• Bulletin of the Korean Chemical Society
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• v.34 no.6
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• pp.1684-1688
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• 2013

A rapid and sensitive method for determining usnic acid of Lethariella cladonioides in rat was established using high performance liquid chromatography (HPLC) quadrupole time-of-flight (QTOF) tandem mass (MS/MS). Rat plasma was pretreated by mixture of acetonitrile and chloroform to precipitate plasma proteins. Chromatographic separation was achieved on a column ($50{\times}2.1$ mm, $5{\mu}m$) with a mobile phase consisting of water (containing $5{\times}10^{-3}$ M ammonium formate, pH was adjusted to 3.0 with formic acid) and acetonitrile (20:80, v/v) at a flow rate of 0.3 mL/min. A tandem mass spectrometric detection with an electrospray ionization (ESI) interface was conducted via collision induced dissociation (CID) under negative ionization mode. The MS/MS transitions monitored were m/z 343.0448 ${\rightarrow}$ m/z 313.2017 for usnic acid and m/z 153.1024 ${\rightarrow}$ m/z 136.2136 for protocatechuic acid (internal standard). The linear range was calculated to be 2.0-160.0 ng/mL with a detection limit of 3.0 pg/mL. The inter- and intra-day accuracy and precision were within ${\pm}7.0%$. Pharmacokinetic study showed that the apartment of usnic acid in vivo confirmed to be a two compartment open model. The method was fully valid and will probably be an alternative for pharmacokinetic study of usnic acid.

• Journal of Microbiology and Biotechnology
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• v.16 no.7
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• pp.1111-1119
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• 2006

Beauvericins and enniatins are cyclohexadepsipeptides exhibiting various biological activities on animal systems, including humans. Fusarium oxysporum FB1501 (KFCC 11363P) that produces four different cyclohexadepsipeptides was isolated from soil in Korea and the structures of the four cyclohexadepsipeptides elucidated by HPLC, MS, IR, and NMR analyses. The molecular weights for compounds 1,2,3, and 4 were determined to be 654.5, 784.5, 668.6, and 682.5, respectively, on the basis of ESI-MS measurements. The IR spectra for all the compounds exhibited absorptions for ester $(1,733-1,743\;cm^{-1})$ and amide $(1,649-1,655\;cm^{-1})$ bonds that were very similar to those for beauvericin and enniatins with ester and amide absorptions. The results of the NMR analysis $(^{1}H,\;^{13}C,\;135-DEPT,\;COSY,\;HMQC,\;and\;HMBC;\;in\;COCl_{3})$ revealed that compounds 1,3, and 4 consisted of $_{L}-N-methyl\;valine$ (N-MeVal), $_{D}-{\alpha}-hydroxyisovaleic\;acid$ (Hiv), and 2-hydroxy-3-methylpentanoic acid (Hmp) residues (compound 1: three N-MeVal residues, two Hiv residues, and one Hmp residue; compound 3: three N-MeVal residues, one Hiv, and two Hmp residues; compound 4: three N-MeVal residues and three Hmp residues). Therefore, the compounds were identified as enniatin H (compound 1), enniatin I (compound 3), and enniatin MK1688 (compound 4). Compound 2 was analyzed as beauvericin according to 1D and 2D NMR analyses. This study is the first report related to the co-production of beauvericin with other unusual enniatins, such as enniatin H, enniatin I, and enniatin MK1688, by Fusarium oxysporum.

• Journal of Microbiology and Biotechnology
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• v.27 no.11
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• pp.1961-1970
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• 2017

Lespedeza cuneata G. Don is a traditional herb that has been associated with multiple biological activities. In this study, we investigated the antioxidative/antiaging activities and performed an active component analysis of the non-fermented and fermented (using Lactobacillus pentosus) extracts of Lespedeza cuneata G. Don. The antioxidative activities of the fermented extract were higher than those of non-fermented extracts. The elastase inhibitory activity, inhibitory effects on UV-induced MMP-1 expression, and ability to promote type I procollagen synthesis were investigated in Hs68 human fibroblasts cells. These tests also revealed that the fermented extract had increased antiaging activities compared with the non-fermented extract. A component analysis of the ethyl acetate fractions of non-fermented and fermented extracts was performed using TLC, HPLC, and LC/ESI-MS/MS to observe changes in the components before and after fermentation. Six components that were different before and after fermentation were investigated. It was thought that kaempferol and quercetin were converted from kaempferol glucosides and quercetin glucosides, respectively, via bioconversion with the fermentation strain. These results indicate that the fermented extract of L. cuneata G. Don has potential for use as a natural cosmetic material with antioxidative and antiaging effects.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.37 no.4
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• pp.309-318
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• 2011

In this study, the antioxidative effect, antibacterial, inhibitory effects on tyrosinase, inhibitory effects on elastase and component analysis of Phellinus linteus (P. linteus) extracts were investigated. The ethyl acetate fraction of P. linteus extracts ($2.94\;{\mu}g/mL$) showed the highest free radical (1,1-diphenyl-2-picrylhydrazyl, DPPH) scavenging activity ($FSC_{50}$). Reactive oxygen species (ROS) scavenging activity ($OSC_{50}$) of P. linteus extracts on ROS generated in $Fe^{3+}$-EDTA/$H_2O_2$ system was investigated using the luminol-dependent chemiluminescence assay. The ethyl acetate fraction ($0.0072\;{\mu}g/mL$) showed the most prominent ROS scavenging activity. The protective effects of extract/fractions of P. linteus extracts on the rose-bengal sensitized photohemolysis of human erythrocytes were investigated. The P. linteus extracts showed cellular membrane protective effects in a concentration dependent manner ($5{\sim}50\;{\mu}g/mL$). The inhibitory effect ($IC_{50}$) on tyrosinase of P. linteus extract was the highest at 50 % ethanol extract ($6.34\;{\mu}g/mL$), and the inhibitory effect ($IC_{50}$) on elastase of P. linteus was the highest at ethyl acetate fraction ($14.08\;{\mu}g/mL$). TLC, HPLC chromatogram and LC/ESI-MS of the ethyl acetate fraction obtained from P. linteus extracts were identified interfungin A (PL RPT-1a). These results indicate that extract/fractions of P. linteus can function as antioxidants in biological systems, particularly skin exposed to UV radiation by scavenging ROS, and protect cellular membranes against ROS. Extract/fractions of P. linteus can be applicable to new cosmeceuticals for antioxidant, antiaging, antiwrinkle and whitening.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.40 no.4
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• pp.391-402
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• 2014

In this study, the antioxidative effects and component analysis for the extracts of Rumex acetosa L. were investigated. All experiments were performed with 50% ethanol extract, ethyl acetate fraction and aglycone fraction obtained from dried R. acetosa L.. Free radical scavenging activities (1,1-diphenyl-2- picrylhydrazyl) size of, in the order of aglycone fraction > ethyl acetate fraction > 50% ethanol extract, aglycone fraction ($45.10{\mu}g/mL$) showed the highest radical scavenging activity. Reactive oxygen species (ROS) scavenging activity (total antioxidant capacity, $OSC_{50}$) on ROS generated in $Fe^{3+}-EDTA/H_2O_2$ system was also, in the order of ethyl acetate fraction> aglycone fraction> 50% ethyl acetate fraction, ethyl acetate fraction ($2.68{\mu}g/mL$) was shown a great antioxidant capacity. The total antioxidant capacity of the ethyl acetate fraction was found to be greater than L-ascorbic acid, known as a typical hydrophilic antioxidant ($6.88 {\mu}g/mL$). The cellular protective effects of R. acetosa L. extracts on the $^1O_2$-induced cellular damage of human erythrocytes were exhibited at all concentration-dependent ($1{\sim}25{\mu}g/mL$). Especially, aglycone fraction (${\tau}_{50}$, 104.80 min) in $25{\mu}g/mL$ showed the most protective effect among extracts. Components of the ethyl acetate fraction obtained from R. acetosa L. extracts were analyzed by TLC, HPLC chromatogram, LC/ESI-MS/MS. As a result, the ethyl acetate fraction contained several flavonoids, such as orientin, isoorientin, vitexin, isovitexin. These results indicate that the R. acetosa L. extracts can be used as antioxidants in biological systems, particularly skins exposed to UV radiation by quenching and/or scavenging $^1O_2$ and other ROS. Thus, the extracts of R. acetosa L. could be applicable to new anti-aging cosmeceutical ingredients.

• Applied Chemistry for Engineering
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• v.28 no.6
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• pp.696-704
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• 2017

In this study, we investigated antioxidative and matrix metalloproteinases (MMPs) inhibitory effects of Sorbus commixta twig extracts and fermented extracts with Lactobacillus pentosus and analyzed active ingredients. The free radical scavenging activity ($FSC_{50}$) of non-fermented and fermented extracts of S. commixta twig' were 41.04 and $58.2{\mu}g/mL$, respectively. In the $Fe^{3+}-EDTA/H_2O_2$ system, the active oxygen scavenging activity ($OSC_{50}$) was 2.6 and $3.0{\mu}g/mL$, respectively. In the dermal fibroblasts, the intracellular reactive oxygen species (ROS) scavenging activity was 35.3% for non-fermented extract and 40.2% for fermented extracts at the concentration of $10{\mu}g/mL$. Also at the same concentration, the expression of MMPs (MMP-1, -2, -3) by western blot was 68.3, 35.0 and 24.2%, respectively for non-fermented extracts and 84.3, 70.5 and 69.2% for fermented extracts. TLC, HPLC, and LC/ESI-MS/MS were used for measuring the changes in the components of the extract before and after fermentation. As a result, caffeic acid, (-)-epicatechin, isoquercitrin, and quercetin were identified. From the results, S. commixta twig fermented extracts by L. pentosus showed greater ROS scavenging activity and inhibitory effects on MMPs expression than those of using non-fermented extracts. Therefore, it is suggested that S. commixta twig fermented extracts can be used as an anti-aging cosmetic material.

• Korean Journal of Pharmacognosy
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• v.44 no.4
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• pp.320-325
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• 2013

"SaCheolNaMu" has been used as a Korean folk medicine for the jaundice, lumbago and uterine diseases. Although a crude drug related to this folk medicine is sold in traditional herbal market, the botanical origin of this drug has not been pharmacognostically confirmed yet. In this study, the morphological and anatomical characteristics of the stem of Euonymus species growing in Korea, i.e. Euonymus japonica and E. fortunei var. radicans were studied to clarify the botanical origin of "SaCheolNaMu". As a result, it was found that these two species could be discriminated by the morphological criteria such as the thickness of cuticles, the number of collenchyma cell layers, and the frequency of druse and resinous substance. According to these criteria, it was elucidated that the commercial folk medicine "SaCheolNaMu" was the stem of E. japonica. Meanwhile, HPLC-DAD analysis on the 70% ethanolic extracts of two species showed significantly different HPLC profiles each other. The molecular ions of three characteristic peaks shown in the chromatogram of two species were identified by ESI-MS, and their structures were estimated to be flavonol glycosides.

• The Korean Journal of Food And Nutrition
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• v.26 no.3
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• pp.547-552
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• 2013

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. In this study, preparative centrifugal partition chromatography (CPC) was successfully carried out to separate antibacterial 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 $m{\ell}/min$ in ascending mode with rotation at 1,000 rpm. The CPC-separated fraction and purification procedures were carried out by preparatory HPLC. Palmatine weas identified by $^1H$, $^{13}C$-nuclear magnetic resonance and electrospray ionization-mass spectroscopy spectral data analysis.

• Journal of Ginseng Research
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• v.44 no.5
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• pp.673-679
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• 2020

Background: Panax notoginseng saponin (PNS) is the extraction from the roots and rhizomes of Panax notoginseng (Burk.) F. H. Chen. PNS is the main bioactive component of Xuesaitong, Xueshuantong, and other Chinese patent medicines, which are all bestselling prescriptions in China to treat cardiocerebrovascular diseases. Notoginsenoside R₁ and ginsenoside Rg₁, Rd, Re, and Rb₁ are the principal effective constituents of PNS, but a systematic research on the rare saponin compositions has not been conducted. Objective: The objective of this study was to conduct a systematic chemical study on PNS and establish the HPLC fingerprint of PNS to provide scientific evidence in quality control. In addition, the cytotoxicity of the new compounds was tested. Methods: Pure saponins from PNS were isolated by means of many chromatographic methods, and their structures were determined by extensive analyses of NMR and HR-ESI-MS studies. The fingerprint was established by HPLC-UV method. The cytotoxicity of the compounds was tested by 3-(4,5-dimethylthiazol-2-yl)-2,5 -diphenyltetrazolium bromide assay. Results and Conclusion: Three new triterpenoid saponins (1-3) together with 25 known rare saponins (4-28) were isolated from PNS, except for the five main compounds (notoginsenoside R1 and ginsenoside Rg1, Rd, Re, and Rb1). In addition, the HPLC fingerprint of PNS was established, and the peaks of the isolated compounds were marked. The study of chemical constituents and fingerprint was useful for the quality control of PNS. The study on antitumor activities showed that new Compound 2 exhibited significant inhibitory activity against the tested cell lines.

• Journal of Microbiology
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• v.45 no.6
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• pp.499-504
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• 2007

A new antagonistic strain of actinomycete, designated AP19-2, was isolated from the feces of giant pandas inhabiting the Foping National Nature Reserve in China. Cultural characteristic studies strongly suggested that this strain is a member of the genus Streptomyces. The nucleotide sequence of the 16S rRNA gene of strain AP19-2 evidenced profound similarity (97-99 %) with other Streptomyces strains. Two pure active molecules were isolated from a fermentation broth of Streptomyces sp. strain AP19-2 via extraction, concentration, silica gel G column chromatography, and HPLC. The chemical structures of the two related compounds (referred to as chromomycin $A_2$ and chromomycin $A_3$) were established on the basis of their Infrared spectra (IR), High Resolution Electrospray Ionization Mass Spectrometry (HR-ESI-MS), and Nuclear Magnetic Resonance (NMR) data, and by comparison with published data.