• Title/Summary/Keyword: Preparative Chromatography

Search Result 245, Processing Time 0.036 seconds

Cosmetic Activities of Nyasol from the Rhizomes of Anemarrhena asphodeloide (지모의 뿌리줄기로부터 분리된 nyasol의 미용효과)

  • Park, Yhun Jung;Ku, Chang-Sub;Kim, Min-Jin;Lee, Mi Kyeong;Kim, Ki Ohk;Ryu, Hyung Won;Song, Hyuk-Hwan;Kim, Doo Young;Oh, Sei-Ryang
    • Journal of Applied Biological Chemistry
    • /
    • v.58 no.1
    • /
    • pp.31-38
    • /
    • 2015
  • The rhizomes of Anemarrhena asphodeloide was extracted with 100% ethanol and concentrated subfractions were separated with medium pressure liquid chromatography-based activity profiling. One compound was isolated from the subfraction 10 through the repeated preparative high performance liquid chromatography (prep-HPLC). According to physico-chemical and spectroscopic data including NMR and MS, the chemical structures of the compound was determined as nyasol (1). Nyasol was exhibited potent inhibitory activity for NO ($IC_{50}:12.5{\mu}g/mL$), tyrosinase ($IC_{50}:12.5{\mu}g/mL$), melanin contents ($IC_{50}:12.5{\mu}g/mL$), thymus and activation-regulated chemokine (TARC) production ($IC_{50}:6.25{\mu}g/mL$). As a result, nyasol has an excellent inflammation-dependent anti-whitening and TARC production activity. It could be used to a large range of functional cosmetics.

Antifungal Activity of Decursinol Angelate Isolated from Angelica gigas Roots Against Puccinia recondita (당귀로부터 분리한 decursinol angelate의 밀 붉은녹병에 대한 항균활성)

  • Yoon, Mi-Young;Kim, Young-Sup;Choi, Gyung-Ja;Jang, Kyoung-Soo;Choi, Yong-Ho;Cha, Byeong-Jin;Kim, Jin-Cheol
    • Research in Plant Disease
    • /
    • v.17 no.1
    • /
    • pp.25-31
    • /
    • 2011
  • Rust causes significant losses in the yield and quality of various crops. The development of new effective and environmentally benign agents against the pathogen is of great interest. In the course of searching a natural antifungal compound from medicinal plants, we found that the methanol extract of Angelica gigas roots had a potent control efficacy against wheat leaf rust (WLR) caused by Puccinia recondita. The antifungal substance was isolated from the methanol extract by silica gel column chromatography, alumina column chromatography and $C_{18}$ preparative HPLC. It was identified as decursinol angelate by EI-MS and $^1H$-NMR data. In in vivo test, decursinol angelate effectively suppressed the development of WLR and red pepper anthracnose (RPA) among the 6 plant diseases tested. In addition, the wettable powder-type formulation of ethyl acetate extract of A. gigas roots significantly suppressed the development of WLR. The crude extract containing decursinol angelate and the chemical appear to be a potential candidate for control of WLR. In addition, this is the first report on the in vivo antifungal activity of decursinol angelate against WLR as well as RPA.

Secondary Metabolites from the Mycelial Culture Broth of Phellinus linteus (상황(Phellinus linteus) 배양 균사체의 2차 대사산물에 대한 화학적 연구)

  • Song, K.S.;Cho, S.M.;Ko, K.S.;Han, M.W.;Yoo, I.D.
    • Applied Biological Chemistry
    • /
    • v.37 no.2
    • /
    • pp.100-104
    • /
    • 1994
  • From the 48 hour-cultured mycelial broth of Phellinus linteus, six compounds were isolated by means of ethyl acetate extraction, silica gel column chromatography and preparative thin layer chromatography, consecutively. Compound 1 was identified as a succinic acid by the comparison of its spectral data with authentic sample. Compounds 2 and 3 were identified as p-hydroxyphenyl acetic acid methyl ester and p-hydroxybenzaldehyde by spectroscopic studies, respectively. NMR and MS studies of compound 6 revealed that it was 2,5-dihydroxymethyl furan. Compound 4, which showed similar NMR absorptions and MS fragmentation pattern with those of compound 6 was identified as 2-hydroxymethyl-5-methoxymethylfuran. These structures were verified by the spectral data of the acetate derivatives of the compounds. Compound 5 was supposed to be a N-acetyltyramine from its $^1H-NMR$ and EI-MS data, and its structure was confirmed by a synthesis starting from tyramine.

  • PDF

Isolation and Identification of an Antioxidant Substance from Heated Onion (Allium cepa L.) (열처리 양파로부터 항산화물질의 분리동정)

  • Hwang, In-Guk;Kim, Hyun-Young;Lee, Sang-Hoon;Hwang, Cho-Rong;Oh, Seung-Hee;Woo, Koan-Sik;Kim, Dae-Joong;Lee, Jun-Soo;Jeong, Heon-Sang
    • Journal of the Korean Society of Food Science and Nutrition
    • /
    • v.40 no.3
    • /
    • pp.470-474
    • /
    • 2011
  • The objectives of this study were to identify antioxidant substance in heated onion. The isolation of active compound was performed in three steps: silica gel column chromatography, preparative TLC, and preparative HPLC. The structure of the purified compound was determined using spectroscopic methods, i.e., ultraviolet, mass spectrometry, $^1H$-NMR, $^{13}C$-NMR, and DEPT. The antioxidant activities of isolated compound were evaluated and compared with $\alpha$-tocopherol, ascorbic acid, and butylated hydroxytoluene (BHT) using DPPH and ABTS assay. The isolated compound was identified as 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one(DDMP). The DPPH radical-scavenging activity ($IC_{50}$) of the DDMP was in the following order: ascorbic acid (45.3 ${\mu}g/mL$)>$\alpha$-tocopherol (69.2 ${\mu}g/mL$)>DDMP (241.6 ${\mu}g/mL$)>BHT (268.0 ${\mu}g/mL$). In addition, DDMP showed strong ABTS radical-scavenging activity of 569.0 mg AA eq/g.

Preparative Isolation of Ginseng Saponin from Panax ginseng Root Using High-speed Countercurrent Chromatography (High-speed countercurrent chromatography를 이용한 인삼 saponin의 대량 분리 농축)

  • Lee, Chang-Ho;Lee, Boo-Yong
    • Korean Journal of Food Science and Technology
    • /
    • v.36 no.3
    • /
    • pp.518-521
    • /
    • 2004
  • Ginseng saponin was isolated from panax ginseng root using high-speed countercurrent chromatography (HSCCC). Preliminary studies were performed to optimize physical properties of two-phase solvent system and operating parameters including rotation speed of column, elution mode of mobile phase, and flow rate. Two-phase solvent system for isolation of ginseng saponins was composed of chloroform, water, and methanol as blending solvent. Chloroform-aqueous methanol (4:6) systems with various concentration of methanol in water were evaluated for retention of stationary phase in column. Retention of stationary phase decreased with increasing flow rate in tail-to-head elution mode using upper phase as mobile phase and head-to-tail elution mode using lower phase as mobile phase. Latter mode produced high retention at flow rate of 5 mL/min. Optimum conditions for isolation of saponin were chloroform/methanol/water (40/39/21) solvent system; mobile phase, of lower organic layer, flow rate, of 5 mL/min, head to tail elution mode, rotation speed, of 800 rpm, and sample injection, of $200{\mu}L$, Recovery yield of ginseng saponin from panax ginseng root extract by HSCCC was 63.6%, and the purity of HSCCC fractions was verified by TLC.

Isolation and Structural Analysis of Acetyl Soyasaponin $A_1$ from Hypocotyl of Soybean (콩 Hypocotyl에서 Acetyl Soyasaponin $A_1$의 분리 및 구조 분석)

  • Kim, Sun-Lim;Bang, Myun-Ho;Kim, Jung-Tae;Chi, Hee-Youn;Chung Ill-Min;Kim, Hyun-Bok;Berhow Mark A.
    • KOREAN JOURNAL OF CROP SCIENCE
    • /
    • v.51 no.spc1
    • /
    • pp.166-173
    • /
    • 2006
  • Soyasaponins are phytochemicals of major interest fur their health benefits. Chemical investigation of a soybean phytochemical concentrate resulted in the isolation and identification of triterpenoid saponins. The MeOH extraction of defatted hypocotyl separated from soybeans was peformed by the automated solvent extractor (ASE). Fractionation was performed on a flash column ($150mm{\times}40mm$ i.d.) packed with a preparative $C_{18}$ reverse phase bulk packing material $(125\AA,\;55-105{\mu}m)$ and monitored at 210 nm, and collected 14 fractions. Consequent Fsat preparative column liquid chromatography (Fast PCLC) was performed for the purification of Fraction-I (Fr-I) collected from the fraction 8 and 9 of flash chromatography. Fsat PCLC was performed on a Luna $C_{18}\;10{\mu}m,\;100{\AA}$, semipreparative reverse phase column ($250cm{\times}50mm$ i.d.) for the purification of isolated unknown compound (Fr-I-2). Chemical structure of acetyl soyasaponin $A_1\;(MW:1436.6,\;C_{67}H_{104}O_{33})$ was identified and determined by a combination of extensive NMR ($^1H-NMR$, 400 MHz; $^{13}C-NMR$, 100 MHz; DEPT), IR, UV, and ESI-MS analysis.

Antioxidative Effects of Cultivation of Streptomyces sp. BH-405 Isolated from Marine Origin (해양에서 분리한 Streptomyces sp. BH-405 배양액의 항산화 효과)

  • 류병호;이영숙;양승택
    • KSBB Journal
    • /
    • v.15 no.2
    • /
    • pp.150-155
    • /
    • 2000
  • Antioxidative activity of c비ture of Streptomyces sp. BH-405 was investigated. After removal of pellets of Streptomyces sp. B BH-405, antioxidative substances were is미ated and suc$\infty$sively purified from culture of Streptomyces sp. BH-405 by by thin | layer chromatography $\pi$LC) or silica gel column chromatography. The fraction 3 obtained from ethylether fractionation of the C culture appeared highest level of anti oxidative activity as determined by thiocyanate method. Band 2 obtained by further P purification of this fraction showed higher anti oxidation level than that of same concentration of dl- $\alpha$ -tocopherol, butylated h hydroxy anisole (BHA). The band 2 showed higher rate of 1, 1.diphenyl 2-picrylhydrazyl (DPPH) decolorization than dl-$\alpha$-tocopherol. In the rat liver microsomes, band 2 rapidly inhibited lipid peroxidation which was initiated enzymatically by r reduced nicotinamide adenine dinucleotide phosphate (NADPH) or non-enzymatically by Fenton’s reagent. Band 2 inhibited on | lipid peroxidation of mitochondria or the linoleic acid hydro peroxide induced peroxidation system. It is concluded that band 2 obtained by fractionation of Streptomyces sp. BH-405 cultivation contained antioxidants with the capacity to inhibit oxidative m modification.

  • PDF

Enzymatic Synthesis and Characterization of Galactosyl Trehalose Trisaccharides

  • Kim, Bong-Gwan;Lee, Kyung-Ju;Han, Nam-Soo;Park, Kwan-Hwa;Lee, Soo-Bok
    • Food Science and Biotechnology
    • /
    • v.16 no.1
    • /
    • pp.127-132
    • /
    • 2007
  • [ ${\alpha},\;{\alpha}$ ]-Trehalose was efficiently modified by a transgalactosylation reaction of Escherichia coli ${\beta}-galactosidase$ using lactose as a donor to yield two galactosyl trehalose trisaccharides. The reaction products of trehalose by the enzyme were observed by thin layer chromatography (TLC) and high performance anion exchange chromatography (HPAEC) and were purified by BioGel P2 gel permeation chromatography and recycling preparative HPLC. Liquid chromatography-mass spectrometry (LC-MS) and ^{13}C$ nuclear magnetic resonance (NMR) analyses revealed that the structures of the main products were $6^2-{\beta}-D-galactosyl$ trehalose (1) and $4^2-{\beta}-D-galactosyl$ trehalose (2). A reaction of 30%(w/v) trehalose and 15%(w/v) lactose at pH 7.5 and $45^{\circ}C$ resulted in a total yield of approximately 27-30% based on the amount of trehalose used. The galactosyl trehalose products were not hydrolyzed by trehalose. In addition the mixture of transfer products (9:1 ratio of 1 to 2) showed higher thermal stability than glucose, lactose, and maltose, but less than trehalose, against heat treatment over $100^{\circ}C$ at pH 4 and 7. It also exhibited better thermal stability than sucrose at pH 4 alone.

Rational and efficient approach to the preparation of the active fractions of Scutellaria baicalensis (황금(Scutellaria baicalensis) 유효분획물 제조의 합리적이고 효율적인 접근방법)

  • Kim, Doo-Young;Kim, Won Jun;Kim, Jung-Hee;Oh, Sei-Ryang;Ryu, Hyung Won
    • Journal of Applied Biological Chemistry
    • /
    • v.62 no.1
    • /
    • pp.31-38
    • /
    • 2019
  • Scutellaria baicalensis Georgi (Scutellariae Radix) has been widely used as a dietary ingredient and traditional herbal medicine such as diuretic, hyperlipidemia, antibacterial, anti-allergy, anti-inflammatory and anticancer properties. In this study, the isolation of biomarkers or bioactive compounds from complex S. baicalensis extracts represents an essential step for de novo identification and bioactivity assessment. The bioactive fraction consisted of eight compounds which was chromatographed on an analytical high performance liquid chromatography column using two different gradient runs. A simulative replacement of the analytical column with a medium pressure liquid chromatography and open column allowed the determination of gradient profile to allow sufficient separation in the preparative scale. From the optimized method, eight standard compounds have been identified in the fractions. In addition, MS, UV, HRMS detection was provided by ultraperformance liquid chromatographyequadrupole time-of-flight mass spectrometry (UPLC-QTof-MS) of all fractions. Therefore, this scale up procedure was successfully applied to a S. baicalensis extract.

Isolation of Berberine from the Rhizome of $Coptis$ $chinensis$ by Centrifugal Partition Chromatography (향류분배 크로마토그라피법에 의한 황련($Coptis$ $chinensis$) 뿌리로 부터 Berberine의 분리)

  • Kim, Jung-Bae
    • The Korean Journal of Food And Nutrition
    • /
    • v.24 no.4
    • /
    • pp.617-621
    • /
    • 2011
  • $Coptis$ $chinensis$ Franch rhizome is one of the important traditional Korea medicines with anti-inflammatory, anti-bacterial, anti-hypertensive and anti-cancer properties. The methanol extract of rhizome from the $Coptis$ $chinensis$ rhizome was purified by using preparative centrifugal partition chromatography (CPC) and HPLC method. The optimum two-phase CPC solvent system was composed of n-butanol:acetic acid:water at a ratio of 4:1:5. Berberine (16.8 mg) was successfully isolated by CPC and HPLC. The chemical structure of the compound was identified by (1 H)$^1H$, $^{13}C$-NMR and ESI-MS spectral data analysis.