• Title/Summary/Keyword: liquid column separation

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Achiral and Chiral Determination of Benzophenanthridine Alkaloids from Methanol Extracts of Hylomecon Species by High Performance Liquid Chromatography

  • Kang, Jong-Seong;Long, Pham-Hoai;Lim, Hwan-Mi;Kim, Young-Ho;Gottfried-Blaschke
    • Archives of Pharmacal Research
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    • v.26 no.2
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    • pp.114-119
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    • 2003
  • A high performance liquid chromatographic (HPLC) method was developed for the qualitative and quantitative determination of benzophenanthridine alkaloids from the methanol extracts of Hylomecon hylomeconoides and H. vernale (Papaveraceae). Achiral and chiral methods were adapted for the separation of 6-methoxydihydrosanguinarine (1), 6-acetonyldihydrosanguinarine (2) and dihydrosanguinarine (3). The achiral reversed phase HPLC method made it possible the simultaneous separation and determination of 1, 2 and 3 within 20 min on ODS column using acetonitrile-phosphate buffer (50 mM, pH 7.0) (50 : 50, v/v). The separation and determination of 1 and 2 enantiomers was available using chiral columns. The same amount of (+) and (-)-enantiomers of 1 was found from the methanol extract of specimen, indicated that 1 could be the artifact produced by the reaction of sanguinarine with methanol. H. hylomeconoides showed higher level of 1 and 3 in compared with H. vernale, especially in root samples permitting the possibility of chemical discrimination between two species.

High-Performance Liquid Chromatographic Analysis of Chrysin Derivatives on A $Nova-Pak^{\circledR}C_{18}$ Column

  • Kim, Kyoung-Soon;Shin, Joon-Su;Park, You-Mie;Lee, Sanghyun;Kim, Yang-Bae;Kim, Bak-Kwang
    • Archives of Pharmacal Research
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    • v.25 no.5
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    • pp.613-616
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    • 2002
  • A high-performance liquid chromatographic method has been developed for the separation and quantification of chrysin and synthetic chrysin derivatives (12 chrysin alkyl and 7 chrysin acyl derivatives). The chromatography was performed using a $Nova-Pak^{\circledR}C_{18}$ column. A RP-HPLC was performed by using a binary mixture (MeOH-10 mM H$_3$PO$_4$) as a mobile phase, and the column temperature was maintained at room temperature. A flow rate was 1.0 ml/min, and the effluent was monitored at a wavelenth of 280 nm. The retention times for chrysin acyl and alkyl derivatives were within 10 minutes and 20 minutes, respectively. The absolute recovery of samples were all over 96%. The detection limits were 0.1~18 ng at S/N = 3 ratio.

Determination of Nebramycin Factor 2,4,5,5',6 and Kanamycin A in Fermentation Broth of Streptoalloteichus hindustanus ATCC 31218 Mutant Using 2,4-Dinitrofluorobenzene(DNFB) as a Derivatizing Agent by High Performance Liquid Chromatography (HPLC법에 의한 2,4-디니트로플루오로벤젠을 유도체화제로 한 Streptoalloteichus hindustanus ATCC 31218 변이균의 배양액 중 네브라마이신 펙터 2,4,5,5',6, 가나마이신 A 분석)

  • 박영근;박명용;김승철;양호길
    • YAKHAK HOEJI
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    • v.37 no.1
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    • pp.1-8
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    • 1993
  • A procedure for the high-performance liquid chromatographic determination of Nebramycin factors in fermentation broth of Streptoalloteichus hindustanus ATCC 31218 mutant was investigated using pre-column derivatization and LTV detection. The method is based on pre-column derivatization of Nebramycin factors with 2,4-dinitrofluorobenzene(DNFB) in the presence of Tris (hydroxymethyl)aminoethane. The chromatographic separation of derivatives of Nebramycin factors and unknown impurities is achieved using reversed-phase column (NOVA-PAK $C_{18}$, Waters Co.) and AcCN : H$_{2}$O : AcOH (53.0:46.5:0.5) as a mobile phase. The mixture of these derivatives were separated within 35 minutes and the optimum wavelength($\lambda_{max}$ ) of the UV detector was 353 nm. The linearity of response for derivatives of Nebramycin factors is demonstrated for concentrations up to 500 $\mu\textrm{g}$/ml and the relative standard deviation is less than 0.79%. Detection limit was 1.67 ng for the 10 $\mu\textrm{l}$ sample volume employed.

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Reversed-Phase High Performance and Liquid Chromatographic Separation of the Enantiomers of Terbutaline by Derivatization with 2,3,4-Tetra-o-acetyl-\beta-glucopyranosyl Isothiocyanate

  • Kim, Kyeong-Ho;Kim, Dong-Sig;Hong, Seon-Pyo;Keon, Oh-Seung
    • Archives of Pharmacal Research
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    • v.23 no.1
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    • pp.26-30
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    • 2000
  • The enantiomers of the bronchodilator terbutaline were separated by reversed-phase high performance liquid chromatograhy after derivatization with 2,3,4,6-tetra-O-acetyl-\beta-D-glucopyranosyl isothiocyanate(GITC) reagent. The derivatization proceeded quantitatively within 1 h at room temperature. The corresponding diastereomeric thiourea derivatives were well resolved on an ODS column with acetonitrile-acetate buffer as a mobile phase. Elution orders of the diastereomers were confirmed by derivatization of R-(-)-terbutaline and S-(+)-terbutaline which were collected by semi-preparative chiral HPLC using Sumichiral OA-4700 column. The native fluorescence of terbutaline was quenched by derivatization with GITC. The detection limit was 25ng when monitored at UV 278 nm.

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Continuous Separation of Lysozyme from Egg White by Ion Exchange Column Chromatography (이온교환 칼럼 크로마토그래피를 이용한 난백에서 Lysozyme의 연속추출)

  • Park, Seong-Joon;Kim, Hyeon-Seok;Kim, Hyean-Wee;Ahn, Tae-Hoe;Park, Ki-Moon;Choi, Chun-Un
    • Korean Journal of Food Science and Technology
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    • v.22 no.6
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    • pp.711-715
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    • 1990
  • Continuous column chromatographic separation of lysozyme from egg white was investigated. A weak acid type cation exchange resin, Duolite C-464, was used because of high lysozyme recovery and ease of column operation in this experiment. The resin was equilibrated at $pH\;7.9{\pm}0.1$ in Na+form. Continuous lysozyme separation was processed by repeating cycles(one cycle : resin equilibration, flow egg white, rinse, lysozyme elution) in automated preparative Liquid Chromatography(LC) system(column size ; i.d. 50 mm, resin bed volumn ; 1020 ml). At comparison of UV levels in rinse end point and elution end point of every cycle, the UV levels of rinse end point are maintained below 30% for 19 cycles and that of elution end point are also maintained below 30% for 17 cycles, stably, but was increased above 50% after 18 cycle. That indicated the eluting ability of lysozyme was reduced conspicuously after 18 cycle in continuous cycling process. The recovery of lysozyme was maintained above 90% from one to 17 cycle, but was decreased to 72% and 65% in 18 cycle and 19 cycle, respectively.

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A Study on the Development for a Cryogenic Air Separation Unit (심랭식 공기분리장치 개발 연구)

  • 문흥만
    • Proceedings of the Korea Institute of Applied Superconductivity and Cryogenics Conference
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    • 2001.02a
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    • pp.132-135
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    • 2001
  • Cryogenic air separation unit(ASU) was developed about 100 year ago in Europe. However, because there is not any ability of process design or manufacturing of ASU in Korea, many ASUs come from advanced countries every year. The purpose of this study is the development of cryogenic air separation unit by our own ability, especially cold box for nitrogen production. On this study, we developed the computer program for physical properties of gases and process simulation. We also did process design and manufactured of cold box, including air separation column, liquid air heat exchanger and condenser. The result of cold box test was successful.

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Comparing the Performance of One-column Process and Four-zone Simulated Moving Bed by Computer Simulation

  • Kim Young Sik;Lee Chong Ho;Wankat Phillip C.;Koon Yoon Mo
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.9 no.5
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    • pp.362-368
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    • 2004
  • A new one-column chromatography process, analogous to a four-zone simulated moving bed (SMB), was presented. The basic principle of the process was identical to that of a four-zone SMB. The process consisted of one chromatographic column and four tanks, instead of the four columns in the four-zone SMB (1-1-1-1), and has been used for the separation of two amino acids, phenylalanine and tryptophan, using an ion exchange resin. The operating parameters for the one-column process and four-zone SMB were obtained from equilibrium theory. Computer simulations were used to compare the performances of the new one column process to that of the general four-zone SMB, using Aspen $Chromatography^{TM}$ v 11.1. The differences between the one-column and SMB processes in terms of the purities and yields of phenylalanine and tryptophan were less than 4 and about $6\%$, respectively. The lower purities of the one-column process were due to the loss of the developed concentration profiles in the column when the liquid was stored in tanks. The one-column process gave great flexibility, and would be useful for reconstructing an existing conventional chromatography process to one of a SMB.

On the Pyrolysis of Polymers II. Identification of the Products from Polymer Pyrolysis by Gas Chromatography (高分子物質의 熱分解에 關한 硏究 (第2報) Gas Chromatography 에 依한 熱分解生成物의 檢索)

  • Chwa-Kyung Sung
    • Journal of the Korean Chemical Society
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    • v.7 no.2
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    • pp.106-114
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    • 1963
  • The products from polymer pyrolysis at $450^{\circ}$ are cooled with ice, then liquid and gaseous portions are analysed by gas chromatography. Di-2-ethyl hexyl sebacate column, silicone oil column, silica gel column and tetraethyleneglycol dimethylether column, which was most effective for the separation of hydrocarbon gases, are used. Identification of isomers could be secured more effectively by gas chromatography than mass spectrometry. Elucidation of the mechanism for thermal decomposition of polymers could be done through the identification of pyrolysis products. Although more extensive work is needed, some patterns of polymer pyrolysis are discussed.

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Comparison of Axial and Radial Flow Chromatography on Protein Separation Speed and Resolution (축방향과 반경방향흐름 크로마토그래피의 단백질 분리속도와 분리능에 대한 비교)

  • 김윤하;이은규
    • KSBB Journal
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    • v.10 no.5
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    • pp.482-490
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    • 1995
  • The relationship between pressure drop and liquid flow rate, for an axial and a radial flow chromatographic column packed with compressible porous media was theoretically analyzed using modified Kozeny-Carman equation. The results were compared with experimental observations obtained using compressible DEAE-agarose as a model medium. At 2-9 psi range studied, the theoretical derivation accounting for 'gel compression' effect predicted simple Langmuirian type response of volumetric flow rate to changes in pressure drop. On the other hand, the experimental response was more or less sigmoidal. At the same pressure drop, radial column showed 2-3 times higher flow rates than those of axial column both theoretically and experimentally. Using r-HBsAg crude extract, protein resolution effects between the two types of columns at different flow rates were compared side-by-side. It turned out that, though general chromatographic behavior was very similar, axial column was somewhat superior in terms of r-HBsAg recovery yield and specificity. However, the number of theoretical plates analysis indicated the protein resolution effects were comparable.

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$SO_2/O_2$ Separation Process with EMIm[$EtSO_4$] in SI Cycle for the Hydrogen Production by Water Splitting (물분해 수소제조를 위한 SI cycle에서의 EMIm[$EtSO_4$]를 이용한 $SO_2/O_2$ 분리공정)

  • Lee, Ki-Yong;Kim, Hong-Gon;Jung, Kwang-Deog;Kim, Chang-Soo
    • Journal of Hydrogen and New Energy
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    • v.22 no.1
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    • pp.13-20
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    • 2011
  • $SO_2$ has been absorbed and separated selectively by an ionic liquid from $SO_2/O_2$ mixture decomposed from sulfuric acid during the thermochemical SI cycle for the water splitting. In order to design and operate high pressure $SO_2/O_2$ separation system, the solubility of $SO_2$ in [EMIm]$EtSO_4$ (1-ethyl-3-methylimidazolium ethylsulfate) has been measured by Magnetic Suspension Balance at high pressure and temperature. Based on the measured solubility, a pressurized separation system was set up and operated. 194 L/h of $SO_2$($SO_2:O_2$=0.65:1) has been separated with 99.85% of $O_2$ at the vent of absorption tower, which is 22.7% of the theoretically ideal capacity of the system. This discrepancy results from the reduced contact between the gaseous $SO_2$ and the ionic liquid. Increased $SO_2$ supply, scale-up of the absorption column, and a faster ionic liquid circulation speed were suggested to improve the separation capacity.