• Title/Summary/Keyword: Preparative Chromatography

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A Novel Design of Simulated Moving Bed (SMB) Chromatography for Separation of Ketoprofen Enantiomer

  • Yoon, Tae-Ho;Chung, Bong-Hyun;Kim, In-Ho
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.9 no.4
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    • pp.285-291
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    • 2004
  • A simulated moving bed (SMB) chromatography system is a powerful tool for preparative scale separation, which can be applied to the separation of chiral compound. We have de-signed our own lab-scale SMB chromatography using 5 HPLC pumps, 6 stainless steel columns and 4 multi-position valves, to separate a racemic mixture of ketoprofen in to its enantiomers. Our design has the characteristics of the low cost for assembly for the SMB chromatography and easy repair of the unit, which differs from the designs suggested by other investigators. It is possible for the flow path through each column to be independently changed by computer control, using 4 multi-position rotary valves and 5 HPLC solvent delivery pumps. In order to prove the operability of our SMB system, attempts were made to separate the (S)-ketoprofen enantiomer from a ketoprofen racemic mixture. The operating parameters of the SMB chromatography were calculated for ketoprofen separation from a batch chromatography experiment as well as by the triangle theory. With a feed concentration of 1 mg/mL, (S)-ketoprofen was obtained with a purity of 96% under the calculated operating conditions.

Antioxidative Activity and Structural Analysis of the Steroid Compound from Fomitella fraxinea (Fomitella fraxinea 중 Steroid계 화합물의 항산화 활성 및 구조분석)

  • Park, Sang-Shin;Lee, Jong-Seok;Bae, Kang-Gyu;Yu, Kook-Hyun;Han, Hey-Chul;Min, Tae-Jin
    • The Korean Journal of Mycology
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    • v.29 no.1
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    • pp.67-71
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    • 2001
  • A steroid compound, F-l with antioxidative activity from the fruit bodies of Fomitella fraxinea was isolated by ethyl acetate extraction, silica gel column chromatography, and preparative silica thin layer chromatography. The structure of the compound was determined to be crgosta-7,22-diene-3-one-$16{\beta}-ol$ by IR, NMR, and GC-Mass. The compound exhibited inhibition on lipid peroxidation of rat liver microsomes, with $IC_{50}$ value of $3.8{\mu}g/ml$.

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Studies on the Constituents of Korean Edible Oils and Fats -Part 3. Studies on the oil soluble constituents of sunflower seed- (한국산(韓國産) 식물식용유지(植物食用油脂)의 성분(成分)에 관(關)한 연구(硏究) -제3보(第3報) 해바라기 종자(種子)의 유성성분(油性成分)에 대하여-)

  • Choi, Kee-Young;Ko, Young-Su
    • Journal of Nutrition and Health
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    • v.12 no.2
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    • pp.75-85
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    • 1979
  • The Korean origin sunflower (Helianthus Annus Linn.) seed of netural lipid were analysed by thinchrography, High performance liquid chromatography, preparative Thinlayer and Gas liquid chromatography. 1) The seed oil triglyceride components were conveniently separated based on their degree of unsaturation by employing the chromatography on silica gel sintered rod impregnated with 12.5% silver nitrate. Sunflower seed oil was composed of triglyceride, especially trilinolein 57. 74% triolein 25.28%, tripalmitin 7 55% ana tristearin 9.43% by a thinctrography. 2) The fatty acid compositions of seed oil have been determined by a high performance liquid chromatographic analysis using a ALC/GPC 244 type from Waters Association (Japan) with ${\mu}$ Bondapak FFAA column. It contained stearic acid 8.59%, oleic acid 27. 19%, palmitic acid 7.50% and linoleic acid 56.72% respectively. 3) The composition of sterols were determined by a preparative Thinlayer and Gas liquid chromatographic analysis. It was noted that sitosterol was the major sterol in the Korean sunflower seed. The results showed that contents of sterols were cholesterol trace, campesterol $13_.^{22\sim}13.9%$, stigmasterol $13.8{\sim}14.1%$, If, sitosterol $58.4{\sim}60.7%$, ${\vartriangle}^7$-stigmastenol $10.2{\sim}10.5%$ and ${\vartriangle}^{7,24(25)}$-stigmastenol $3.6{\sim}3.8%$ by method of planimetry and triangulation.

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Screening of Antifungal Compounds from Microorganisms with Preferential Activity against the Mycelial Phase of Candida albicans (토양으로부터 Candida albicans 의 균사형태에 선택적인 활성을 나타내는 미생물로부터 항진균 물질의 탐색)

  • Kim, Sung-Uk;Nam, Ji-Youn;Kwon, Byoung-Mok;Son, Kwang-Hee;Bok, Song Hae
    • Microbiology and Biotechnology Letters
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    • v.23 no.2
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    • pp.170-177
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    • 1995
  • To search and develop the compounds exhibiting antifungal activities against the mycelial phase of Candida albicans, approximately 2,900 microorganisms isolated from soil were examined for antifungal activity. Among them, a strain with preferential activity against the mycelial phase of Candida albicans was isolated and identified as Streptomyces sp. A393. Isolation and purification of compounds A393 showing antifungal activity against the mycelial phase of C. albicans were performed using XAD-7 column chromatography, silica gel chromatography, preparative thin- layer silica gel chromatography, and HPLC. The molecular weights of compounds isolated from Streptomyces sp. A393 were determined as 774, 790, 804 and 820. These compounds appeared to have a structure of macrolide antibiotics, oligomycin A, B, C and E. Especially, oligomycin E, which is formerly reported to have no antifungal activity, showed antifungal activity against the mycelial phase of Candida albicans.

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Chiral Separation of Tryptophan Enantiomers by Liquid Chromatography with BSA-Silica Stationary Phase

  • Kim Kwonil;Lee Kisay
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.5 no.1
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    • pp.17-22
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    • 2000
  • The separation of tryptophan enantiomers was carried out with medium-pressure liquid chromatography using BSA (bovine serum albumin)-bonded silica as a chiral stationary phase. The influence of various experimental factors such as pH and ionic strength of mobile phase, separation temperature, and the presence of organic additives on the resolution was studied. In order to expand this system to preparative scale, the loadability of sample and the stability of stationary phase for repeated use were also examined. The separation of tryptophan enantiomers was successful with this system. The data indicated that a higher separation factor (a) was obtained at a higher pH and lower temperature and ionic strength in mobile phase. Addition of organic additives (acetonitrile and 2-propanol) in mobile phase contributed to reduce the retention time of L-tryptophan. About $30\%$ of the separation factor was reduced after 80 days of repeated use.

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Physico-chemical and Antagonistic Properties of Antibiotics Produced by Actinomycetes Isolate G-37 (방선균 분리주 G-37이 생산하는 항생물질의 물리.화학적 특성과 항균활성)

  • 여운형;김영호;채순용;박은경
    • Journal of the Korean Society of Tobacco Science
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    • v.17 no.2
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    • pp.103-108
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    • 1995
  • Antibiotic and physico-chemical properties of an active compound from actinomycetes isolate G-37, of which the culture filtrate had an inhibitory effect against tobacco mosaic virus(W) infection, were examined. The active compound, which was purified by ethylacetate extraction, silica gel column chromatography, preparative thin layer chromatography, and high performance liquid chromatography, showed strong antibacterial activities especially against Gram-positive bacteria including Bacillus subtillis, Sarcina lutea and Staphylococcus aureus. From the IH-NMR, FAB/RfS, UV spectral data, and physicochemical properties, the active compound of G-37 appears to belong to a peptide antibiotic group. Among the known peptide antibiotics in the antibiotic group, No. 280, A-30912, and Taitomycin showed molecular weights and ultra violet spectrum similar to those of the active compound from G-37, but was not identical to the compound, which suggests that it may be a new peptide antibiotics.

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Analysis of Angiotensin I Converting Enzyme Inhibitory Activity of Oligosacchride Extracted from Capsosiphon fulvescens (매생이 유래 올리고당의 추출 분리 및 Angiotensin I Converting Enzyme 저해능 분석)

  • Kim, Hyun-Woo;Lee, Jung-Heon
    • KSBB Journal
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    • v.28 no.2
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    • pp.131-136
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    • 2013
  • The hydrolysates prepared with various enzyme digestion of Capsosiphon fulvescens were used to measure the inhibitory effects against angiotensin I converting enzyme (ACE). The commercially available enzymes such as Celluclast, Viscozyme, Lysing enzyme, Flavourzyme, Alcalase and Pectinex were used to digest C. fulvescens and produce hydrolysates. The maximum ACE inhibitory activity was observed using Alcalase hydrolysis (72.9%). The optimal conditions of Alcalase extraction were pH 8.0 and extraction time for 12 hr. The hydrolysates were fractionated using preparative-LC and anion-exchange chromatography on DEAE-cellulose and the fraction B and B-2 were isolated. The ACE inhibitory activity of fraction B-2 by anion-exchange chromatography was 82.6%. The molecular weight of fraction B-2 estimated using size exclusion chromatography was about 1 kDa. The monosaccharide composition of the fraction B-2 was determined to be mannose (1.1%), glucuronic acid (1.3%), galactose (1.3%) and glucose (96.3%).

Studies on the Sterol Components of Torreya Nut of Korea (한국산 비자중의 스테롤 성분에 관한 연구)

  • 정보섭;고영수
    • YAKHAK HOEJI
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    • v.22 no.2
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    • pp.87-90
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    • 1978
  • "Bija"(Torreya nut), a tree belonging to the Torreyaceae family, is cultivated in Jae Joo Do and Jun Ra Do, Korea. The seed of Torreya nucifera, which has been widely used as folkmedicine in the treatment of tapeworm infestation, was examined on the sterol composition determined by gas liquid chromatography and thin layer chromatography on the preparative plates. Sterols were obtained from the nonsaponifiable matters of ether extract of the seed. It was noted that .betha.-sitosterol was the major sterol in the nut. The results showed that contents of sterols were campesterol 3.15-3.75%, stigmasterol 5.38-5.67%, $\beta$-sitosterol 85.61-86.28% and ${\delta}^{7}$-sterol 4.91-5.19% by gas liquid chromatography.

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Isolation and Identification of Free Phenolic Acids in Korean Ginseng (인삼의 유리 페놀성 분획중 phenolic acid의 순수분리 동정)

  • Kim, Man-Wook;Wee, Jae-Joon;Park, Jong-Dae
    • Korean Journal of Food Science and Technology
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    • v.19 no.5
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    • pp.392-396
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    • 1987
  • A method for isolation of some phenolic acids from Korean ginseng(Panax ginseng C.A.Meyer)was studied using silicic acid column chromatography. preparative thin layer chromatography and high performance liquid chromatography. Two phenolic compounds were isolated and identified as ferulic acid, mp $156-157^{\circ}C$ and vanillic acid. mp $154-156^{\circ}C$ by spectral data of Mass and NMR spectroscopy.

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Studies on the Anthocyanin Pigments in Fruits of Panax Species - Part I. Identfication of major Pigment - (Panax속(屬)의 과피(果皮) Anthocyanin 색소(色素) - 제1보(第一報). 주색소(主色素)의 동정(同定) -)

  • Parklee, Qwi-Hee;Park, Hoon
    • Applied Biological Chemistry
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    • v.23 no.4
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    • pp.242-245
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    • 1980
  • The anthocyanin pigments in the fruit skin of Panax ginseng and Panax quinquefolius were extracted with 1% HCl/propanol. The pigments were purified by preparative thin layer and paper chromatography. The major bands in the 2 varieties were identified as pelragonidin-3-monoglucoside by chromatographic, spectrophotometric and high performance liquid chromatographic methods. The possibility of the anthocyanin acylation was not studied in this report. One of minor red band found in the Panax ginseng (not identified) was missing in the Panax quinquefolius.

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