• Title/Summary/Keyword: Silica gel-water

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Isolation and Identification of Antimicrobial Active Substances from Rhodiola sachlinensis (홍경천(Rhodiola sachlinensis)에서 항균성 물질의 분리 및 동정)

  • 심창주;이규희;정재홍;이상덕;김영호;오만진
    • Food Science and Preservation
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    • v.11 no.1
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    • pp.63-70
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    • 2004
  • The antimicrobial substances from Rhodiola sachalinensis were extncted, isolated and identified. The highest level of antimicrobial activity and its yield were obtained in methanol extract. The minimum inhibition concentrations of the methanol extract were 500 $\mu\textrm{g}$mL on agar plate and 100 $\mu\textrm{g}$mL in broth media for four gram positive and four gram negative microbials. The methanol extract was fractionated by n-hexane, chloroform, ethyl ether, ethyl acetate, and butanol, orderly. The separate was developed on the TLC plate with different solvent system ratio of chloroform and methanol. Nine substances were isolated from chloroform and methanol mixture(9:1, v/v). Among them, three isolates showed antimicrobial activity. Three substances separated by HPLC were identified by GC/MS(EI) spectrum and $^1$H, /sup13/C-NMR spectrum. They were gallic acid, (-)-epicatechin and kaempferol. The antimicrobial activities of each substances were shown gallic acid, (-)-epicatechin, kaempferol orderly.

Isolation of 20(S)-Ginsenoside Rg3 and Rg5 from the Puffed Red Ginseng (팽화 홍삼으로부터 20(S)-Ginsenoside Rg3와 Rg5의 분리 및 구조동정)

  • An, Young-Eun;Cho, Jin-Gyeong;Baik, Nam-In;Choi, Sung-Won;Hur, Nam-Yoon;Park, Seok-Jun;Kim, Byung-Yong;Baik, Moo-Yeol
    • Food Engineering Progress
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    • v.14 no.2
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    • pp.159-165
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    • 2010
  • Red ginseng tail roots (9.8 g water/100 g sample) were puffed at 7, 8, 9, and 10 $kg_{f}/cm^{2}$ using a rotational puffing gun. Puffed red ginseng was extracted with 70% ethanol, and the concentrated extract was successively partitioned with diethyl ether, n-butanol and $H_{2}O$. Two unknown ginsenosides from puffed red ginseng were found at 63 and 65 min of retention time in HPLC chromatogram suggesting that chemical structure of some ginsenosides might be altered during the puffing process. Identification of two unknown compounds was carried out using TLC, HPLC and NMR. Two major compounds were isolated from TLC. According to TLC result, compound I was expected to be the mixture of ginsenosides Rk1 and Rg5, and compound II was expected to be a 20(S)-ginsenoside $Rg_{3}$. Three compounds were isolated from n-butanol fraction through repeated silica gel and octadecyl silica gel column chromatographies. From the result of $^{1}H$- and $^{13}C$-NMR data, the chemical structures of unknown compounds were determined as ginsenoside $Rg_{5}$ and 20(S)-ginsenoside $Rg_{3}$. Unfortunately, ginsenoside $Rk_{1}$ could not be separated from ginsenoside-$Rg_{5}$ in the compound I. It was carefully reexamined using HPLC and confirmed that the last unknown compound was ginsenoside-$Rk_{1}$.

Effect of Solidago altissima L. Extract on Forage Crop Germination

  • Ho-Jun Gam;Yosep Kang;Eun-Jung Park;Ki-Yong Kim;Sang-Mo Kang;In-Jung Lee
    • Proceedings of the Korean Society of Crop Science Conference
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    • 2022.10a
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    • pp.114-114
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    • 2022
  • There are 28 families and 166 species of exotic weeds on agricultural land and among these, 23 families and 80 species of exotic weeds occur on pastures. Among them, the Solidago altissima is a perennial weed belonging to the asteraceae family and it is an exotic weed that spreads to the surrounding area using methods such as high seed production, vegetative propagation using underground rhizomes and allelochemical. Accordingly, in 2009, the Ministry of Environment designated it as an ecosystem-disrupting species. This study was conducted to obtain basic data about the effects of S.altissima derived allelochemicals on forage crops. The root of S.altissima was separated, dried in the shade and then pulverized to prepare an root powder. Powder was repeatedly extracted with methanol for 3 days and concentrated under reduced pressure to obtain an root methanol extract. Dissolve the extract in distilled water, dispense it in a separate-funnel and proceed with liquid-liquid extraction by adding equal amounts of n-haxane (Hex), chloroform (CHCI3), ethyl acetate (EtoAC), and butanol (BuOH) in order of increasing polarity. A seed-bioassay was performed using fractions for each solvent, followed by separation and purification by silica gel column chromatography. As a result of the fraction germination test for each solvent, the IC50 values using the fresh weight of each fraction were 898.3 mg L-1, 676.3 mg L-1, 1160 mg L-1 and 1360 mg L-1. CA, CB, and CC fractions were obtained through primary silica gel column chromatography that used CHCI3 fraction. As a result of seed-bioassay using each fraction, the IC50 values for the fresh weight of each fraction was 537.3 mg L-1, 1280 mg L-1 and 1947 mg L-1. Based on this, 5 fractions were obtained as a result of secondary silica gel column chromatography using the CA fraction. A seed-bioassay was performed, as a result, the lowest IC50 value was calculated as 226.7 mg L-1 in the CAE fraction. Based on this, the fraction was analyzed by GC-MS. The results of this study can be used as basic research data on the effects of weeds on forage crops and allelochemicals secreted from S. altissima.

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Development of Biologically Active Compound from Edible Plant Sources-XV. Isolation of Triterpene Glycosides from the Leaf of Petasites japonicus (식용식물자원으로부터 활성물질의 탐색-XV. 머위(Petasites japonicus)잎으로부터 Triterpene 배당체의 분리)

  • Bang, Myun-Ho;Park, Jin-Kyu;Song, Myoung-Chong;Yang, Hye-Joung;Yoo, Jong-Su;Ahn, Eun-Mi;Kim, Dae-Keun;Baek, Nam-In
    • Applied Biological Chemistry
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    • v.48 no.4
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    • pp.421-424
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    • 2005
  • The leaf of Petasites japonicus was extracted with 80% aqueous MeOH and solvent fractionated with EtOAc, n-BuOH and water successively. From the EtOAc fractions, two triterpenoids were isolated through the repeated silica gel and ODS column chromatographies. The chemical structures of the isolated terpenoids were determined as rosamutin (1) and peduncloside (2) through the interpretation of several spectral data including 2D-NMR such as $^1H-{^1H}$ gCOSY, gHSQC and gHMBC.

Purification and Characterization of an Antifungal Antibiotic from Bacillus subtilis LAM 97-44 (Bacillus subtilis LAM 97-44가 생산하는 항진균성 항생물질의 정제 및 특성)

  • Lee, No-Woon;Kwon, Tae-Jong;Yi, Dong-Heui
    • Applied Biological Chemistry
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    • v.46 no.2
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    • pp.69-73
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    • 2003
  • A novel antifungal antibiotic for azole-resistant Candida albicans was purified from the culture broth of Bacillus subtilis LAM 97-44 by butanol extraction, Diaion HP-20 and Dowex-50 adsorption chromatography, silica gel flash chromatography followed by HPLC and designated LAM-44A. LAM-44A was stable for 60 min at $100^{\circ}C$, and pH range from 2 to 10. MIC values were observed at $0.5-3.5\;{\mu}g/ml$ against various Candida albicans strains. The antibiotic showed no cytotoxicity for S180, MKN-45, P388, HeLa and 373 at the concentration of 1 mg/ml. LAM-f4A was colorless powder soluble in water, methanol, ethanol, butanol and negative to ninhydrin reaction. The antibiotic had maximum absorption at 273 nm in methanol, and melting point was $202^{\circ}C$. The molecular weight and formula were determined to be 282 and $C_{14}H_{34}O_5$ by $^1H-NMR,\;^{13}C-NMR$, IR spectrum and elemental analysis.

Purification of Materials Produced by Amylocolatosis sp. and Anticancer Effect in Oral Cancer Model (Amylocolatosis sp.가 생산하는 항암물질의 정제 및 구강암 모델에 미치는 항암 효과)

  • Kim, Jung;Park, Young-Min;Lim, Do-Seon
    • Journal of dental hygiene science
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    • v.3 no.1
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    • pp.11-14
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    • 2003
  • A methylotrophic Actinomycetes strain, which produce the anti-oral cancer activity compound, was isolated from soil and estimated as Amylocolatosis sp. based on taxonomic studies. A methanol didn't have influence on the production of the anticancer compounds. These compound were isolated by ethylacetate extract, silica gel column chromatography, sephadex LH-20 column and reverse phase HPLC. The compounds were very stable under heat ($121^{\circ}C$), acid(pH 2.0) and alkali(pH 11.0) treatment. The cytotoxic effect of isolated anticancer compounds on various cancer cell lines such as A549, SNU-1, KB, L1210, and Sarcoma 180 was investigated by MTT assay method. And these produced compounds also showed the broad antimicrobial spectrum to test strains such as bacteria and yeast.

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Isolation and Identification of Antimicrobial Compound from UlGeum (Curcuma longa L.) (울금으로부터 식품부패미생물에 대한 항균성 물질의 분리 및 동정)

  • Choi, Hae-Yeon
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.38 no.9
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    • pp.1202-1209
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    • 2009
  • Antimicrobial activity of UlGeum (Curcuma longa L.) was investigated. Methanol extract of dried UlGeum was fractionated to hexane, chloroform, ethyl acetate, butanol and water fraction. The antimicrobial activity of five crude fractions were examined using impregnated paper disk agar diffusion. Ethyl acetate fraction showed the highest inhibitory effect on the microorganisms such as B. subtilis, S. aureus, E. coli, L. monocytogenes and V. parahaemolyticus at 1,000 ${\mu}g$/disc. Ethyl acetate fraction was further fractionated by silica gel column and thin layer chromatography (TLC). The antimicrobial compound was isolated from their fractions and its chemical structure was identified as a 2,3-dihydrobenzofuran by GC-MS and $^1H$-NMR.

Physicochemical Characterization and NMR Assignments of Ginsenosides Rb1, Rb2, Rc, and Rd Isolated from Panax ginseng

  • Cho, Jin-Gyeong;Lee, Min-Kyung;Lee, Jae-Woong;Park, Hee-Jung;Lee, Dae-Young;Lee, Youn-Hyung;Yang, Deok-Chun;Baek, Nam-In
    • Journal of Ginseng Research
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    • v.34 no.2
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    • pp.113-121
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    • 2010
  • The fresh ginseng roots were extracted with aqueous methanol, and the obtained extracts were partitioned using ethyl acetate, n-butanol, and water, successively. The repeated silica gel and octadecyl silica gel column chromatogaraphy for n-butanol fraction afforded four diol ginseng saponins, ginsenosides $Rb_1$, $Rb_2$, $R_c$, and Rd. The physicochemical, spectroscopic, and chromatographic characteristics of these ginsenosides were measured and compared with those reported in the literature. Some of the peak assignments in previously published $^1H$- and $^{13}C$-nuclear magnetic resonance (NMR) spectra were inaccurate. This study employed two-dimensional NMR experiments, including $^1H-^1H$ correlation spectroscopy, heteronuclear single quantum correlation, and heteronuclear multiple bond connectivity, to determine exact peak assignments.

Antioxidative Activity and Cytotoxicity on Human KB cell of Extracts from Rhododendron mucronulatum Turcz. Flower (진달래꽃 추출물의 항산화 효과 및 인체 KB cell에 대한 세포독성)

  • Park Seung-Woo;Kim Sang-Gyo;Kim Mee-Jeoung
    • Food Science and Preservation
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    • v.13 no.4
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    • pp.501-505
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    • 2006
  • This study was carried out to investigate the antioxidative activity and cytotoxicity on human KB cell of extract from Rhododendron mucronulatum flower, and also to determine the contents of total polyphenol and flavonoid. The methanol extract of Rhododendron mucronulatum flower was fractionated with various solvents such as hexane, chloroform, ethyl acetate, butanol and water. The DPPH radical scavenging activities of ethyl acetate fraction had stronger activity than other fractions. So, antioxidative substances of ethyl acetate fraction were crude purified by silica gel column chromatography. The DPPH radical scavenging activities of crude purified fraction 2 and 3 were more than 90% at 40 ppm. In the presence of $100{\mu}g/mL$, growth inhibition on human KB cell by WST-1 assay showed 81.2% in chloroform fraction and 74.6% in hexane fraction. The contents of total polyphenol and flavonoid of ethyl acetate traction were 32.70% and 20.30%, respectively, The antioxidative activity showed correlation with total polyphenol and flavonoid contents.

Biological Activity of Phenol Compound from a Cactus Cheonnyuncho (Opuntia humifusa) in Korea (천년초선인장으로부터 분리한 페놀성 화합물의 생리활성 효과)

  • Lee, Kyung-Seok;Lee, Ki-Young
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.39 no.8
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    • pp.1132-1136
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    • 2010
  • After Cheonnyuncho (Opuntia humifusa) was extracted by 70% ethanol and partitioned with hexane, chloroform, ethyl acetate, butanol, and water in order, ethyl acetate fraction with excellent antioxidant activities was acquired. Ethyl acetate fraction was conducted by TLC, and the third spot of 10 spots was selected due to its best antioxidant activities. When the third fraction further isolated on silica gel chromatography, the fourth fraction of 10 fractions had the best antioxidant activities and purified by HPLC. The molecular weight on EI-MS, and $^1H$- and $^{13}C$-NMR spectrum showed that the purified compound was taxifolin. In addition, antioxidant activities were analyzed, and the purified compound from Cheonnyuncho was found to be effective as much as $\alpha$-tocopherol, BHA. According to the analysis on antibacterial activities, the purified compound also showed more activity than benzoic acid against all pathogenic bacteria.