• Title/Summary/Keyword: 추출 크로마토그래피

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Purification and Characterization of Homoharringtonine from Cephalotaxus koreana

  • Kim, Byung-Sik;Kim, Jin-Hyun
    • 한국생물공학회:학술대회논문집
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    • 2005.04a
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    • pp.351-354
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    • 2005
  • A new isolation and purification method was developed aiming at increasing yield and purity for homoharringtonine. This method was a simple andefficient procedures, for the isolation and purification of homoharringtonine from Cephalotaxus koreana, consisting of solvent extraction, adsorbent treatment, low-pressure chromatography, and high performance liquid chromatography (HPLC). The crude homoharringtonine was efficiently pre-purified adequately to perform HPLC through a combination withadsorbent treatment and low-pressure chromatogaphy. The homoharringtonine can be simply obtained with high purity and yield from crude homoharringtonine by HPLC. Purified homoharringtonine was characterized.

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세포능식촉진인자(MPF)의 특이적 억제제 생산 토양균주의 검색 및 억제제의 분리와 특성 규명에 관한 연구

  • 박희동;박상곤;이승기
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1994.04a
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    • pp.258-258
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    • 1994
  • 본 연구에서는 토양균이 생성하는 2차 대사산물로부터 세포증식 촉진인자 (Maturation Promoting Factor. MPF)인 cdc2/cdk2-cyclin의 복합체를 특이적으로 억제하는 물질을 분리하고 그 물질의 생리활성을 조사하였다. 토양으로부터 순수분리된 300여개의 토양균에서 생성된 배양액을 취하여 MPF의 특이적인 기질인 합성 peptide (CSH103 :HATPPKKKRK)를 사용하여 인산화 활성을 측정하였다. 그중 MPF 활성 억제능이 90% 이상인 19개의 균주를 1차적으로 선정한 후 각각에 대하여 열/pH에 대한 안정성, 각종 용매에 대한 추출성 등 이화학적 성질을 규명하였으며 이중 균주 LPL 931로부터 MPF 활성 억제제를 분리하고자 하였다. 예비실험의 결과로부터 토양균 LPL 931을 대량배양하여 열처리하고, 비이온성 수지인Amberlite XAD-2에 결합시키고 70% acetone으로 용출시켰다. 이 추출물로부터 ethylacetate와 n-butanol을 사용하여 MPF 억제 활성물질을 추출하였다. 이 추출액을 실리카겔 관 크로마토그래피, 분취 TLC, 분취 HPL를 하여 MPF 활성 억제 분획을 분리하였다.

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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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Procyanidins from Lindera obtusiloba Bark (생강나무 수피의 Procyanidins)

  • Lee, Sang-Keug;Park, Wan-Geun;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
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    • v.25 no.2
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    • pp.110-116
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    • 1997
  • 생강나무의 수피를 아세톤-물 (7:3)의 혼합용액으로 추출하여 에틸아세테이트용성과 수용성 화합물로 분리하였고 이중에서 에틸아세테이트용성 부분을 Sephadex LH-20과 TSK 40F로 충진한 칼럼크로마토그래피를 사용하여 5개의 화합물, 즉 (+)-catechin, (-)-epicatechin, quercetin 그리고 epicatechin-($4{\beta}{\rightarrow}6$-catechin 이량체와 epicatechin-($2{\beta}{\rightarrow}7$, $4{\beta}{\rightarrow}8$)-epicatechin 이량체를 단리 하였다. 단일물의 확인을 위하여 박층크로마토그래피를 실시하였으며, 화합물의 정확한 구조는 $^1H$-NMR과 $^{13}C$-NMR 스펙트럼을 이용하여 규명하였다.

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Antibacterial Activities of Galla Rhois Extracts against Fish Pathogenic Bacteria (오배자 추출물의 어병 세균에 대한 항균 효능)

  • Choi, Hye-Sung;Kim, Jin-Sook;Jang, Dae-Sik;Yu, Young-Beob;Kim, Yi-Cheong;Lee, Joo-Seok
    • Journal of fish pathology
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    • v.18 no.3
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    • pp.239-245
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    • 2005
  • Galla Rhois was extracted with various solvents such as ethyl alcohol, ethyl acetate, n-hexane, and n-butyl alcohol, and antibacterial activity of the extracts were also tested. The ethyl acetate extracted Galla Rhois showed high antibacterial activities and was the most effective extract, was further fractionated into 8 subfractions with silica gel column chromatography. The subfractions 4 and 5 exhibited an excellent antibacterial activity against Streptococcus iniac KCTC3657.

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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Simultaneous determination of aromatic material causing allergic in children's products by Gas Chromatography (어린이 제품 중 가스 크로마토그래피를 이용한 알러지 유발 방향성 물질의 동시분석법)

  • Ko, Kyeong Mok;Rhu, Chan Joo;Kim, Jong Won;Lee, Seok Ki
    • Analytical Science and Technology
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    • v.31 no.1
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    • pp.23-30
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    • 2018
  • Twenty-two allergy-induced aromatics in children were analyzed using a gas chromatography flame ionization detector (GC-FID) and gas chromatography mass spectrometer (GC-MSD). Analytes were extracted using an automatic Soxhlet extractor and centrifuged for 10 min in a fast freezing centrifuge, and the supernatant was transferred into a 2 mL vial and injected in split mode. Under the established conditions, the calibration curve showed linearity with a correlation coefficient of 0.996 or more. A wide range of sensitivity of 6.7 to 1,859,839 depending on the device characteristics and detector used was shown. The detection limit of the device was 0.0032 to $0.0335{\mu}g/mL$, and the maximum detection limit was less than $0.1{\mu}g/mL$. The detection limit of the method ranged from 0.0033 to $0.1161{\mu}g/mL$. In addition, the limit of quantification ranged from 0.0100 to $0.5422{\mu}g/mL$, with a level of precision ranging from 0.21 % to 4.89 % and a degree of accuracy ranging from 89 % to 111 %. The analytical method developed in this study was applied to commercial products.

Determination of Iodide in spent PWR fuels (경수로 사용 후 핵연료 내 요오드 정량)

  • Choi, Ke Chon;Lee, Chang Heon;Kim, Won Ho
    • Analytical Science and Technology
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    • v.16 no.2
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    • pp.110-116
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    • 2003
  • A study has been done on the separation of iodide from spent pressurized water reactor (PWR) fuels and its quantitative determination using ion chromatography. Spent PWR fuels were dissolved with mixed acid of nitric and hydrochloric acids (80 : 20 molL%) which can oxidize iodide to iodate to prevent it from be vaporized. After reducing ${IO_3}^-$ ­to $I_2$ in 2.5 M $HNO_3$ with $NH_2OH{\cdot}HCl$, Iodine was selectively separated from actinides and all other fission products with carbontetrachloride and back-extracted with 0.1 M $NaHSO_3$. Recovered iodide was determined using the ion chromatograph of which the column was installed in a glove box for the analysis of radioactive materials. In practice, spent PWR fuel with 42,000~44,000 MWd/MtU was analyzed and its quantity was compared to that calculated by burnup code, ORIGEN2. The agreement was achieved with a deviation of -8.3~-0.5% from the ORIGEN 2 data, $324.5{\sim}343.6{\mu}g/g$.

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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Separation of Taxol from Taxanes by NP-HPLC (정상 액체 크로마토그래피를 이용한 taxane으로부터 taxol의 분리)

  • Chang, Kyung Kon;Row, Kyung Ho;Chung, Sung Taik
    • Applied Chemistry for Engineering
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    • v.8 no.2
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    • pp.286-291
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    • 1997
  • Taxol which is recognized as a powerful anticancer reagent was extracted from yew extract and separated by NP-HPLC (Normal-PhaseHigh Performance Liquid Chromatography). The experiments were performed in the isocratic mode with $5{\mu}l$ to $100{\mu}l$ injection volume and 1ml/min mobile phase flow rate. The major mobile phase was hexane and small amounts of ethanol, methanol, 1-propanol and isopropanol were added to change the retention behavior. Prior to a real sample, the artificial mixture of taxol, cephalomannine and 10-deacetyltaxol was tested. They are hard to be separated because of similar chemical structures. The experimental results showed that the proper composition of mobile phase for separating the three components was found 96% hexane and 4% ethanol(vol.%) or 96% hexane, 2% 1-propanol and 2% methanol(vol.%). Compared to the run time of 80 minutes for the binary system, the mixture was separated within 50 minutes with the less amount of mobile phase for the ternary system. Finally, $1{\mu}g$ of taxol was separated from yew tree extracts under the optimum operating conditions.

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