• Title/Summary/Keyword: Preparative separation

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Preparative Chromatographic Separaction: Simulated Moving Bed and Modified Chromatography Methods

  • Yi Xie;Koo, Yoon-Mo;Nien-Hwa Linda Wang
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.6 no.6
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    • pp.363-375
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    • 2001
  • Chromatography has been method of choice for the separation complex biologi-cal mixtures fro analytical purpose, particularly for the last fifty years. Its use has recently been extended to preparative separation where the productivity relative to the amount of resin and sol-vent used is a matter of concern. To overcome the inherent thermodynamic inefficiency of batch chromatography, as exemplified by the partial temporal usage of the resin and dilution of the product with the solvent, chromatography has been continually modified by separation engineers. Column switching and recycling represnet some of the process modifications that have brought high productivity to chromatography. Recently, the simulated moving bed (SMB) method, which claims a high separation efficiency based on counter-current moving bed chromatography. has be-come the mainstay of preparative separation, especially in chiral separation. Accordingly, this pa-per reviews the current status of SMB along with several chromatographic modification, which may be helpful in routine laboratory and industrial chromatographic practices.

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Enantioseparation of Racemic 1,1'Binaphthyl-2,2'diamine by Preparative Liquid Chromatography

  • Ryoo, Jae-Jeong;Kwon, Woo-Jeong;Kim, Tae-Hyuk;Lee, Kwang-Pill;Choi, Seong-Ho
    • Bulletin of the Korean Chemical Society
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    • v.25 no.9
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    • pp.1336-1340
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    • 2004
  • The same kind of chiral stationary phase with a commercialized chiral column was used to make preparative chiral columns and was applied to resolve racemic N-acetyl-1-naphthylethylamide (3) by preparative liquid chromatography. An improved chromatographic condition to resolve racemic 3 on the CSP was examined by changing flow rate and kind of the mobile phase and the sample injection volume. The optimized separation conditions were applied to resolve racemic 1,1'-Binaphthyl-2,2'-diamine(4).

Simulated Moving Bed [SMB] (모사 이동층 크로마토그래피)

  • Lee Chong-Ho;Koo Yoon-Mo
    • KSBB Journal
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    • v.20 no.3
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    • pp.192-196
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    • 2005
  • Chromatography has been a method of choice in the separation of complex biological mixtures for the analytical purpose in particular for the last half of century. In current years, chromatographic method extends its use to the preparative separation where the productivity per resin amount and solvent use become a matter of concern. Recently, simulated moving bed (SMB) method which claims high separation efficiency of the ideal counter-current moving bed chromatography has become a workhorse of preparative separation. SMB technology was developed in the early 1960s for large-scale hydrocarbon separation by UOP and approximately 120 Sorbex units have been licensed to date. Recently, SMB separation technology has been successfully extended from hydrocarbons and sugars to fine chemicals, particularly biochemicals, from laboratory to pilot to production plant. In this paper, the current status of SMB and its modifications were reviewed.

A Newly Developed Analytical and Semi-preparative Enantiomer Separation of Fluoxetine using Polysaccharide-derived Chiral Stationary Phases by High Performance Liquid Chromatography (고성능 액체 크로마토그래피에 의한 다당 유도체의 키랄 고정상에서 플록세틴의 새롭게 개발된 분석 및 반분취의 광학분리)

  • Kim, Seok Jin;Nam, Kyung Wook;Park, Bohyun;Islam, Md. Fokhrul;Lee, Wonjae
    • KSBB Journal
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    • v.31 no.3
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    • pp.186-191
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    • 2016
  • A liquid chromatographic method for the enantiomer separation of fluoxetine was performed using covalently bonded and coated type polysaccharide-derived chiral stationary phases (CSPs). The degree of enantioseparation is affected by the used CSPs and mobile phases. The performance of Chiralpak IC was superior to the other CSPs used in this study. Out of various solvent composition and additives, the greatest separation and resolution was observed using Chiralpak IC with mobile phase of 2-propanol in hexane with diethylamine as an additive. Semi-preparative separation of fluoxetine was performed on the analytical Chiralpak IC column to obtain (R)- and (S)-fluoxetine enantiomer with high chemical and optical purity. From the overall study, the developed liquid chromatographic method on polysaccharide-derived CSPs is expected to be very useful for the enantiomer separation of fluoxetine.

Preparative separation of minor saponins from Panax notoginseng leaves using biotransformation, macroporous resins, and preparative high-performance liquid chromatography

  • Liu, Fang;Ma, Ni;Xia, Fang-Bo;Li, Peng;He, Chengwei;Wu, Zhenqiang;Wan, Jian-Bo
    • Journal of Ginseng Research
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    • v.43 no.1
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    • pp.105-115
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    • 2019
  • Background: Ginsenosides with less sugar moieties may exhibit the better adsorptive capacity and more pharmacological activities. Methods: An efficient method for the separation of four minor saponins, including gypenoside XVII, notoginsenoside Fe, ginsenoside Rd2, and notoginsenoside Fd, from Panax notoginseng leaves (PNL) was established using biotransformation, macroporous resins, and subsequent preparative high-performance liquid chromatography. Results: The dried PNL powder was immersed in the distilled water at $50^{\circ}C$ for 30 min for converting the major saponins, ginsenosides Rb1, Rc, Rb2, and Rb3, to minor saponins, gypenoside XVII, notoginsenoside Fe, ginsenoside Rd2, and notoginsenoside Fd, respectively, by the enzymes present in PNL. The adsorption characteristics of these minor saponins on five types of macroporous resins, D-101, DA-201, DM-301, X-5, and S-8, were evaluated and compared. Among them, D-101 was selected due to the best adsorption and desorption properties. Under the optimized conditions, the fraction containing the four target saponins was separated by D-101 resin. Subsequently, the target minor saponins were individually separated and purified by preparative high-performance liquid chromatography with a reversed-phase column. Conclusion: Our study provides a simple and efficient method for the preparation of these four minor saponins from PNL, which will be potential for industrial applications.

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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Separation and Characterization of Dust and Ground Water Particulates Using Gravitational SPLITT Fractionation.

  • Lee, Seung Ho;Park, Hui Yeong;Lee, Sang Geun;Yong, Seong Gwon;Eum, Cheol Hun
    • Bulletin of the Korean Chemical Society
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    • v.22 no.6
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    • pp.616-622
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    • 2001
  • Split-flow thin (SPLITT) cell Fractionation(SF) is a technique that allows separation of particulates and macromolecules into two fractions. A gravitational SF(GSF) system is constructed and tested for its applicability for separation of dust and ground water particulates. When tested with polystyrene latex particles, experimental data were in good agreements with theory. The 9.8 and 21.4㎛ polystyrene particles were successuflly separated in a continuous mode, where the mixture is continuously fed into the GSF channel allowing separation in a large sacle. The GSF system is successfully applied to continuous separation of dust and ground water particels based on the sedimentation coefficient, which is closely related to the particle size. The separations were confirmed by microscopy and energy-dispersive X-ray (EDX) analysos.