• Title/Summary/Keyword: silica-gel column chromatography

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Novel Sesquiterpenoid Compounds from Culture Broth of Stereum hirsutum

  • Cho, Yang-Rae;Yun, Bong-Sik;Lee, In-Kyoung;Lee, Tae-Ho;Yoo, Ick-Dong
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1998.11a
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    • pp.130-130
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    • 1998
  • Two novel compounds SSC1 and SSC2 were isolated from culture broth produced from the strain of Stereum hirsutum by using of YM broth. They were isolated through HP-20 column chromatography, silica gel column chromatography and preparative HPLC, successively. The molecular formulas of SSC1 and SSC2. were determined as C$\sub$15/H$\sub$22/O$_3$ by high resolution EI -mass. The chemical structures of SSC1 and SSC2 were determined as sesquiterpenoid compounds by spectroscopic analysis of UV, IR, $^1$H NMR, $\^$13/C NMR, DEPT, HMQC and HMBC spectrum.

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Purification and Identification of Squalene Synthase Inhibitor Isolated from Fermented Soybean Paste

  • Choi, Sung-Won;Kim, Dong-Seob;Hur, Nam-Youn;Park, Cheon-Seok;Baik, Moo-Yeol
    • Food Science and Biotechnology
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    • v.14 no.1
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    • pp.89-93
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    • 2005
  • Squalene synthase (SQS) inhibitors were screened from various plants and food extracts. Effective SQS inhibitor was purified from fermented soybean paste using ethanol extraction, HP-20 column chromatography, ethyl acetate extraction, silica gel column chromatography, and crystallization. Through UV spectrometry, $^1H$ NMR, $^{13}C$ NMR, and mass spectrometry, SQS inhibitor was identified as daidzein with molecular mass of 254 and molecular formula of $C_{15}H_{10}O_4$. Daidzein showed $IC_{50}$ value of 50 nmol/L against SQS, confirming its potential as therapeutic agent for hypercholesterolemia.

Aspergillus candidusF1484 균주가 생산하는 항진균 화합물의 분리 및 특성

  • Kim, Sung-Uk;Lee, So-Young;Kim, Sung-Kyu;Son, Kwang-Hee;Kim, Young-Kook;Moon, Surk-Sik;Bok, Song-Hae
    • Microbiology and Biotechnology Letters
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    • v.24 no.5
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    • pp.574-578
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    • 1996
  • In the course of screening for the antifungal compounds against Candida albicans, an antifungal compound (F1480) was isolated from the culture broth of Aspergillus candidus F1484. Isolation and purification of compound F1484 were performed using ethyl acetate extraction, silica gel column chromatography, ODS column chromatography, and preparative HPLC. The structure of compound F1484 was determined by the spectroscopic analyses of EI-MS, $^{13}$C, $^{1}$H-NMR, DEPT, HMQC, and HMBC. This compound appeared to have a structure of antifungal agent, chloroflavonin. In addition to antifungal activities against the yeast phase of Candida species, compound F1484 showed cytotoxic effect against various human tumor cell lines.

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Determination of Monocrotophos Residues by HPLC

  • Lee, Young-Deuk;Kwon, Chan-Hyeok
    • Korean Journal of Environmental Agriculture
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    • v.23 no.4
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    • pp.245-250
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    • 2004
  • An analytical method was developed to determine monocrotophos residues in apple, citrus, and soil using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. Monocrotophos was extracted with acetone from apple, citrus and moist soil samples. The extract was concentrated, added with saline water, and subjected to n-hexane washing to remove nonpolar co-extractives. Dichloromethane partition was then followed to recover monocrotophos from the aqueous phase. Silica gel column chromatography was employed to further purify the extract prior to HPLC determination. Reverse-phase HPLC using an oct-adecylsilyl column was successfully applied to separate and quantitate the monocrotophos residue in sample extracts at the wavelength of 230 nm. Overall recoveries of monocrotophos from fortified samples averaged $95.3{\pm}2.1%$ (n=6), $970{\pm}0.7%$ (n=6), and $92.8{\pm}4.3%$ (n=12) for apple, citrus, and soil, respectively. The proposed method was quite reproducible and sensitive enough to replace the troublesome gas-liquid chromatographic analysis for monocrotophos residues.

Study on the Antitumor Activity of Dichloromethane Extract of Tripterygium regelii SPRAGUE (뇌공등(雷公藤) 디클로메탄(CH$_2$Cl$_2$)분획의 항암효능 연구)

  • Park, Wan-Su
    • Journal of Physiology & Pathology in Korean Medicine
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    • v.20 no.5
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    • pp.1196-1199
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    • 2006
  • Tripterygium regelii SPRAGUE is distributed in Korea and Northern China. This extract has been used as a herb medicine, especially antiparasitic, anti-inflammatory and detoxifying agent in East asia. During our research to develop new antitumor agents from natural products, Dichlorornethane (CH$_2$Cl$_2$) extract of Tripterygium regelii SPRAGUE (DTR) showed the potent apoptotic effects in A-549 lung cancer, HeLa-3 cervical cancer, SKMEL-2 melanoma cells in a dose-dependent manner. in order to purify major compounds from DTR, column chromatography was carried out gradually. Silica gel and RP-18 column chromatography for active fractions led to the isolation of a compound. The compound determined by 1 H-NMR was turned out to De Celastrol known to have antitumor activity.

Polyacetylene Compounds from Panax Ginseng C. A. Meyer

  • Shim, Sang-Chul;Koh, Hun-Yeoung;Han, Byung-Hoon
    • Bulletin of the Korean Chemical Society
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    • v.4 no.4
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    • pp.183-188
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    • 1983
  • Two major and two minor polyacetylenes were isolated from fresh white Korean ginseng roots. The petroleum ether-ethyl ether fractions containing the polyacetylene compounds were collected through solvent fractionation, partition and silica gel column chromatography. Further separation of polyacetylenic fractions was proceeded by bonded normal phase HPLC utilizing a moderately nonpolar microparticulate column. The low pressure liquid chromatography was used for the semi-preparative separation. The chemical structures of the two major polyacetylenes separated were determined by UV, IR, $^1H$ NMR, $^{13}C$ NMR, mass spectra and elemental analysis. One of them is identified to be heptadeca-1-en-4, 6-diyne-3, 9, 10-triol, a new structure, and the other is heptadeca-1, 9-dien-4, 6-diyn-3-ol, known as panaxynol.

Adsorption Column Chromatography for Simultaneous Determination of Multi-pesticide Residues (잔류농약 다성분 동시분석을 위한 흡착 크로마토그래피의 적용)

  • Kim, Chan-Sub;Ihm, Yang-Bin;Choi, Ju-Hyun;Lee, Kyoung-Mi;Lee, Young-Deuk
    • The Korean Journal of Pesticide Science
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    • v.14 no.4
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    • pp.347-360
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    • 2010
  • In order to develop the multi-residue purification method for 180 pesticides commonly used in Korea, many analytical methods on individual and multi- pesticide residues in the agricultural commodities and food product were examined. Through the modification of adsorption chromatographic methods used in Europe, the United States and Korea, the Florisil and silica-gel chromatographic systems were developed. Through these purification systems, elution profiles for all pesticides were examined. As the results, 145 pesticides were recovered in the range of 70-120% in Florisil clean-up system. The distribution of pesticides in the elution profile was 12 pesticides in the first fraction, 76 pesticides in the second fraction, 81 pesticides in the third fraction, 60 pesticides in the fourth fraction and 30 pesticides in the last fraction. And, in silica-gel system, 137 pesticides were recovered in the range of 70~120%. The distribution of pesticides in the elution profile was 22 pesticides in the first fraction, 59 pesticides in the second fraction, 102 pesticides in the third fraction, 46 pesticides in the fourth fraction and 8 pesticides in the last fraction.

Chemical Structures of Compounds Isolated from Mushroom Suillus granulatus (젖비단 그물버섯(Suillus granulatus)으로부터 분리한 저분자 화합물)

  • 강희철;윤봉식;유승헌;유익동
    • Microbiology and Biotechnology Letters
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    • v.29 no.3
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    • pp.149-154
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    • 2001
  • We have investigated the secondary metabolites from the mushroom Suillus granulatus. The methanolic extract of fruit body was separated by silica gel and Sephadex LH-20 column chromatographies. TLC and HPLC were also used for the further purification on compounds from the extracts, Nine compounds were finally isolated and their structures were assigned as 4-hydroxyphenylacetic acid 4-hydroxybenzaldehyde 2,5-dihydroxybenzoic acid methyl ester 5'-deoxy-5'methylthioadenosine. indole-3- carboxlic acid methyl ester indole 3-carboxaldehyde 1,3,5-trihydroxy 7-methylanthraquinone nicotinamide and 3-geranylgeranyl-4-hydroxybenzoic acid on the basis of NMR studies.

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Exploitation of the biologically active components in Youngia sonchifolia Max (고들빼기 생리활성물질의 검색)

  • Shin, Soo-Cheol
    • Applied Biological Chemistry
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    • v.36 no.2
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    • pp.134-137
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    • 1993
  • Yongia sonchifolia Max. has been used as raw materials of traditional Kimchi and medicinal herb in Korea. This study was performed to investigate biologically active components in the plant. First, the writer carried out the experiment of antitumor screening test against Sarcoma-180A and the cytotoxic activity against Chinese hamster V-79 cells with methanol extract of the plant. And the aqueous solution of the extract from roots of Youngia sonchifolia Max. was partitioned into n-hexane. The concentrated extract of n-hexane layer was chromatographed on silica gel column and developed with n-hexane and ethylacetate. Two yellow elutes, on concentration, were recrystallized from ethylacetate, and the $R_f$ value of TLC of the crystal was 0.43. After analysis by $^{1}H-NMR$, $^{13}C-NMR$ and MS to confirm the structure, the author could identify the compound as bauerenyl acetate, a naturally occurring pentacyclic triterpene. The crystal was colorless plate and m.p. was $280{\sim}282^{\circ}C$.

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Isolation of Phenolic Antioxidant Components from Panax ginseng (인삼으로부터 페놀성 항산화 성분의 분리)

  • Wee, Jae-Joon;Park, Jong-Dae;Kim, Man-Wook;Lee, Hyong-Joo
    • Applied Biological Chemistry
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    • v.32 no.1
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    • pp.44-49
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    • 1989
  • To isolate new antioxidants from Panax ginseng, methanol extract of Panax ginseng was fractionated into several subfractions and their antioxidant activities were measured by using ${\alpha}$, ${\alpha}-diphenyl-{\beta}-picrylhydrazyl$(DPPH). Four compounds were isolated from two subfractions that showed high DPPH quenching activities by silica gel, ${\mu}$ Bondapak $C_{18}$ or Sephadex LH-20 column chromatography. The four compounds were confirmed to be phenolic substances by color reaction and UV spectral analysis.

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