• Title/Summary/Keyword: 추출 크로마토그래피

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NMR Spectral Analysis of Steroids Isolated from the Sponge Penares incrustans (핵자기공명분광기를 이용한 해면동물 Penares incrustans에서 분리된 스테로이드 화합물의 분석)

  • 서영완
    • Journal of Aquaculture
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    • v.15 no.3
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    • pp.139-143
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    • 2002
  • Saringosterols have been isolated from the sponge Penares incrustans. The structure of these compounds have been determined by extensive 2-D NMR experiments such as $ ^1 H$ COSY, HMQC, and HMBC and by comparison with published data. Assignment for carbons of saringosterols for the first time has been done.

Analysis of Organic Acids in Urine by Gas Chromatography/Mass Spectrometry (기체 크로마토그래피/질량분석법을 이용한 요 중에서의 유기산 분석)

  • Yoo, Eun Ah;Ko, Sun Young;Kim, Jong Won;Kim, Jeong Uk;Myung, Seung Woon
    • Journal of the Korean Chemical Society
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    • v.41 no.9
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    • pp.471-482
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    • 1997
  • GC/MS was used to find an optimum experimental condition for the screening of organic acids in urine. Urinary organic acids were isolated through the liquid-liquid extraction method (LLE) to examine the influence of pH and the effect of including the back extraction and oximation processes respectively on the extraction. When pH was adjusted to 0.5 during the extraction without oximation process, relatively higher recovery rate and the smallest relative standard deviations (0.3-12.4%) were obtained. By removing the interference, the addition of back extraction made possible surer identification of organic acids with retention time of 15-16 minutes. Under this condition, we obtained the content distribution of urinary organic acids in healthy Korean children (n=16) by establishing the calibration curves for 51 standard organic acids.

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Extractives from Epimedium koreanum Nakai (삼지구엽초(Epimedium koreanum Nakai)의 추출성분)

  • Lee, Tae-Seong;Cho, Jae-Hyun;Hwang, Byung-Ho
    • Journal of Korea Foresty Energy
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    • v.24 no.2
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    • pp.16-23
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    • 2005
  • The air dried of Epimedium koreanum Nakai was extracted with MeOH and its extractives were concentrated with a vacuum evaporator. The extractives were fractionated with a series of n-hexane, chloroform (${CHCl}_3$), butanol (BuOH), ethyl acetate (EtOAc) and water on a separately funnel. Each fraction was freeze dried to give some dark brown powder. The EtOAc and BuOH soluble fractions were chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-n-hexane mixture as eluents. The isolated compounds were tested with a cellulose TLC developed with TBA and 6% acetic acid and then visualized on UV lamp or sprayed with vanillin-HCl-EtOH. The purified compounds were flavonoids and their glycosides, and organic acid as follows : (+)-catechin, icariin, hyperoside, Ikarisoside A and caffeic acid. The structures of each compounds were confirmed by $^1H-NMR,\;^{13}C-NMR$ and Mass spectra. Also, executed qualitative analysis as use GC/MS(Libraries search) about ${CHCl}_3$ soluble compounds of each part.

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Studies on the Development of Liquid Chromatographic Methods for Pesticide Residues (II) : The Development of the Analytical Method for Thiocarbamates Herbicides (잔류농약의 액체 크로마토그래피 분석법 개발에 관한 연구 (II) Thiocarbamates 제초제의 잔류농약 분석법 개발)

  • Lee Dai Woon;Choi Yong Wook
    • Journal of the Korean Chemical Society
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    • v.36 no.1
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    • pp.66-74
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    • 1992
  • A method for the multiresidual simultaneous analysis of 11 thiocarbamates was studied using HPLC. Thiocarbamate in Chinese cabbage was analyzed in the order of extraction, partition, and cleanup in their optimum condition. Acetone was chosen as an extracting solvent. As a partitioning solvent, the mixture of 50% methylene chloride and petroleum ether containing extremely small water content showed good recoveries of thiocarbamate from the water layer. Partition efficiency was affected by pH of the water layer; it remained almost constant under the acidic and neutral condition while decreasing under the basic condition. The comparison done in cleanup step showed that the column chromatographic method is superior to the treatment of coagulating reagent. As an absorbent, the mixture of charcoal, magnesia, and celite with the ratio of 1 : 2 : 4 gave better recoveries and also effectively removed chlorophyll. Over the total procedure, the average recoveries for thiocarbamates in Chinese cabbage were 91% at about 2 ppm fortification level within the relative standard deviation of 8%, and the minimum detection limit (MDL) was 2.2${\sim}$9.3 ng.

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Extraction of Glycosaminoglycan from Sea Hare, Aplysia kurodai, and Its Functional Properties 1. Optimum Extraction of Polysaccharide and Purification of Glycosaminoglycan (군소(Aplysia kurodai)에 분포하는 글루코사미노글리칸의 추출과 기능특성 1. 다당류 추출의 최적화와 글루코사미노글리칸의 정제)

  • Yoon, Bo-Yeong;Choi, Byeong-Dai;Choi, Yeung-Joon
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.39 no.11
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    • pp.1640-1646
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    • 2010
  • The optimum condition was investigated for the extraction of glycosaminoglycan (GAG) from sea hare, Aplysia kurodai. The most effective enzyme was Flavourzyme for extraction of glycosaminoglycan. The optimum incubation temperature and time for hydrolysis were $60^{\circ}C$ and 15 hr, respectively. The yield of precipitated polysaccharide depended on Brix and ethanol volume. The most effective concentration of Brix and ethanol were sixty and 5 volume of ethanol, respectively. Most GAG was eluted between 0.5 M and 0.75 M NaCl gradient on DEAE-Sepharose column, and identified by electroconductivity. The contents of hexuronic acid from polysaccharide extract and GAG were 1.0 g/100 g and 6.0 g/100 g, respectively. Hexosamine of polysaccharide and GAG as indicator of GAG component was 5.6 g/100 g and 25.7 g/100 g, respectively. GAG was identified as heparan sulfate compared with bands of other GAG on agarose gel electrophoresis, and its molecular weight was 29.6 kDa on Superdex 200 HR column.

Isolation of Alliin in Garlic and Its Quantitative Determination by High Performance Liquid Chromatography and Studies on the Antimicrobial Efforts of Alliin and Ethanol Extracts from Korean Garlic(Alliium sativum L.) (마늘 중 고속 액체 크로마토그래피에 의한 알린의 분리 및 정량과 Alliin과 에탄올 추출물의 항균효과에 관한 연구)

  • 위성언
    • The Korean Journal of Food And Nutrition
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    • v.16 no.4
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    • pp.296-302
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    • 2003
  • First. the purification and analysis of alliin in garlic from different origins by alliin-HPLC determination method were studied. Allinase in garlic was inactivated by heating in boiling water followed by extraction of alliin in garlic with 80% methanol. To remove free amino acids and alliin homologs in garlic, garlic extract was separated by cation exchange column which was packed with amberlite CG-120 resin using 40L d-water as eluent. Alliin in garlic extract was crystallized in a mixture of acetone (50$^{\circ}C$):H$_2$O:acetic acid=70:29:1 and then recrystallized in a mixture of acetone (50$^{\circ}C$):H$_2$O:acetic acid=75:24:1. Obtained alliin was identified by melting point. TLC, microscope observation and mass spectrometry. High performance liquid chromatography (HPLC) following pre-column derivatization of cystein derivatives with o-phthaldialdehyde/2-mercaptoethanol has succeessfully been applied to the analysis of various garlics. Each alliic of standard solution and garlic extract was derivatized to isoindole derivative by o-phthaldialdehyde /2-mercaptoethanol and then analyzed by HPLC. Six point calibration was done by using alliin peak area. Lineality was observed at 0 ∼ 1.0mg/ml of alliin concentration. Weighted regression line function was Y=6254X - 256077. By this function, alliin contents in various garlics were 0.34 ∼ 0.73% fresh weight. Second study was designed to evaluate the effects of garlic extracts of various concentrations on the growth of various pathogenes (Eubacterium limonsum, Bacteroides fragilis, Salmonella typhimurium, Salmonella typhi, Shigella sonnei, Kiebsiella pneumoniae, Enterobacter cloacae, Pserdomonas aeruginosa, Escherichia coli). For antimicrobial effects against microorganism, totally minimal inhibition concentrations (MIC) of alliin were from 5,000 to 20,000ppm. MIC of ethanol extract were 1,250 to 10,000ppm.

Isolation and Structural Identification of Antioxidant Substances from Ethyl Acetate Extract of Conyza canadensis (망초(Conyza canadensis) Ethyl Acetate 추출물의 항산화성 물질의 분리와 동정)

  • Hyun Sook Song
    • Journal of Naturopathy
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    • v.12 no.1
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    • pp.7-15
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    • 2023
  • Background: As a result of analyzing the components of wild Conyza canadensis, it contains physiologically active ingredients, so it is necessary to identify the compound. Purposes: It was to study the compound's molecular structure; a previous study showed that C. canadensis contains antioxidant substances. Methods: The ultrasonic pulverized lysate of C. canadensis stem and leaves was first extracted with 90% methanol and then five organic solvents. Next, the extracts was fractionated by HPLC, LC/MS chromatography, and NMR analyzers identified the molecular structure. Results: 100 g of dry C. canadensis was sonicated in 90% methanol and concentrated under reduced pressure to 11.96 g of a crude extract. Then, this crude was extracted with five types of solvents to obtain 123.8 mg of n-hexane, 448.2 mg of dichloromethane, 1047.7 mg of ethyl acetate (EA), 2563.8 mg of butanol, and 7.04 g of water. The EA extracts were fractionated by LC-MS and then re-fractionated to obtain F1 to F20. Next, the F15 was further fractionated to obtain nine fine fractions. Finally, the F17 fraction was re-fractionated to obtain ten fine fractions. As a result of LC-MS and NMR spectrometer analysis of the F15-7, the structure of this compound was confirmed as 3,5-dicaffeoylquinic acid. As a result of examining the structures of the F17-4 and F17-5 fractions, Quercetin-3-o-β-galactose was identified. In addition, the form of the F17-10 was confirmed to be 1,3,4-tri-caffeoylquinic acid. Conclusions: This study demonstrated that C. canadensis contained phenolic antioxidants, and its utilization may be expected.

Supercritical Fluid Extraction of Catecnin Compounds from Green Tea (녹차에서 카테킨 화합물의 초임계 유제 추출)

  • 나영진;이윤우;김재덕;노경호
    • KSBB Journal
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    • v.16 no.4
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    • pp.327-331
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    • 2001
  • Catechin compounds from the Green tea cultivated in Bosung (Chollanamdo) were extracted using supercritical fluid and various additives, and analyzed by reversed-phase high performance liquid chromatography (RP-HPLC). The chromatographic column was packed with LiChrospher 100RP-18(15 $\mu$m), and water was used as the mobile phase with 0.05% phosphoric acid and acetonitrile. Gradient election was applied to separate EGCG by changing the mobile phase compositions. Comparing the extraction yield of three different types of supercritical fluids, pure CO$_2$, with additives of water and ethanol (5 wt,%), the extraction amount of EGCG was most abundant in the suprcritical CO$_2$with ethanol. However, more was extracted and pure higher purity was achieved by solvent extraction using ethanol.

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The Analysis on VOCs That Occurs in Leather Cultural Heritage with SPME (고체상미세추출법(SPME)을 이용한 피혁 재질로부터 발생된 휘발성 유기화합물 분석기술 연구)

  • Chung, Yong-Jae
    • Journal of Conservation Science
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    • v.28 no.2
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    • pp.113-118
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    • 2012
  • Cultural heritages emit volatile organic compounds(VOCs) during degradation as chemical, biological factors. These VOCs in the atmosphere are degradation factors for another materials. But non-destructive organic analysis methods are uncommon, and have difficulties for field application. In this study, solid phase micro-extraction(SPME) and gas chromatography( GC) are carried out for analysis of VOCs which are emitted from leather, and prove SPME field holder's efficiency. I analize leather archival objects at The National Archives of Korea by cross-checking GC and SPME methods. It could be confirmed that the compounds are (E)-2-nonenal, butyl hydroxy toluene emitted itself from leather.

Anti-platelet Effect of Carvacrol Extracted from Thuja Orientalis L.;A Possible Mechanism Through Arachidonic Acid Pathway (백자인에서 추출된 Carvacrol의 항혈소판 효과)

  • Ahn, Byeong-Joon;Song, Ho-Sueb
    • Journal of Acupuncture Research
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    • v.24 no.2
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    • pp.31-38
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    • 2007
  • 목적 : 백자인에서 추출된 Carvacrol이 혈소판 활성화와 혈액 응고에 미치는 영향에 대해 알아보고자 하였다. 방법 : Carvacrol의 항혈소판 효과의 기제를 밝히기 위해 토끼 혈소판으로 Arachidonic Acid 유리,TXB2, PGD2, 12-HETE의생성을 방사선 크로마토그래피 분석을 사용하여 측정하였다. 결과 : 1. U46619를 제외하고 Collagen과 AA에 의해 유발된 응고는 Carvacrol 농도에 따라 억제되었다. 2. Collagen으로 인하여 자극된 AA 유리에 대한 Carvacrol의 유의한 억제 효과는 나타나지 않았다. 3. AA로 유발된 TXB2, PGD2와 12-HETE의 생성억제에 대한 실험에서 Carvacrol은 유의한 억제가 있는 것으로 나타났으며,농도의존적으로 억제되었다. 결론 : Carvacrol은 항혈소판 작용이 있는 것으로 볼 수 있다. 이는 한의학에서 활혈거어 작용으로 해석될수 있으며,타박상,윌경곤란증,탈모증 등 어혈질환의 예방 및 치료와 관련된 약침개발에 기초가 될수 있을 것으로 사료된다.

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