• Bulletin of the Korean Chemical Society
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• 제34권6호
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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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• 제16권7호
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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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• 제27권11호
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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.

• 대한화장품학회지
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• 제37권4호
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• pp.309-318
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• 2011

본 연구에서는 상황버섯 추출물의 항산화 및 항노화 활성 및 항균 효과, 그리고 성분분석에 관한 연구를 수행하였다. 상황버섯 추출물의 자유 라디칼(1,1-diphenyl-2- picrylhydrazyl, DPPH) 소거활성($FSC_{50}$)은 에틸아세테이트(ethylacetate) 분획($2.94\;{\mu}g/mL$)에서 가장 큰 활성을 나타내었고, 루미놀-의존성 화학발광법을 이용한 $Fe^{3+}$-EDTA/$H_2O_2$계에서 생성된 활성산소종(reactive oxygen species, ROS)에 대한 상황버섯 추출물의 총항산화능은 추출물의 에틸아세테이트 분획($0.0072\;{\mu}g/mL$)에서 가장 큰 활성을 나타내었다. 광증감제인 rose-bengal로 증감된 사람 적혈구의 광용혈에 대한 억제 효과를 측정하였을 때 농도범위($5{\sim}50\;{\mu}g/mL$)에서 50 % 에탄올 추출물과 에틸아세테이트 분획 모두 농도 의존적으로 세포 보호 효과를 나타내었다. 타이로시네이즈의 활성 저해 효과($IC_{50}$)를 측정한 결과 50 % 에탄올 추출물($IC_{50}=6.34\;{\mu}g/mL$)에서 우수한 효과를 나타내었으며, 엘라스테이즈의 활성 저해 효과($IC_{50}$)는 에틸아세테이트분획($IC_{50}=14.08\;{\mu}g/mL$)에서 큰 효과가 나타났다. TLC, HPLC 및 LC/ESI-MS를 이용하여 상황버섯 추출물 ethylacetate 분획의 주성분을 분석하였고 hispidin 유도체인 interfungin A를 확인하였다. 이상의 결과들은 상황버섯 추출물이 ROS에 대항하여 세포막을 보호함으로써 생체계, 특히 태양 자외선에 노출된 피부에서 항산화제로써 작용할 수 있으며, 특히 상황버섯 추출물의 에틸아세테이트 분획을 항산화, 항노화 및 미백 기능성 화장품 소재로써의 응용 가능성을확인하였다.

• 대한화장품학회지
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• 제40권4호
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• pp.391-402
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• 2014

본 연구에서는 수영 전초 추출물에 대하여 항산화 활성 평가와 성분 분석을 실시하였다. 실험에는 수영전초의 50% 에탄올 추출물, 에틸아세테이트 분획, 아글리콘(aglycone) 분획을 사용하였다. 자유라디칼 소거활성(1,1-diphenyl-2-picrylhydrazyl, DPPH, $FSC_{50}$)의 크기는 아글리콘 분획 > 에틸아세테이트 분획 > 50% 에탄올 추출물 순으로, 아글리콘 분획($45.10{\mu}g/mL$)이 가장 큰 라디칼 소거활성을 나타냈다. $Fe^{3+}-EDTA/H_2O_2$계를 이용한 활성산소 소거활성(총항산화능, $OSC_{50}$)도 에틸아세테이트 분획 > 아글리콘 분획 > 50% 에탄올 추출물 순으로 에틸아세테이트 분획($2.68{\mu}g/mL$)에서 가장 큰 항산화능을 나타내었다. 에틸아세테이트 분획의 총항산화능은 수용성 항산화제로 알려진 L-ascorbic acid ($6.88{\mu}g/mL$)보다 큰 것으로 나타났다. 활성산소인 $^1O_2$으로 유도된 사람 세포 손상에 있어서, 수영 전초 추출물은 모두 농도 의존적($1{\sim}25{\mu}g/mL$)으로 세포보호 활성을 나타내었다. 특히 아글리콘 분획(${\tau}_{50}$, 104.80 min)은 가장 큰 세포 보호 활성을 나타내었다. TLC, HPLC, LC/ESI-MS/MS을 이용하여 수영 전초 추출물 중 에틸아세테이트 분획에 대하여 성분 분석을 실시하였다. 그 결과, 에틸아세테이트 분획은 orientin, isoorientin, vitexin, isovitexin 등의 플라보노이드가 함유되어 있음을 확인하였다. 이상의 결과들은 수영의 전초 추출물이 $^1O_2$을 비롯한 활성산소종을 소광 또는 소거함으로써 태양 자외선에 노출된 피부에서 항산화제로서 작용할 수 있음을 가리키며 항노화 기능성 화장품 원료로서 응용 가능성이 있음을 시사한다.

• 공업화학
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• 제28권6호
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• pp.696-704
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• 2017

본 연구에서는 마가목 가지 비발효 추출물과 발효균주 Lactobacillus pentosus를 이용하여 발효시킨 발효 추출물에 대하여 항산화 및 MMPs 발현 억제 효과를 조사하고 유효 성분을 분석하였다. 마가목 가지 비발효 추출물과 발효 추출물의 자유 라디칼 소거 활성($FSC_{50}$)에서 비발효 추출물은 $41.0{\mu}g/mL$, 발효 추출물은 $58.2{\mu}g/mL$이었다. $Fe^{3+}-EDTA/H_2O_2$계에서 활성산소 소거 활성($OSC_{50}$)은 각각 2.6, $3.0{\mu}g/mL$로 나타났다. 진피 섬유아세포에서 세포내 활성산소 소거활성은 $10{\mu}g/mL$에서 각각 35.3, 40.2%를 나타났다. 진피 섬유아세포에서 MMPs (MMP-1, MMP-2 및 MMP-3) 발현은 $10{mu}g/mL$에서 비발효 추출물은 각각 68.3, 35.0 및 24.2%이었고, 발효 추출물은 각각 84.3, 70.5 및 69.2% 억제되었다. 마가목 발효 전후 추출물의 성분 변화는 TLC, HPLC 및 LC/ESI-MS/MS를 이용하였다. 그 결과, caffeic acid, (-)-epicatechin, isoquercitrin 및 quercetin을 확인하였다. 이상의 결과들은 L. pentosus를 이용한 마가목 가지 발효 추출물은 비발효 추출물보다도 ROS 소거 활성이 크게 나타났고 또한 MMPs 발현 억제 효능도 보여주었다. 따라서 마가목 가지 발효 추출물은 항노화 화장품 소재로서 응용 가능성이 있음을 시사하였다.

• 생약학회지
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• 제44권4호
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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.

• 한국식품영양학회지
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• 제26권3호
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• pp.547-552
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• 2013

황백 껍질은 황벽나무(Phellodendron amurense)의 건조된 수피로부터 얻어진다. 이 수피는 한국의 전통 한약제로서, 설사, 황달, 무릎과 발의 통증, 요도관 및 피부 감염증에 폭넓게 사용되어 왔다. 본 연구는 황벽나무의 메탄올 추출액으로부터 항균성 화합물 분리를 위해 CPC 방법으로 효과적으로 수행하였다. 두 용매의 CPC 최적조성은 n-butanol:acetic acid:water(4:1:5 v/v/v)이었다. 이동상의 유속은 1,000 rpm 회전력에서 상승법으로 분당 3 $m{\ell}$ 속도로 전개시켰다. CPC에서 분리된 분획분은 prep-HPLC로 정제하였다. 분리된 palmatine은 $^1H$, $^{13}C$-NMR, ESI-MS 데이터 분석으로 확인하였다.

• Journal of Ginseng Research
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• 제44권5호
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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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• 제45권6호
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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.