteria for Sansuyu. The volatile compounds were obtained from 20 samples of domestic Corni fructus (Sansuyu) and 45 samples of Chinese Sansuyu by steam distillation. The metabolites were identified in the NIST Mass Spectral Library via the obtained gas chromatography/mass spectrometer (GC/MS) data of 53 training samples. Data binning at 0.2 min intervals was performed to normalize the number of variables used in the statistical analysis. Multivariate statistical analyses, such as principle component analysis (PCA), partial least squares-discriminant analysis (PLS-DA), and orthogonal partial least squares-discriminant analysis (OPLS-DA) were performed using the SIMCA-P software package. Significant variables with a variable importance in the projection (VIP) score higher than 1.0 were obtained from OPLS-DA, and variables that resulted in a p-value of less than 0.05 through one-way ANOVA were selected to verify the marker compounds. Finally, among the 11 variables extracted, 1-ethylbutyl-hydroperoxide (9.089 min), nonadecane (20.170 min), butylated hydroxytoluene (25.319 min), 5β,7βH,10α-eudesm-11-en-1α-ol (25.921 min), 7,9-bis(2-methyl-2-propanyl)-1-oxaspiro[4.5]deca-6,9-diene-2,8-dione (34.257 min), and 2-decyldodecyl-benzene (54.717 min) were selected as markers to indicate the origin of Sansuyu. The statistical model developed was suitable for the determination of the geographical origin of Sansuyu. The cultivation areas of four Korean and eight Chinese Sansuyu samples were predicted via the established OPLS-DA model, and it was confirmed that 11 of the 12 samples were accurately classified.

• Journal of Applied Biological Chemistry
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• v.65 no.3
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• pp.215-219
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• 2022

The flowers of Cosmos bipinnatus were extracted with solvent made with methanol:water (4:1) and the concentrates were partitioned into ethyl acetate (EtOAc), n-butanol (n-BuOH), and water (H₂O) fractions. The octadecyl silica gel (ODS) and silica gel (SiO₂) column chromatographies were repeated for the EtOAc fraction to isolated of two phenolic compounds. The chemical structure of the isolated compounds were identified as benzyl O-β-ᴅ-glucopyranoside (1), and 2-phenylethyl O-β-ᴅ-glucopyranoside (2) through spectroscopic datas such as nuclear magnetic resornance, infrarad spectroscopy, and mass spectroscopy. These two compounds were first isolated from C. bipinnatus flowers through this study. To evaluate the anti-atopic activity of the two isolated compounds using a HaCaT cell line induced by ultraviolet light, several experiments were conducted and neither both compounds showed toxicity in the concentration range of 1 to 1,000 ㎍/mL. In the results of anti-atopic activity through Thymus and activation regualted chemokine (TARC) assay, both compounds showed dose-dependent TARC inhibitory activity. In particular, compound 1 showed significant activity even in a low concentration range of 10 ㎍/mL, and in different concentration ranges. Also compound 1 showed higher inhibitory activity than other compound, confirming that the anti-atopic activity was the most excellent. Based on these results, it is considered that it can be used as a functional cosmetic material.

• Korean Journal of Food Science and Technology
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• v.45 no.2
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• pp.174-179
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• 2013

Three low-molecular compounds were isolated from methanol extracts of pear (Pyrus pyrifolia N. cv. Chuhwangbae) fruit peels using solvent fractionation, various types of column chromatogrphy (Diaion HP-20, Sephadex LH-20, and silica gel), and high performance liquid chromatography with an assay guided by 1,1-diphenyl-2-picrylhydrazyl radical-scavenging activity. The isolated compounds were identified as 2-carboxyl-4(1H)-quinolinone (kynurenic acid, 1) from butanol fraction, cis-p-coumaric acid (2) from ethyl acetate-acidic fraction, and vanillin (3) from the ethyl acetate-phenolic fraction, respectively. These isolated compounds were confirmed on the basis of the spectroscopic data of electrospray ionization mass spectrometry and nuclear magnetic resonance. This is the first time that compounds 1-3 were isolated and identified in pear.

• Polymer(Korea)
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• v.25 no.4
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• pp.486-495
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• 2001

Degradable poly(butylene succinate) (PBS)/poly(TEX>${\varepsilon}$-caprolactone) (PCL) copolyesters were prepared by using transesterification between poly(butylene succinate) and poly(TEX>${\varepsilon}$-caprolactone). The thermal and mechanical properties of copolyesters were investigated using differential scanning calorimetry and tensile testing. Interchange reaction between PBS and PCL molecules could be identified from proton NMR spectra. The reduced viscosity of the PBS/PCL copolyesters increased with reaction time except for a series of PBS/PCL (50/50 wt%) copolyesters. For all the compositions, the melting point and crystallization temperature of high-$T_m$ component (PBS) decreased as reaction time increased. From the results of tensile testing, it was found that stress and strain at break of the PBS/PCL copolymers containing less than 40 wt% PCL improved as compared to those of pure PBS, but at 50 wt% PCL stress at break of PBS/PCL copolymers was lowered due to decrease of crystallinity. On the other hand, Young's moduli of all the copolyesters decreased with both reaction time and PCL content.

• Korean Journal of Medicinal Crop Science
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• v.21 no.5
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• pp.361-371
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• 2013

This study was performed to determine the antimelanogenic effect and tyrosinase inhibitory activities of anthocyanin rich fraction (AN-SLP) from Liriope platyphylla Wang et Tang seeds. Anthocyanins isolated from L. platyphylla seeds revealed the presence of four major anthocyanin components, which were tentatively identified as delphinidin-3-Oglucoside, delphinidin-3-O-rutinoside, petunidin-3-O-rutinoside, and malvidin-3-O-rutinoside using semipreparative HPLC, $^1H$-NMR, $^{13}C$ NMR, FAB-MS and LC/ES-MS. The inhibitory effect of AN-SLP on tyrosinase activity was studied using in vitro (against mushroom tyrosinase) and ex vivo (against B16 melanoma cell tyrosinase) models. Cellular tyrosinase activity was decreased by AN-SLP treatment in B 16 melanoma cells through dose dependent manner, but AN-SLP did not inhibit mushroom tyrosinase and L-DOPA oxidation directly. AN-SLP showed melanin inhibition by 53.2% at 50 ${\mu}g/m{\ell}$ which was 0.7 times more efficient than the antimelanogenic effect of commercial arbutin and kojic acid (36.5%) also did not show cell toxicity. Additionally, AN-SLP inhibited the activity of ${\alpha}$-glucosidase and the glycosylation of tyrosinase in melanoma cell. The resulting unsaturated glycosylation of tyrosinase makes it unstable and disturb correct transportation. From theses results, we conclude that AN-SLP could be used as anti-melanogenic agent for skin whitening.

• Korean Journal of Food Science and Technology
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• v.33 no.6
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• pp.753-759
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• 2001

To evaluate antiinflammation of Aloe vera peel, antiimflammation substances were extracted from Aloe vera peel and identified, and we investigated the effect of the its substance the inhibitory effect on the activity of hyaluoronidase, elastase, collagenase and prostaglandin endoperoxide synthase. The water extract from Aloe vera peel were successfully purified with solvent fractionation, silica gel column chromatography, preparative thin layer chromatography and UV spectrometer. Two purified active substances were identified as aloe-emodin and barbaloin by Mass Spectrometer, $^1H-NMR$ and FT-IR. Aloe-emodin and barbaloin. $IC_{50}$ values of aloe-emodin and barbaloin against hyaluronidase activity were 40 and $70\;{\mu}g/mL$, respectively. Leuckocyte elastase, which is related to the destruction of various tissue, $IC_{50}$ values of them were 50 and $60\;{\mu}g/mL$, respectively. $IC_{50}$ values of aloe-emodin and barbaloin against collagenase activity were 40 and $60\;{\mu}g/mL$, respectively. and $IC_{50}$ values of aloe-emodin and barbaloin aganist the prostaglandin endoperoxide synthase, which play an important role in inflammatory reactions, were 40 and $70\;{\mu}g/mL$, respectively. Inhibitory effects of aloe-emodin, barbaloin and aspirin against carrageenan paw edema were 74.9, 52.9 and 51.9% as inhibiton percentage, respectively, at dose of 100 mg/kg and that of indomethancin was 49.7 at dose of 10 mg/kg. Cell cytotoxicity of barbaloin against human gingival cells was lower than that of aloe-emodin. Aloe-emodin and barbaloin did not show cytotoxicity against human gingival cells at concentration of 1.0 and $5.0\;{\mu}g/mL$, However, aloe-emodin and barbaloin showed less cytotoxicity than chlorhexidine, which usually have been used as the agent of anticaries and antiinflammation. These results suggested that aloe-emodin and barbaloin from Aloe vera peel have the effect of anticaries and antiinflammation.

• Journal of the Korean Applied Science and Technology
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• v.8 no.1
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• pp.35-43
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• 1991

Dried seeds of Camellia japonica and Thea sinensis were investigated to determine the nature of their antioxidative activity. Activity was measured by the induction period in the coupled oxidation of a substrate lard and extracts or isolates to be tested. 70% methanol and dichloromethane extracts were found to be antioxidative abilities. Their unsaponifiables revealed weak antioxidative activity, although hexane extracts did not show antioxidative effect on lard. Column chromatography for dlchloromethane extracts gave 4 fractions(only 2 fractions were potent). HPLC was used in isolating potent antioxidative components from the column fractions and the precolumn-passed methanol extracts. They were separated into 7 and 8 components, respectively. The column fractions obtained from both seeds comprised trans-p-coumaric acid. trans-p-ferulic acid and an unknown component with minor components such as chlorogenic acid and catechin. On the other hand, the most prominent components in the methanol extracts were an unidentified component. trans-pcoumaric acid, trans-p-ferulic acid, catechin and chlorogenic acid. The unknown compound isolated from the column fractions and methanol extracts was identified as epicatechin by $^1H-and\;^{13}C-NMR$. The antioxidative activities of these components were epicatechin > catechin > chlorogenic acid > trans-p-ferulic acid > trans-p-coumaric acid.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.14 no.5
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• pp.2550-2558
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• 2013

Poly(o-hydroxyamides)(PHAs) copolymers having oligo(oxy ethylene) pendant in the main chain were synthesized by solution polycondensation reaction at low temperature. Copolymer precursors were studied by fourier transform infrared(FT-IR), differential scanning calorimeter(DSC), thermogravimetric analyzer(TGA), universal testing machine(UTM) and limited oxygen index(LOI). The inherent viscosities of the PHAs measured at $35^{\circ}C$ in DMAc or DMAc/LiCl solution were in the range of 0.74~1.42 dL/g. Solubility of the precursors with higher oligo(oxy ethylene) unit was increased, but the PBOs were nearly insoluble in a variety of solvents. The degradation temperature of the copolymer precursors was recorded in the ranges of $408{\sim}664^{\circ}C$ in nitrogen and char yields showed 13~59% values at $900^{\circ}C$. The mechanical properties and flame retardancy of copolymer precursors decreased with higher oligo(oxy ethylene) unit.