• Title/Summary/Keyword: 크로마토 그래피 추출

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Determination of Polybrominated Biphenyls in Biota Samples Using Gas Chromatography/Mass Spectrometry (기체크로마토그래피/질량분석법을 이용한 생체시료 중 Polybrominated Biphenyls의 분석법)

  • Hong, Jongki;Baek, In-Girl;Kim, Hyub;Kim, Do-Gyun;Seo, Jung-Joo;Seo, Jong-Bok;Park, Hyun-Mee;Lee, Kang-Bong
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.666-674
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    • 2000
  • The present study describes an analytical method for the determination of polybrominated biphenyls (PBBs) in biota samples by gas chromatography-mass spectrometry (GC/MS). PBBs are extracted twice from 20 g samples with mixture solvent 40mL acetone and 80mL hexane using ultrasonic agitation for 20 min. Lipids in extracts are degraded by concentrated sulfuric acid and then PBBs are purified with Florisil column. The purified extracts are analyzed by GC/MS-selected ion monitoring mode for the quantitation of PBBs in biota sample. The overall recovery yields of PBBs range between 77 and 111% under these experimental conditions.

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Determination of Phthalates in Biota Samples Using Gas Chromatography/Mass Spectrometry (기체크로마토그래피/질량분석법을 이용한 생체시료 중 프탈산 에스텔류의 분석법)

  • Seo, Jung-Ju;Na, Yuncheol;Hong, Jongki
    • Analytical Science and Technology
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    • v.14 no.5
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    • pp.400-409
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    • 2001
  • A method for the analysis of most common phthalate acid esters (9 secies) in biota samples by gas chromatography-mass spectrometry-selected ion monitoring mode is described. Phthalates in biota samples are extracted by organic solvent and purified by Florisil column. Phthalates are easily contaminated during extraction prodedure. Since the extraction and cleanup steps for biota samples generally are more complicate than those for water or sediment samples, we compared with contamination state of each sample work-up step. By applying this developed method, the overall recoveries ranged between 79 - 117% in biota sample which was spiked with standards. For phthalates used in this study, the quantitaive accuracy, elution pattern on Florisil column, and detection limits were also investigated.

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Inhibition of Aflatoxin-producing Fungi with Antifungal Compound Produced by Bacillus subtilis (Bacillus subtilis가 생산하는 길항물질에 의한 아플라톡신 생성균의 억제)

  • Kang, Kill-Jin;Jeoung, Ji-Hyun;Cho, Jung-Il
    • Journal of Food Hygiene and Safety
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    • v.15 no.2
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    • pp.122-127
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    • 2000
  • An antifungal bacterium was isolated to inhibit of the growth of Asp. flavus and Asp. parasiticus, and its antifungal compounds were purified from lyophilized culture broth using chromatographic methods. Antifungal bacterium #19 which was shown a higher inhibitory activity on the growth of aflatoxin producing fungi was identified as Bacillus subtilis. The purified antifungal compound(1 mg) was demonstrated strong antifungal activity against the aflatoxin producing fungi.

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Determination of the Homocysteine, Cysteine and Methionine in Human Plasma by Gas Chromatography with Electron Capture Detector (기체크로마토그래피-전자포획검출기를 이용한 혈장 중의 Homocysteine, Cysteine 및 Methionine의 동시 분석법)

  • Myung, Seung-Woon;Chang, Yoon-Jung;Yoo, Eun-Ah;Park, Joon-Ho;Min, Hye-Ki;Kim, Myung-Soo
    • Analytical Science and Technology
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    • v.12 no.5
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    • pp.408-414
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    • 1999
  • A selective and sensitive method for the derivatization of total homocysteine (Hcy) and the related compounds in plasma by gas chromatograph (GC)-electron capture detector (ECD) has been developed. To determine total homocysteine, cysteine (Cys), and methionine (Met) in human plasma using GC-ECD, analytes were reduced and converted into their N(O,S)-ethylearbonyl pentafluoropropyl (PFP) ester by derivatization with ethyl chloroformate and pentafluoropropyl alcohol (PFP-OH) in plasma. The best derivatizing agent N(O,S)-ethyl carbonyl PFP ester, was chosen by comparing the sensitivity of derivatized analysis in GC-ECD. The derivatized analytes in plasma were extracted by chloroform, and subsequently back-extracted with hexane and analyzed by GC-ECD. The calibration carves ($R^2$ > 0.990) were linear over the range $5-50{\mu}mol/L$ of Hcy and Met, $40-400{\mu}mol/L$ of Cys spiked in plasma. The detection limit observed by the established method was below $0.5{\mu}mol/L$. This method is highly sensitive and specific in the analysis of Hcy, Cys, and Met. Therefore, we suggest that this method is appropriate in the analysis of trace concentration of Hcy, Cys, and Met in biological fluids.

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Radioactivity Analysis of $^{55}Fe\;and\;^{63}Ni$ in Dismantled Concrete (해체 콘크리트 폐기물에 포함된 $^{55}Fe$$^{63}Ni$ 방사능 분석)

  • Kang, Mun-Ja;Chung, Kun-Ho;Hong, Sang-Bum;Choi, Geun-Sik;Lee, Chang-Woo
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.5 no.1
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    • pp.19-27
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    • 2007
  • Combined method of extraction chromatography and liquid scintillation analysis was established for determinating $^{55}Fe\;and\;^{63}Ni$ radioactivity in solid samples. Activated concrete wastes generated from dismantling KRR-2 were analysed. The sequential separation including precipitation and extraction chromatography resulted in the above 90% chemical recoveries of Fe. Above 62% recoveries of Ni were obtained by this procedure exception to 43.6 and 46.5% recoveries. The seperation and counting procedure was also confirmed with spiked samples of known quantity. The measured and spiked quantity were agreed with the 3.7% and 0.7% variations in the $^{55}Fe\;and\;^{63}Ni$ experiments, respectively. The radioactivities of $^{55}Fe$ in the dismantled concretes are shown from below MDA to maximum 362 Bq/g. The radioactivities of $^{63}Ni$ in all concrete samples are below MDA. The $^{63}Ni$ doesn't exist in dismantled concretes from KRR-2. The radioactivity of $^{55}Fe$ is decreased rapidly as the sampling depth is increased from the concrete surface.

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Gibberellin-like Activities Produced by mycorrhizal fungus, Pisolithus tinctorius (균근균(菌根菌), Pisolithus tinctorius가 생산(生産)하는 Gibberellin양(樣) 활성(活性))

  • Park, Keun-Hyung;Kang, Sung-Hoon;Kim, Dong-Youn;Kim, Kwan;Rhee, Chong-Ouk;Jung, Ji-Heun
    • Applied Biological Chemistry
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    • v.27 no.1
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    • pp.40-44
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    • 1984
  • Experiments on the GA production ability by ectomycorrhizal fungus, Pisolithus tinctorius was carried out to investigate specific physiological phenomena of growth increase in host plants by formation of mycorrhizae, The culture extract of P. tinctorius was purified by solvent fractionation, sephadex LH-20 chromatography, silica gel partition chromatography and TLC, successively. GA activities in the purified GA fractions were monitored by micro-drop bioassay using dwarf rice seedlings, 'Tan-ginbozu'. $30{\sim}60%$ EtOAc election fractions of silica gel pardon chromatography and the zone of Rf $0.1{\sim}0.4,\;0.6{\sim}0.8$ of TLC exhibited the GA-like activities. The GA activities were increased with the more treated amount of culture extracts. This activity in 100ml of culture solution was equivalent to 0.1ng of $GA_3$.

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Separation for the Determination of $^{59/63}Ni$ in Radioactive Wastes (방사성 폐기물 내 $^{59/63}Ni$ 정량을 위한 분리)

  • Lee, Chang-Heon;Jung, Kie-Chul;Choi, Kwang-Soon;Jee, Kwang-Young;Kim, Won-Ho
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.3 no.4
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    • pp.309-317
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    • 2005
  • A study on the separation of $^{99}Tc,\;^{94}Nb,\;^{55}Fe,\;^{90}Sr\;and\;^{59/63}Ni$ in various radioactive wastes discharged from nuclear power plants has been performed for a use in their quantification which is indispensible for the evaluation of the radionuclide inventory Ni was recovered along with Ca, Mg, Al, Cr, Ti, Mn, Ce, Na, K, and Cu through the sequential separation procedure of Re(as a surrogate of $^{99}Tc$), Nb, Fe and Sr by anion exchange and Sr-Spec extraction chromatography. In this research, chemical separation of Ni from the co-existing elements was investigated by cation exchange and Ni-Spec extraction chromatography. Precipitation behaviour of Ni and the co-existing elements with dimethylglyoxime(DMG) was investigated in ammonium $citrate/ethanol-H_2O$ and tartaric $acid/acetone-H_2O$ in order to purify separated Ni fractions and to prepare $^{59/63}Ni$ source for the radioactivity measurement using a gas proportional counter. Recovery of Ni separated through ion exchange chromatographic separation procedure was $92.1\%$ with relative standard deviation of $0.9\%$. In addition, recovery of Ni with DMG in the tartaric $acid/acetone-H_2O$ was $85.6\%$ with relative standard deviation of $1.9\%$.

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Effect of Spore-forming Eumycetes on the Chemical Change of Korean Ginseng Components -II. Spectroscopic Studies on Free Fatty Acid and Total Saponin in the Root of Panax ginseng C. A. Meyer- (포자형성진균류(胞子形成眞菌類)가 한국산(韓國産) 인삼성분(人蔘成分)의 화학적(化學的) 변화(變化)에 미치는 영향(影響) -제(第) 2 보(報): Panax ginseng C. A. Meyer의 뿌리에 존재(存在)하는 유리지방산(遊離脂肪酸)과 total saponin의 분광학적(分光學的) 연구(硏究)-)

  • Han, Kang-Wan;Nam, Chang-Woo;Jo, Jae-Sun;Oh, Sung-Ki
    • Korean Journal of Food Science and Technology
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    • v.13 no.3
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    • pp.209-218
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    • 1981
  • Free fatty acid and total saponin, which were extracted from the spent media and colony of the strain Phizopus delemar Rh-1, were qualitatively examined by GLC and spectroscopic methods and compared with these of intact ginseng media. The 18, 18, and 14 free fatty acids were respectively identified from the control, spent media and colony. Among them, $iC_{12:0},\;C_{16:2},\;C_{17:0},\;C_{18:3}\; and\;C_{20:0}$ acids were not detectable from the colony. In add ition, $C_{16:2}\;and\;C_{20:0}$ peaks were rot found in the spent media and control, respectively. The isible absorption spectra of free fatty acids and total saponins in the control, spent media and colony were invariable. In contrast, however, the infrared and ultraviolet absorption spectra showed significant spectral variations, particularly in the it finger-print region, demonstrating that the ginseng components were considerably utilized by the strain Rhizopus delemar Rh-1.

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Separation of High Purity Terbium Using Extraction Chromatography (추출 크로마토그래피를 이용한 고순도 테르븀의 분리)

  • Lee, Kwang-Pill;Park, Myoung-Jin;Park, Keung-Shik;Lee, Hueng-Lark;Piao, Zhexiu
    • Analytical Science and Technology
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    • v.12 no.5
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    • pp.370-374
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    • 1999
  • Extraction chromatography was used to scarch optimum separation conditions of terbium. Stationary phase was 2-ethylhexyl-2-ethylhexyl phosphonic acid(HEH[EHP])levextrel (-100~+150 mesh), column size was ${\Phi}20{\times}530mm$ and kept constantly temperature at $50^{\circ}C$, adsorption flow rate of $0.2mL/cm^2{\cdot}min$, elution flow rate of $1.0mL/cm^2{\cdot}min$, column diameter to packing height of 1:15. But to search optimum separation conditions of terbium, it changed the eluent acidity, the loading weight of sample. the composition of sample. In conclusion, acidity was 0.6 N HCl, loading weight of sample was about 5% and composition of sample was $Gd_2O_3(20%)+Tb_4O_7(60%)+Dy_2O_3(20%)$. Moreover purity of separated terbium by ICP-AES analysis was 99.98% in yield of 99.99%.

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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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