• Title/Summary/Keyword: 크로마토 그래피 추출

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The Analysis of Dioxin-like PCBs in Fishes and Shellfishes using Accelerated Solvent Extraction (ASE) System and Multilayer Column Chromatography (가속용매추출장치(ASE) 및 다층크로마토그래피를 이용한 어패류 중의 dioxin-like PCBs의 분석)

  • Oh, Keum-Soon;Park, Seong-Soo;Chung, So-Young;Sho, You-Sub;Kim, Jung-Soo;Jang, Seoung-Chul;Lee, Jong-Ok;Kim, Hee-Yun;Woo, Gun-Jo;Suh, Jung-Hyuck
    • Korean Journal of Food Science and Technology
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    • v.39 no.2
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    • pp.122-127
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    • 2007
  • In this study, an analytical method was optimized for detecting dioxin-like PCBs in fish and shellfish. Here, homogenized samples were extracted using an accelerated solvent extraction (ASE) system with 33 mL cell size. Multilayer column chromatography, which consisted of acidic, basic and neutral silica gels, was used for the clean up of the extracts. The instrumental analysis was executed by HRGC/HRMS to a resolution of 10,000 using 4 window multiple ion detection (MID) mode. For the results, the average recoveries ranged from 94.1 to 104.1% (${\pm}8.4$) and the limit of detection was approximately 0.1 pg/g at S/N ratio >3. Finally, the detected concentrations of dioxin-like PCBs for fish and shellfish were in the range of 0.030-1.836 pg TEQ/g.

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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Separation of Chromophoric Substance from Madder Plant under Different Extraction and Analytical Conditions (염료추출 및 분석 조건에 따른 꼭두서니의 색소성분 분리 거동)

  • ;S. Kay Obendorf
    • Journal of the Korean Society of Clothing and Textiles
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    • v.27 no.11
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    • pp.1350-1357
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    • 2003
  • This research was aimed to establish the standard extraction and analytical procedures for examining the chromophoric substance in madder root with the ultimate goal of identifying the dyes in badly faded textiles of archaeological origin. The separation temperature of gas chromatography, pH and other extraction conditions were tested. The results were as follows: The suitable separation temperature for the GC cappillary column was 50∼305$^{\circ}C$, and methanol was a good GC solvent for both standard alizarin and madder extraction. The best extraction of madder was achieved by 90 min soaking in room temperature followed by filtration and the actual heat extraction procedure. The best pH for extracting alizarin was pH 3 and above pH 5 alizarin was not detectible. Only alizarin and no purpurin was found in the extraction of the currently used madder plant.

Flavonoid Glycosides from Needles of Taxus cuspidata(Taxaceae) (주목 잎의 후라보노이드 배당체)

  • Ham, Yeon-Ho;Park, Wan-Geun;Han, Sang-Sup;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
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    • v.25 no.2
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    • pp.45-51
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    • 1997
  • 주목 잎을 채취하여 건조하고 아세톤-물 (7 : 3, v/v) 의 혼합액으로 추출한 후 에틸아세테이트 및 수용성 부분으로 분리하고 Sephadex-LH 20으로 충진한 칼럼을 이용하여 2개의 flavan 단량체와 2개의 후라보노이드 배당체를 단리하였다. 에틸아세테이트용성 추출물은 대부분 (+)-catechin 과 (-)-epicatechin으로 구성되어 있었으며 수용성 부분에서는 quercetin-3-0-arabinopyranosyl-($1"'{\rightarrow}6"$)-${\beta}$-D-glucoside와 quercetin-3-O-rutinoside 인 두 개의 탄수화물로 구성된 배당체를 분리하였으며 주목에서는 이들 화합물은 아직 보고된 바가 없다. 이들의 구조결정을 위하여 박층크로마토그래피를 실시하고 $^1H$-NMR과 $^{13}C$-NMR 스펙트럼을 기존의 스펙트럼과 비교, 분석하여 정확한 구조를 규명하였다.

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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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Ursolic Acid Isolated from Mume Fructus Inhibits Urease Activity of Helicobacter pylori (오매 추출물에 함유된 Ursolic Acid에 의한 Helicobacter pylori의 Urease 활성억제)

  • Park, Chan-El;Park, Chang-Ho
    • Korean Chemical Engineering Research
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    • v.51 no.5
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    • pp.591-596
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    • 2013
  • Urease activity of Helicobacter pylori was most strongly inhibited by extract of Mume Fructus among ethanol (70%, v/v) extract of 6 herbal materials selected from our previous work, database on traditional herbal materials, and literature data on Korean plant resources. Active compounds in the extract of Mume Fructus were separated by batch extraction, and further purified by chromatography in a silica gel column and an octadecyl silica gel column using solvents of different polarity. By NMR analysis of the last chromatographic fraction we identified ursolic acid as the active compound of urease inhibition. The result suggests that this component in Mume Fructus can possibly be used for the eradication of H. pylori.

Simultaneous Determination of Pesticides in Water Using a GC/MS Coupled with Micro Extraction by Packed Sorbent (MEPS-GC/MS를 이용한 농약류 동시 수질분석)

  • Lee, Ki-chang;Lee, Wontae
    • Journal of Korean Society of Environmental Engineers
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    • v.37 no.5
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    • pp.262-268
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    • 2015
  • This study established an analytical method to simultaneously determine six organophosphorous pesticides [methyldemetone-S, diazinon, fenitrothion, parathion, phentoate, and O-ethyl O-(4-nitrophenyl) phenylphosphonothioate (EPN)] and carbaryl in water using a gas chromatography/mass spectrometry (GC/MS) system coupled with on-line micro extraction by packed sorbent (MEPS) and programmed temperature vaporizer (PTV) injector. Polystyrene divinylbenzene (PDVB) was used as a sorbent of MEPS. The effects of elution solvents, pH, elution volume and draw-eject cycles of samples on sample pretreatment process were investigated. Also, quality assurance and quality control (QA/QC) and the recovery of the pesticides in environmental samples were evaluated. The elution was performed using $30{\mu}L$ of a mixed solvent (acetone : dichloromethane = 80 : 20 (v/v)). Sample pretreatment processes were optimized with seven cycles of draw-eject of sample (1 mL) spiking an internal standard and sulfuric acid. At lower pH, the analytical sensitivity of diazinon decreased, but that of carbaryl increased. The method detection limit and the limit of quantification for this method were 0.02~0.18 and $0.08{\sim}0.59{\mu}g/L$, respectively. The method precision and accuracy were 1.5~11.5% and 83.3~129.8%, respectively, at concentrations of $0.5{\sim}5.0{\mu}g/L$. The recovery rates for all the pesticides except carbaryl in various environmental samples ranged 75.7~129.3%. The recovery rate of carbaryl in effluent sample was over 200% whereas carbaryl in drinking water, groundwater, and river water were in the acceptable range.

Studies of separation and quantitation for selenium species in food (식품중의 셀레늄 화학종의 분리 및 정량연구)

  • Jang, Hee-Young;Min, Hyungsik;Lee, Jonghae;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.26 no.3
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    • pp.182-189
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    • 2013
  • The purpose of this research is to separate and quantitate selenium species in some food samples with HPLC-ICP-MS. Cation exchange chromatography showed efficient separation only for inorganic Se species while reversed phase ion pair chromatography showed good separation for both inorganic and organic Se species. $C_8$ column ($Symmetryshield^{TM}\;RP_8$, 3.5 ${\mu}m$, $4.6{\times}150$ mm) was used with optimum condition of 5% methanol mobile phase, 0.05% of nonafluorovaleric acid ion pairing reagent. Five standard Se species of Se(IV), Se(VI), SeCys(selenocystein), SeMet(selenomethionine) and Se-M-C(seleno methyl cystein) were separated successfully under the optimum condition (mobile phase; 5% methanol, ion-pairing reagent; 0.05% nonafluorovaleric acid, flow rate; 0.9 mL $min^{-1}$). To extract Se species, microwave assisted and enzyme-assisted extraction methods were studied. In enzyme-assisted extraction method, protease I for garlic, protease I plus trypsin for pork and mackerel, and protease XIV for tuna showed the best extraction efficiency. With the optimum condition for each sample, it was found that mostly inorganic Se, SeCys and SeMet are present in the sample studied ranging from few ${\mu}g$ $g^{-1}$ to few tens of ${\mu}g$ $g^{-1}$.