• Title/Summary/Keyword: 추출크로마토그래피법

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Analytical Determination of Alkylphenols, Chlorophenols and Bisphenol A in Biota Samples using Gas Chromatography/Mass Spectrometry (기체 크로마토그래피/질량분석기를 이용한 생물시료 중 알킬 페놀류, 클로로페놀류 및 비스페놀 A의 분석법)

  • Hong, Jongki;Kim, Hyup;Baek, In-Girl;Kim, Do-Gyun;Seo, Jung-Joo;Seo, Jong-Bok;Chung, Bong-Chul;Pyo, Hee-Soo;Kim, Kyung-Rae;Kim, Yong-Hwa
    • Analytical Science and Technology
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    • v.13 no.4
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    • pp.484-493
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    • 2000
  • The simultaneous analysis of alkylphenols, chlorophenols and bisphenol A in biota samples was performed by gas chromatography-mass spectrometry-selected ion monitoring mode. The phenols were extracted from sample with organic solvent and Forisil and Silica columns for clean-up procedure were compared. Recovery studies were performed at 1-ppm level of phenols added to each biota sample. Their recoveries ranged between 83 and 116% with coefficient of variations of 2.4-11.9%. To improve the detection limits of phenols, trimethylsilyl (TMS) derivatization was applied. The gas chromatographic properties of free phenols and TMS derivatized phenols were also investigated.

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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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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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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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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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Simultaneous Determination of Chlorogenic Acid and Linarin in Chrysanthemum Sibiricum Fisher by Reversed-Phase High Performance Liquid Chromatography (역상 액체 크로마토그래피에 의한 구절초 중 Chlorogenic Acids와 Linarin의 동시 정량분석)

  • Kim, Taek-Jae;Lee, Tae-Ryong;Park, Ho-Koon
    • Journal of the Korean Chemical Society
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    • v.35 no.6
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    • pp.720-724
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    • 1991
  • Simultaneous determination of chloragenic acid (CA), 3,4-o-dicafeoyl quinic acid(3,4-DCQA), 4,5-o-dicaffeoyl quinic acid (4,5-DCQA) and linarin in Chrysanthemum sibiricum Fisher was newly established by a reversed-phase high performance liquid chromatography (HPLC). Sample was extracted with 20 ml methanol for 4 hrs. The extract was cleaned up by using Sep-Pak $C_18$ cartridge and 4 ml methanol-$H_2$O(1 : 1) as eluent. Their determination was performed by means of RP-HPLC with Bondapak $C_18$ column (30 cm ${\times}$ 3.9 mm i.d., 10 ${\mu}m$ and gradient elution mode as methanol-5 mM $H_3PO_4$ solution (30 : 70). The established method was applied to various samples purchased. As a result, their content ranges showed to be 0.35~0.55% for CA, 0.46~0.76% for 3,5-DCQA, 0.077~0.23% for 4,5-DCQA and 0.16~2.72% for linarin, respectively.

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토양균에서 항생물질 및 효소억제제의 분리와 구조 연구

  • 구양모;이윤영;김경자;최응칠;김범태;주정호;이창훈
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1994.04a
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    • pp.179-179
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    • 1994
  • 새로운 항생물질을 개발하기 위하여 토양으로부터 분리한 균주를 액체 및 고체배지에서 배양하여 여러 검정균에 대하여 종이디스크법으로 항균효력을 조사하였다. 그 결과 (+), G(-), fungi 등에 강한 항균 효력을 보인 토양균 SNUS 8810-43과 Mycobacterium, fungi에 항균력을 보인 토양균 SNUS 8810-129를 선택하여 각각의 배양액에서 항생물질을 분리하고, 분리한 항생물질의 구조를 규명하고자 하였다. 토양균 SNUS 8810-43의 배양액으로부터 항생물질을 분리하기 위하여 양이온 교환 수지 관 크로마토그래피와 셀룰로오스 관 크로마토그래피를 수행하여 시료 JJH-II-46-43을 얻었다. 시료 JJH-II-46-43의 IR, $^1$H-NMR, $^{13}$C-NMR, $^1$H-$^1$H COSY, $^1$H-$^{13}$C COSY, FAB-MS 스펙트럼을 얻어 분리한 항생물질의 구조를 분석하여 이 항생물질의 구조가 N-methylstreptothricin과 동일하다는 것을 확인하였다. Mycobacterium smegmatis에 강한 활성을 나타내는 물질을 토양균 SNUS 8810-129로 부터 분리하였다. 토양균 SNUS 8810-129를 배양한 V-8 아가판을 메탄올로 추출하여 이를 실리카겔 관 크로마토그래피와 preparative TLC로 시료 LCH-IV-17B, LCH-III-387을 얻었다. 시료LCH-IV-l7B, LCH-III-387의 $^1$H-NMR, $^{13}$C-NMR, FAB-MS, CI-MS, IR등의 스펙트럼을 얻어 분리한 항생물질의 구조를 분석하여 이 항생물질이 glycolipid계 항생물질이라는 것을 알았다. $^{13}$C-NMR 상의 자료와 화학적인 방법으로 구성당을 조사한 결과 이 항생물질을 이루고있는 당은 rhamnose 임을 알았다. 또 이 항생물질을 구성하는 지방산은 화학적인 방법과 MS 스펙트럼, $^{13}$C-NMR 스펙트럼으로부터 hydroxydecanoic acid인 것으로 확인되었다. 항생물질 LCH-III-387와 항생물질 LCH-IV-l7B는 각각 rhamnose를 1, 2개 포함하고 있는 것으로 확인되었다. 그리고 동일한 탄소수의 지방산을 가지고 있는 것으로 생각되었다. 이들 항생물질을 이루는 구성당과 지방산간의 정확한 연결및 구조, 생리활성에 관한 연구는 계속 수행중에 있다.

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Purification of antigenic protein of sparganum by immunoaBnity chromatography using a monoclonal antibody (단세포군항체를 이용한 친화성 크로마토그래피에 의한 스파르가눔 항원의 순수분리)

  • Cho, Seung-Yull;Kang, Shin-Yong;Kong, Yoon
    • Parasites, Hosts and Diseases
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    • v.28 no.3
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    • pp.135-142
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    • 1990
  • The quality improvement of antigen (crude saline extract) of Spirometra maptscni 1)lerocercoid (sparganum) was investigated by protein purificatioll. The crude extract was fractionated by gel filtration through Sephacryl S-300 Superfine. Its third fraction was purified by affinity chromatography using a monoclonal antibody as ligand. When observed by SDS-PAGE, the purified protein was composed of 2 bands of 36 kDa and 29 kDa which were found already as the most sensitive components in the crude extract by immunoblots with patients sera. The quality of the purified antigen was evaluated in comparison with the crude extract by ensyme-linked imnunosorbent assay (ELISA) for the specific (IgG) antibody in sera of human sparganosis, other parasitic and neurologic diseases, and normal control. When the purified antigen was used: the sensitivity was not altered but remained high (96.4%) while the specificity was increased from 86.8% to 96.9%.

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Isolation and Purification of DHA from Skipjack Orbital Tissue Oil (가다랭이 안와조직으로부터 DHA의 추출 및 정제)

  • JEONG Bo-Young
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.26 no.6
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    • pp.529-537
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    • 1993
  • Several methods were examined for purification of docosahexaenoic acid (DHA, 22:6n-3) from skipjack Euthynnus pelamis orbital tissue oil, a marine by-product, and a modified method for isolation of a high purity DHA was proposed. Skipjack orbital tissue contained $55.4\%$ of total lipid(TL), and DHA accounted for $23.7\%$ of the TL. Application of low-temperature crystallization and urea inclusion compound methods to the orbital fatty acid mixture resulted in increases of DHA concentrations to approximately $46\%\;and\;61\%$, respectively. These methods were suitable for large production of DHA with relative low purity because of the simple purification procedure. DHA of approximately $74\%$ in purity was obtained by silver nitrate aqueous solution method, but the method gave a very low recovery($<10\%$). Silver nitrate-impregnated silica column chromatography was suitable for purification of a high purity DHA(purity, $>98\%$ and recovery, $>90\%$) A modified method, silver nitrate-impregnated silica column chromatography combined with low-temperature crystallization(two step purication method) was proposed as the most effective method to obtain DHA with high purity($99.9\%$) from the skipjack orbital oil.

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Separation and Adsorption-Desorption Characteristics of Heavy Rare Earth Elements (Gd, Tb, Dy) using P507 Resin (P507 추출수지를 이용한 중희토류 원소(Gd, Tb, Dy)의 흡탈착 분리특성에 관한 연구)

  • Lee, Sungeun;Kim, Joung Woon;Jeon, Jong Hyuk;Jun, Hong Myeong;Lee, Jin Young;Han, Choon
    • Resources Recycling
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    • v.25 no.4
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    • pp.60-67
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    • 2016
  • This study was conducted to establish the adsorption-desorption mechanism and the optimum condition of chromatographic operation for separations of heavy rare earth elements (Gd, Tb, Dy) using a p507-containing resin. By employing Langmuir and Freundlich isotherm together with pseudo first and second order kinetics, absorption-desorption reaction mechanism was investigated. Langmuir and Freundlich isotherm was applied under assumption that adsorption reaction occurs in form of monolayer, and because the result was identical to the assumption, now we know adsorption of heavy rare earth elements occurs in form of monolayer. Concerning the pseudo first and second order kinetic, the pseudo second order seemed to be more suitable to represent heavy rare earth element adsorption mechanism. By using the extraction chromatography to separate heavy rare earth elements, ${\alpha}^{Tb}_{Gd}=1.24$, and ${\alpha}^{Dy}_{Tb}=1.03$ were confirmed in eluent HCl 0.25 M which indicates almost perfect separations of three elements. Furthermore, as concentrations of eluent became higher, the resolution value decreased and the elution area got shortened.