• Title/Summary/Keyword: Silica Gel Chromatography

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Isolation of Herbicidal Compounds from Pulsatilla koreana Roots (백두옹(Pulsatilia koreana Nakai) 뿌리로부터 제초활성물질의 분리)

  • 정형진
    • Korean Journal of Plant Resources
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    • v.9 no.1
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    • pp.47-54
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    • 1996
  • To search herbicidal compounds in Pulsatilla koreana Nakai, methanol extract of P. koreana roots was purified by sequences of XAD-7 column chromatography, silica gel adsorption column chromatography, silica gel flash column chromatography, preparative layer chromatography and preparative high performance liquid chromatography(Prep, HPLC).The final Prep. HPLC gave two herbicidally-active fractions. These fractions treatment at 100ppm inhibited the root length of Echinochloa crus-galli seedlings by 48% and 60% as compared with the control, respectively. Components in the two active fractions were analyzed by GC-MS Spectrometry. These compounds, which were isolated from P. koreana roots, were identified as several fatty esters, hydrocarbons, squalene, evidonol, and a diazepin analogue.

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A Study of Glutathione S-transferase Inhibitors obtained from Allium cepa var. cepa Extract (양파 추출물에서의 글루타티온 전달효소 활성 저해제에 관한 연구)

  • Lee, Kwang-Soo;Park, Kyung-Sook
    • The Korean Journal of Food And Nutrition
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    • v.26 no.4
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    • pp.725-730
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    • 2013
  • In this study, an ethanol extract being obtained from Allium cepa var. cepa examins the inhibitory effects on the glutathione S-transferase and the separation had been done by silica-gel column chromatography using various eluents, such as ethyl acetate, methanol, and 50% methanol. A volume of column fraction was 50ml and evaporation has been performde by the rotary evaporator under reduced pressure. Each fraction is being examined by thin layer chromatography and the UV spectrum at 365 nm was used to investigate separation patterns of spots on thin layer chromatography. When the eluent was changed, the spot patterns showed another different pattern on thin layer chromatography, so on. Fractions showing similar pattern are combined and eventually, three fractions are obtained. Each fraction is testified to examine the inhibition effects on glutathione S-transferase. All of these showed inhibition effects on glutathione S-transferase. The GC-MS shows that each fraction contains more than 2 compounds.

Identification and Biological Activity of Two New Phytotoxins Isolated from Botrytis cinerea (Botrytis cinerea로부터 분리한 두 개의 새로운 phytotoxin의 구조 결정 및 생물활성)

  • Kim, Geum-Jung;Yoon, Mi-Young;Kim, Heung-Tae;Choi, Gyung-Ja;Jang, Kyoung-Soo;Choi, Yong-Ho;Park, Myung-Soo;Cha, Byeong-Jin;Kim, Jin-Cheol
    • Research in Plant Disease
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    • v.15 no.2
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    • pp.112-119
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    • 2009
  • We discovered two novel phytotoxins produced by the pathogenic fungus, Botrytis cinerea. Among the twenty-five B. cinerea isolates, which were obtained from various host plants in 1994 and 1996, twenty-two showed strong or moderate pathogenicity on five plants such as cucumber, tomato, red pepper, tobacco and Chinese cabbage. The culture filtrate of the B. cinerea 2-16 strain showed the most potent phytotoxic activity in a tobacco leaf-wounding assay. Two novel phytotoxins were isolated from the liquid cultures of B. cinerea 2-16 by ethyl acetate extraction, flash silica gel column chromatography, silica gel column chromatography, Sephadex LH-20 column chromatography, preparative TLC and subsequently preparative HPLC. Their chemical structures were determined to be 3-O-acetyl botcinol and 3-O-acetyl botcinolide, respectively, by mass and NMR spectral analyses. These two phytotoxins caused leaf necrosis in a leaf-wounding bioassay, and significant electrolyte leakage from leaf tissues of tobacco. In the two bioassays tested, 3-O-acetyl botcinol exhibited stronger phytotoxic activity than 3-O-acetyl botcinolide. This is the first report on the production of both 3-O-acetyl botcinol and 3-O-acetyl botcinolide from B. cinerea.

β-Galactosidase-catalyzed Synthesis of 1, 2-Hexanediol Galactoside and its Purification using Ethyl Acetate Extraction followed by Silica Gel Chromatography (대장균 β-Galactosidse를 이용한 1, 2-Hexanediol galactoside의 합성과 Ethyl Acetate 추출 및 Silica Gel Chromatography를이용한 정제)

  • Kim, Yi-Ok;Jung, Kyung-Hwan
    • Journal of the Korean Applied Science and Technology
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    • v.33 no.3
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    • pp.498-506
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    • 2016
  • 1, 2-Hexanediol galactoside (HD-gal) has been previously synthesized from 1, 2-hexanediol (HD), in which recombinant ${\beta}$-galactosidase (${\beta}$-gal) of Escherichia coli (E. coli) was used for transgalactosylation reaction. In this study, a method for HD-gal purification from the reaction mixture was particularly investigated. Using ${\beta}$-gal-containing E. coli, HD-gal was synthesized from 75 mM HD for 48 hr under 300 g/l lactose concentration. Then, HD-gal synthesis from HD was confirmed by TLC analysis, and the existence of E. coli ${\beta}$-gal during 48 hr-reaction was also confirmed by Western blotting, in which the conversion yield of HD to HD-gal reached about 94% during 48 hr. To establish an efficient method for HD-gal purification, we carried out the solvent extraction of the reaction mixture, followed by silica gel chromatography, particularly in order to remove the residual HD. Two water-immiscible solvents, such as methylene chloride and ethyl acetate, were investigated comparatively to find out appropriate solvent. Then, it was found that residual HD was almost removed when ethyl acetate extraction of water phase of reaction mixture was carried out four times. Subsequently, silica gel chromatography was carried out, and purified HD-gal could be finally obtained. The production yield for HD-gal from 75 mM HD was $8.9{\pm}0.6%$ (n=3) (mole basis) or $21.1{\pm}1.4%$ (n=3) (weight basis). For further study, using purified HD-gal, we will investigate the minimum inhibitory concentrations (MICs) of HD-gal against bacteria. In addition, cytotoxicity to human skin cells of HD-gal will be examined.

Chromatographic Techniques for the Isolation and Purification of Metalloporphyrins from Crude Asphalts (크로마토그래피를 이용한 아스팔트로 부터 금속 포르피린의 분리및 정제)

  • Woo Ki Chae
    • Journal of the Korean Chemical Society
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    • v.28 no.6
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    • pp.393-398
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    • 1984
  • Porphyrin-rich materials were obtained from some crude asphalts by gel permeation chromatography and silica gel chromatography. After extraction of each chromatographic fractions through alumina with pyridine, more concentrated metalloporphyrins were obtained. Demetallation of metalloporphyrins was possible without destroying porphyrin ring to provide different type of metal free porphyrins.

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Optimum Synthesis and Characterization of Precursor Solution for a Hard Coating Silica Film Prepared by Sol-Gel Process

  • Kim, Seon Il;Kim, Gu Yeol;Im, Hyeong Mi;Lee, Bong U;Na, Jae Un
    • Bulletin of the Korean Chemical Society
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    • v.21 no.8
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    • pp.817-822
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    • 2000
  • Crack-free hard coating siIica films were prepared by sol-gel processfrom twokinds of silicon alkoxide (tetra-ethoxysilane and methyltrimethoxysilane) and two kinds of alcohol (methanol and isopropyl alcohol) with an acid catalyst,acetic acid. A silicate framework of the precursor solution was investigated by infrared spectros-copy (IR) in the process of hydrolysis and condensation. Theextent of the condensation in the intermediates was elucidated by gel permeation chromatography (GPC) and 29Si-NMR spectroscopy. The hard coating films werecharacterized by IR,scanning electron microscope (SEM), thermo gravimetric analyzer (TGA) and dif-ferential scanning calroimeter (DSC). The synthetic condition for the crack-free and transparent silica film for-mation was optimized interms of starting materials for the precursor solution as well as preparation method of the silica film.

The Chemical Constituents of the Stem Barks of Fraxinus rhynchophylla (물푸레나무(Fraxinus rhynchophylla) 수피의 추출성분)

  • Yang, Eun-Ju;Lee, Dong-Geun;Lee, Jong-Won;Kim, Yae-Sil;Lim, Sun-Ha;Song, Kyung-Sik
    • Applied Biological Chemistry
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    • v.50 no.4
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    • pp.348-351
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    • 2007
  • The stem barks of Fraxinus rhynchophylla was extracted with 95% EtOH, and the concentrated extract was successively partitioned with $CH_2Cl_2$, n-BuOH, and $H_2O$ in order to investigate the major phytochemicals. From the $CH_2Cl_2$ soluble fraction, a sterol (1) was isolated through the repeated silica gel column chromatographies. Three additional compounds (2-4) were isolated from the n-BuOH soluble fraction through silica gel, RP-18, and Sephadex LH-20 column chromatographies. Their chemical structures were elucidated as daucosterol $(1;{\beta}-sitosterol-3-O-{\beta}-D-glucopyranoside)$, caffeic acid (2), 6,8-dihydroxy-7-methoxycoumarin (3), and coniferaldehyde glucoside (4) by comparing their spectral data with those in the literatures. All isolates (1-4) were the first to be isolated from F. rhynchophylla.

THIN LAYER CHROMATOGRAPHIC SEPARATION OF LEAF XANTHOPHYLLS (THIN LAYER CHROMATOGRAPHY 에 의한 CAROTENOID의 분석)

  • LEE Kang Ho
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.1 no.2
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    • pp.73-79
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    • 1968
  • The resolving capacities of xanthophyll pigments on thin-layers of Silica Gel, Hyflo super-Cel, and Micro-Cel C with varying concentrations of acetone in petroleum ether as the developing solvent were compared. The results showed that the resolving capacity of Micro-Cel C thin-layer was superior to others and satisfactory for the separation of leaf carotenoids in clearly separated six bands; carotenes, lutein-zeaxanthin, antheraxanthin, violaxanthin, an unidentified band, and neoxanthin, when it was developed with $13\%$ acetone-petroleum ether solution for 15 to 20minutes in an unsaturated chamber. Adhension of Micro-Cel C to glass was adequate without binder. Calcium sulfate used as a binder appeared to inactivate the resolving capacity of Micro-Cel C. Removing an about 0.2cm-wide layer on bo side of thin-layer slide helped to prevent 'edge effect' which gave tailing and faster solvent ascending along the side than the center. An adequate thickness of thin-layer was obtained when a 3 ml aliquot of the suspension in which l0g powdered Micro-Cel C was suspended in 75 ml distilled water was coated on a $2\times20cm$ glass slide.

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A Nucleoside with Lipid Peroxidation Inhibitory Activity from Agrocybe cylindracea. (버들송이로부터 분리한 Nucleoside계 화합물의 지질과산화 저해활성)

  • 이인경;윤봉식;유익동
    • Microbiology and Biotechnology Letters
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    • v.26 no.6
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    • pp.558-561
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    • 1998
  • In the screening for lipid peroxidation inhibitors from edible mushroom, Agrocybe cylindracea, a bioactive compound AG 8 was isolated. The AG 8 was purified from methanol extract of its fruit body by Diaion HP-20 column chromatography, ethyl acetate extraction, and silica gel column chromatography, consecutively. Based on various NMR studies including $^1$H irradiation and HMBC experiments, the AG 8 was identified as MTA, 5'-deoxy-5'-methylthioadenosine. This compound inhibited lipid peroxidation with an $IC_{50}$/ value of 3.2 $\mu\textrm{g}$/$m\ell$. The MTA was isolated for the first time from basidiomycetes.

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Isolation and Characterization of Benzoic Acid with Antimicrobial Activity from Needle of Pinus densiflora (솔잎에서 항미생물 활성을 갖는 benzoic acid의 분리 및 동정)

  • Kuk, Ju-Hee;Ma, Seung-Jin;Park, Keun-Hyung
    • Korean Journal of Food Science and Technology
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    • v.29 no.2
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    • pp.204-210
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    • 1997
  • The ethyl acetate (EtOAc) extracts from needles of Pinus densiflora were showed antimicrobial activities against bacteria, yeast and fungi. The antimicrobial active substance of EtOAc extracts were successively purified with solvent fractionation, silica gel adsorption column chromatography and Sephadex LH-20 column chromatography. The purified active substance was isolated as crystals and identified as benzoic acid by $MS,\;^{1}H-NMR\;and\;^{13}C-NMR$. The amount of benzoic acid was 0.608 mg per gram of fresh needle of Pinus densiflora.

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