• Title/Summary/Keyword: Silica gel 60

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Structure of Three New Terpenoids, Spiciformisins a and b, and Monocyclosqualene, Isolated from the Herbs of Ligularia fischeri var. spiciformis and Cytotoxicity

  • Lee, Kyung-Tae;Koo, Sung-Ja;Jung, Seung-Hee;Choi, Jong-Won;Jung, Hyun-Ju;Park, Hee-Juhn
    • Archives of Pharmacal Research
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    • v.25 no.6
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    • pp.820-823
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    • 2002
  • The diethylet er fraction from the leaves extract of Ligularia fischeri var. spiciformis (Compositae) was subjected to silica gel column chromatography and yielded three new terpenoids named spiciformisin a (1), spiciformisin b (3), and monocyclosqualene (2). Acyclic diterpenes, spiciformisin a and -b, were established as 3,7,11,15-tetramethyl-1,3(20)-hexadecadiene and 3,7,11,15-tetramethyl-1,3,6,10,14-hexadecapentaene (IUPAC), respectively. A monocyclic triterpene, monocyclosqualene, were determined as [3,8,12,16,16-pentamethyl-(3,7,11,15-hexadecatetraenyl)]-3,3,5-trimethyl-1-cyclohexene. The structures were determined on the basis of NMR and MS analysis. Spiciformicin b showed potent cytotoxicity ($IC_{50},{\;}<9.7{;\}{\mu\textrm{g}}/ml$ against HL-60) in contrast to no cytotoxicity ($IC_{50},{\;}>200{\;}}{\mu\textrm{g}}/ml against HL-60 cells) of spiciformicin a with a cis-conjugated dienyl diexomethylene.

Studies on the Quality Control Method of Crude Drug Preparations (I) -Studies on the Quality Control by the TLC Profiles Analysis of ‘Samyo-Tang’- (생약복합제제(生藥複合製劑)의 품질관리(品質管理)에 관(關)한 연구(硏究)(제1보)(第1報) -TLC Scanner에 의(依)한 삼요탕(三拗湯)의 품질관리(品質管理)-)

  • Hong, N.D.;Kim, J.W.;Kim, N.J.;Shon, J.G.
    • Korean Journal of Pharmacognosy
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    • v.12 no.3
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    • pp.119-124
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    • 1981
  • In our country, in order to cure diseases, a large number of crude drug preparations has been available. Nevertheless, the development of crude drug preparations have been inhibited, because the quality control is not completed so far. Therefore, we have eontinued on studing the quality control method by Zig-zag TLC. profile analysis. The water extract of 'Samyo-Tang' and componental crude drug (Glycyrrhizae Radix, Ephedrae Herba, Armenicae Semen) were developed on Silica gel $60F_{254}\;plate\;(E.\;Merck)$ useing elution solvent. The developed plate were examined useing Dual Wavelength Zig-zag Scanner (Shimadzu). According to the results of the experiment, it could be summarized as follow: 1) Original patterns of TLC profiles of 'Samyo-Tang' componental crude drug and mixing two crude drugs of 'Samyo-Tang' were observed. 2) Original patterns TLC profile of each extract after spraying with 2% ninhydrine were observed. 3) In the extract of addition and subtraction of Ephedrae Herba, peak area of Rf 0.48 and Rf 0.60 were varied quantitatively.

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Development of Analytical Method for Cymoxanil in Agricultural Commodities using HPLC/UVD (HPLC/UVD를 이용한 농산물 중 cymoxanil의 개별 분석법 확립)

  • Kim, Ji-Yoon;Kim, Hea-Na;Kim, Ja-Young;Kim, Jong Geol;Ham, Hun-Ju;Lee, Young-Deuk;Hur, Jang-Hyun
    • The Korean Journal of Pesticide Science
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    • v.18 no.2
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    • pp.69-78
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    • 2014
  • In the present study, we developed an official individual analytical method for cymoxanil using HPLC/UVD, respectively in different representative crops. Individual analytical methods for these pesticides are not included in the Korea food code. The samples were extracted with acetonitrile, concentrated and partitioned with dichloromethane and saturated sodium chloride solution. For cymoxanil, extracts were concentrated and clean-up through silica gel column chromatography with dicloromethane/acetone (60/40 v/v) and subjected to instrumental analysis. The limit of detection (LOD) for cymoxanil were 0.1 ng and 1 ng respectively and limit of quantitation (LOQ) were 0.02 mg/kg. Recoveries for cymoxail ranged from 79.6~107.6% respectively, at fortification level of 0.02 mg/kg (LOQ), 0.2 mg/kg (10 LOQ) and 1.0 mg/kg (50 LOQ) and the coefficient of variation (CV) was less than 10%, regardless of sample types. These results were further confirmed with LC/MS. The proposed simultaneous analysis method is reproducible and sensitive enough to determine the residues of cymoxanil in the agricultural commodities. According to the validation data and performance characteristics and high sample throughput, the proposed method is suitable for routine application.

Studies on Biological Activity of Wood Extractives (X VIII) -Isolation and Antioxidant Activity of Chemical Constituents from Maackia amurensis- (수목추출물의 생리활성에 관한 연구(X VIII) -다릅나무(Maackia amurensis) 수피의 추출성분의 분리 및 항산화 활성-)

  • Kim, Woo-Jin;Lee, Hak-Ju;Lee, Sang-Keug;Kang, Ha-Young;Choi, Don-Ha;Choi, Tae-Ho
    • Journal of the Korean Wood Science and Technology
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    • v.35 no.6
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    • pp.135-144
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    • 2007
  • The dried barks of Maackia amurensis were ground, extracted with 95% EtOH, concentrated, and fractionated with a series of light petroleum ether, dichloromethane, ethyl acetate and water on a separatory funnel. Each fraction was concentrated, then a portion of dichloromethane and ethyl acetate soluble was chromatographed on a Sephadex LH-20 and silica gel 60 column using a various solvent system as eluents. The isolated compounds were identified by cellulose TLC, $^1H-$, $^{13}C-NMR$, COSY, NOESY, HMQC, HMBC, FAB and EI-MS. The structures were determined as: 7-O-$\beta$-D-glucopyranosyl-4'-methoxyisoflavone, 7-O-$\beta$-glucopyranosyl(1'''->6'')-$\beta$-D-glucopyranosyl-4'-methoxyisoflavone, 7-O-$\beta$-D-glucopyranosyl(1''''->6''')-$\beta$-D-glucopyranosyl(1'''->6'')-$\beta$-D-glucopyransoyl-4'-methoxyisoflavone, 7-O-$\beta$-D-glucopyranosyl-4', 6-dimethoxyisoflavone. The Free radical scavenging activity using DPPH of the isolated compounds were similar with that of BHT but lower than of $\alpha$-tocopherol.

Antioxidant Effect of the Fraction Isolated from Pyrus ussuriensis Leaves (산돌배나무(Pyrus ussuriensis) 잎 분획물의 항산화 효과)

  • Lee, Chang-Eon;Kim, Young-Hun;Lee, Byung-Guen;Lee, Do-Hyung
    • Journal of Korean Society of Forest Science
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    • v.99 no.6
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    • pp.885-890
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    • 2010
  • This study was conducted to confirm the application as ingredients of cosmetics through an examination of the function for anti-oxidant activity of the fraction isolated from Pyrus ussuriensis leaves. The dried leaf of Pyrus ussuriensis were extracted with acetone-$H_2O$ (6:4, v/v), concentrated and fractionated with the upper layer of acetone on a separatory funnel. Each fraction was freeze dried, then a portion of acetone soluble powder was chromatographed on a Sephadex LH-20 column using a series of aqueous methanol as eluents and also used the MIC-gel using a series of aqueous methanol as developing solvent. The isolated compounds were identified by silica-gel TLC. The concentration of total phenolic compound of Pyrus ussuriensis acetate soluble fraction was high, 914 mg/g. The results obtained from the analyses of the anti-oxidanat effects of Pyrus ussuriensis acetate fraction can be summarized as follows: In the result of DPPH scavenging radical activity, Pyrus ussuriensis acetate soluble fraction showed more than 80% at 100 ppm. SOD-like activity of one of Pyrus ussuriensis acetate soluble fractions was 77% at 1000 ppm. Xanthine oxidase inhibition of Pyrus ussuriensis acetate soluble fraction was 38% at 100 ppm. From these results, we confirmed that acetate fraction of Pyrus ussuriensis has a great potential as a natural ingredients with a natural antioxidant and antimicrobial source.

Isolation and Purification of Resveratrol from a Grape Twig (포도 송이가지에서 레스베라트롤의 분리 정제)

  • Shin, Hyun-Jae;Kang, Byung-Sun;Ahn, Jun-Bae;Kim, Bok-Hee
    • KSBB Journal
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    • v.22 no.5
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    • pp.351-355
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    • 2007
  • Resveratrol, a polyphenolic compound with antioxidative property, was purified from the grape's twig to be used as functional additives of food and/or cosmetics. Extraction of the grape's twig was performed using 80% ethanol in ultrasonic extractor for 60 min. The crude extract was purified up to 99% after elution through silica gel open column chromatography. The stability of the purified resveratrol was as follows: a half life of 90 days at 40$^{\circ}C$ and 60 days at 25$^{\circ}C$. A sensory test of the commercial grape juice including the 1-10 ppm of purified resveratrol showed better preference than the grape juice without purified resveratrol additive. Color and smell test showed no difference between the samples. The grape twig can be used as a valuable resource for the extraction of resveratrol, which would be added to nutraceutical and cosmetic products.

Antioxidant Activity of Daidzin and Puerarin toward Oxidation of Human Low Density Lipoprotein (갈근에서 분리한 Daidzin 및 Puerarin의 사람 Low Density Lipoprotein 대한 항산화 효과)

  • 박종옥;김경순;지영애;류병호
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.26 no.1
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    • pp.25-31
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    • 1997
  • Antioxidative activity of daidzin and puerarin isolated from Puerariae radix against oxidation of low density lipoprotein(LDL) was investigated. The concentration of daidzin at 100$\mu\textrm{g}$/$m\ell$ and puerarin at 60$\mu\textrm{g}$/$m\ell$ inhibited Cu$^{2+}$-mediated oxidation of LDL almost completely. The electrophoretic mobility of oxidized LDL by addition of daidzin(100$\mu\textrm{g}$/$m\ell$) and puerarin(60$\mu\textrm{g}$/$m\ell$) was faster than that of native LDL, but slower than that of oxidized LDL. The oxidized LDL induced by J774 or macrophage was inhibited strongly in the presence of 100$\mu\textrm{g}$/$m\ell$ daidzin and 60$\mu\textrm{g}$/$m\ell$ Puerarin. The formation of conjugated dienes in the oxidized LDL was strongly inhibited by 100$\mu\textrm{g}$/$m\ell$ daidzin and 60$\mu\textrm{g}$/$m\ell$ puerarin.n.

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The Effect of Sodium Gluconic Acid on the Collapsability of $CO_2$ Mold (($CO_2$ 주형의 붕괴성에 미치는 글루콘산 소다의 영향)

  • Shin, Un-Yong;Kwon, Hae-Wook;Nam, Won-Sik
    • Journal of Korea Foundry Society
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    • v.14 no.6
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    • pp.499-507
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    • 1994
  • The effect of sodium gluconic acid on the collapsability of the sodium silicate type $CO_2$ mold was studied. The bending strength was saturated with gassing $CO_2$ for 60 sec. under $1kg/cm^2$ and with the flow rate of $10\;{\ell}\;/min$. It was decreased with aging after having been fully hardened. The retained strength was reduced in the heating temperature range of $100{\sim}1,100^{\circ}C$ and the retained strength peak near the heating temperature of $100^{\circ}C$ was removed by the effect of the sodium gluconic acid. Silica gel, $Na_2CO_3$ and dehydrated sodium silicates were formed from the binder of sodium silicate with the addition of sodium gluconic acid at the heating temperature of $100^{\circ}C$. $Na_4SiO_4$ was formed by the reaction of $Na_2O$, from decomposed $Na_2CO_3$, with the dehydrated sodium silicate at $500^{\circ}C$. The crystobalite type of $SiO_2$ was formed at $900^{\circ}C$. The sodium gluconic acid had no effect on the bending strength at around $1,100^{\circ}C$ due to the combustion loss of it.

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Falcarindiol, a Polyacetylenic Compound Isolated from Peucedanum japonicum, Inhibits Mammalian DNA Topoisomerase I

  • Lee, Gwang;Park, Hyoung-Gun;Choi, Mi-Lim;Kim, Young-Ho;Park, Yong-Bok;Song, Kyung-Sik;Cheong, Chaejoon;Bae, Young-Seuk
    • Journal of Microbiology and Biotechnology
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    • v.10 no.3
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    • pp.394-398
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    • 2000
  • A methanol extract of the root of Peucedanum japonicum, used as a medicinal herb, showed an inhibitory effect on mammalian topoisomerase I activity. The methanol extract was suspended in ethyl acetate, and a topoisomerase I inhibitor in the organic soluble fraction was then isolated by silica gel and thin layer chromatography. The topoisomerase I inhibitory compound was indentified as falcarindiol based on the analysis of EI-MS, $^1$H and \ulcornerC NMR spectroscopy. This inhibitory showed cytotoxicity against human leukemia Jurkat T and HL60 cells with an IC\ulcorner value of 7 $\mu\textrm{g}$/ml. These results suggest the possibility of falcarindiol as a new anticancer agent which can be expected to have a synergistic effect on other anticancer drugs. In addition, the present data show that falcarindiol has antifungal, yet not antibacterial, activity.

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Promotion and Inhibition Phenomenon of Natural Gas Hydrates (촉진 및 저해 현상에 의한 천연가스 하이드레이트의 상평형)

  • Lee, Seungmin;Park, Sungmin;Lee, Youngjun;Kang, Boram;Seo, Yongwon
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.06a
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    • pp.217.1-217.1
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    • 2010
  • 본 연구에서는 실제 천연가스 구성성분인 메탄 (90%)+에탄 (7%)+프로판 (3%) 혼합기체를 사용하여 심해저 퇴적부에 존재하는 천연가스 하이드레이트 개발과 가스 하이드레이트 형성법을 이용한 천연가스 수송 및 저장법 개발을 위한 열역학적 특성을 살펴보았다. 천연가스 하이드레이트 개발 연구에서는 심해저 퇴적층의 영향을 살펴보기 위해 기공의 직경이 6.0, 15.0, 30.0, 100.0 nm인 다공성 실리카 젤을 사용하여 기공 직경에 따른 3상(하이드레이트 (H)-물 (LW)-기상 (V)) 평형을 측정하였다. 천연가스 하이드레이트 수송/저장법 연구에서는 천연가스 하이드레이트 형성 압력을 낮추어 줄 수 있는 열역학적 촉진제인 TBAB(농도: 5, 10, 40, 60 wt%)와 THF(농도: 1, 5.56, 10 mol%)를 첨가하여 각각의 농도에 따른 혼합 가스 하이드레이트의 3상 평형을 측정하였다. 그 결과 다공성 매질인 실리카 젤의 경우 기공 직경의 크기가 작아질수록 벌크상태의 하이드레이트에 비해 평형 온도는 낮아지고, 평형 압력은 높아져 저해효과가 커짐을 알 수 있었고, 열역학적 촉진제를 첨가했을 경우 TBAB의 농도가 40 wt%, THF의 농도가 5.56 mol%일 경우 촉진 정도가 가장 크게 나타났으며, 그 이상의 농도일 경우 가스 하이드레이트 형성 반응에 참여하지 않은 TBAB와 THF에 의해 오히려 촉진 정도가 감소하는 것을 알 수 있었다. 또한 $^{13}C$ NMR 분석을 통해 혼합 가스 하이드레이트의 격자 형성과 기체 포집에 따른 구조적인 변화에 대해서도 살펴보았다.

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