• Title/Summary/Keyword: Preparative liquid chromatography

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Isolation of ginsenosides Rb1, Rb2, Rc Rd, Re, Rf and Rg1 from cinseng root by high performance liquid chromatography

  • Paik, Nam-Ho;Park, Man-Ki;Choi, Kang-Ju;Cho, Yung-Hyun
    • Archives of Pharmacal Research
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    • v.5 no.1
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    • pp.7-12
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    • 1982
  • Ginsenosides Rb1, Rb2, Rc, Rd, Re, Rf and Rg1 were effectively isolated from ginseng root by preparative liquid chromatography (LC) on two PrepPAK-500/c18 cartridges in series and semipreparative LC on a .mu. Bondapak cabohydrate analysis column, a .mu.Bondapak C18 column or a .mu. Porasil column. The identities of the isolated ginsenosides were confirmed by analytical high-performance liquid chromatography (HPLC) and infrared spectrophotometry. By this method large scale isolation of pure ginsenosides was efficiently accomplished.

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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).

New Polyacetylene Compounds from Panax Ginseng C. A. Meyer$^\dag$

  • Shim, Sang-Chul;Chang, Suk-Ku;Hur, Chan-Woo;Kim, Chang-Kew
    • Bulletin of the Korean Chemical Society
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    • v.8 no.4
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    • pp.272-275
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    • 1987
  • Two polyacetylene compounds having diyn-ene chromophore were isolated from fresh Korean ginseng roots through solvent fractionation, partition and silica gel column chromatography. The low pressure semi-preparative liquid chromatography and high performance preparative liquid chromatography were used for final separation of polyacetylenic fractions. The chemical structures of these polyacetylenes were determined to be heptadeca-1,8-dien-4,6-diyn-3,10-diol and heptadeca-1,4-dien-6,8-diyn-3,10-diol by UV, FT-IR, $^1H\;NMR,\;^{13}C\;NMR,$ mass spectra and elemental analysis.

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.

Larqe guantity isolation of Ginsenoside $-Rb_1,\;-Rb_2,\;-Rc,\;-Rd,\;-Re\;and\;-Rg_1$ in Panax ginseng C.A. Meyer by High Performance Liquid Chromatography (고속액체(高速液體) chromatography에 의(依)한 Ginsenoside $-Rb_1,\;-Rb_2,\;-Rc,\;-Rd,\;-Re$$-Rg_1$의 대량분리(大量分離))

  • Choi, Jin-Ho;Kim, Woo-Jung;Bae, Hyo-Won;Oh, Sung-Ki;Oura, Hikokichi
    • Applied Biological Chemistry
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    • v.23 no.4
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    • pp.199-205
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    • 1980
  • Relatively large quantity of the major components of saponin, $ginsenoside-Rb_1,\;-Rb_2,\;-Rc,\;-Rd,\;-Re\;and\;-Rg_1$ from Panax ginseng C.A. Meyer were isolated using preparative and semipreparative high performance liquid chromatography, and analyzed by analytical HPLC. The application of HPLC for isolation of ginsenosides was not only very effective for rapid analysis but also reduced the isolation time. The isolation capacity of pure ginsenosides was $30{\sim}50mg/hr$.

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Transformation of dissolved organic matter in a constructed wetland: A molecular-level composition analysis using pyrolysis-gas chromatography mass spectrometry

  • Park, Jongkwan;Choi, Mijin;Cho, Jaeweon;Chon, Kyongmi
    • Environmental Engineering Research
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    • v.23 no.4
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    • pp.390-396
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    • 2018
  • This study investigated the transformation of dissolved organic matter (DOM) in a free-water surface flow constructed wetland. Pyrolysis gas chromatography-mass spectrometry (Py-GC/MS) coupled with preparative high-performance liquid chromatography (prep-HPLC) was used to analyze the compositions of biopolymers (polysaccharides, amino sugars, proteins, polyhydroxy aromatics, lipids and lignin) in DOM according to the molecular size at three sampling points of the water flow: inflow, midflow, and outflow. The prep-HPLC results verified the decomposition of DOM through the decrease in the number of peaks from three to one in the chromatograms of the sampling points. The Py-GC/MS results for the degradable peaks indicated that biopolymers relating to polysaccharides and proteins gradually biodegraded with the water flow. On the other hand, the recalcitrant organic fraction (the remaining peak) in the outflow showed a relatively high concentration of aromatic compounds. Therefore, the ecological processes in the constructed wetland caused DOM to become more aromatic and homogeneous. This indicated that the constructed wetland can be an effective buffer area for releasing biochemically stable DOM, which has less influence on biological water quality indicators, e.g., biochemical oxygen demand, into an aquatic ecosystem.

Identification of Dammarane-type Triterpenoid Saponins from the Root of Panax ginseng

  • Lee, Dong Gu;Lee, Jaemin;Yang, Sanghoon;Kim, Kyung-Tack;Lee, Sanghyun
    • Natural Product Sciences
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    • v.21 no.2
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    • pp.111-121
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    • 2015
  • The root of Panax ginseng, is a Korea traditional medicine, which is used in both raw and processed forms due to their different pharmacological activities. As part of a continued chemical investigation of ginseng, the focus of this research is on the isolation and identification of compounds from Panax ginseng root by open column chromatography, medium pressure liquid chromatography, semi-preparative-high performance liquid chromatography, Fast atom bombardment mass spectrometric, and nuclear magnetic resonance. Dammarane-type triterpenoid saponins were isolated from Panax ginseng root by open column chromatography, medium pressure liquid chromatography, and semi-preparative-high performance liquid chromatography. Their structures were identified as protopanaxadiol ginsenosides [gypenoside-V (1), ginsenosides-Rb1 (2), -Rb2 (3), -Rb3 (4), -Rc (5), and -Rd (6)], protopanaxatriol ginsenosides [20(S)-notoginsenoside-R2 (7), notoginsenoside-Rt (8), 20(S)-O-glucoginsenoside-Rf (9), 6-O-[$\alpha$-L-rhamnopyranosyl(1$\rightarrow$2-$\beta$-D-glucopyranosyl]-20-O-$\beta$-D-glucopyranosyl-$3\beta$,$12\beta$, 20(S)-dihydroxy-dammar-25-en-24-one (10), majoroside-F6 (11), pseudoginsenoside-Rt3 (12), ginsenosides-Re (13), -Re5 (14), -Rf (15), -Rg1 (16), -Rg2 (17), and -Rh1 (18), and vinaginsenoside-R15 (19)], and oleanene ginsenosides [calenduloside-B (20) and ginsenoside-Ro (21)] through the interpretation of spectroscopic analysis. The configuration of the sugar linkages in each saponin was established on the basic of chemical and spectroscopic data. Among them, compounds 1, 8, 10, 11, 12, 19, and 20 were isolated for the first time from P. ginseng root.

Efficient Isolation of Dihydrophaseic acid 3'-O-β-D-Glucopyranoside from Nelumbo nucifera Seeds Using High-performance Countercurrent Chromatography and Reverse-phased High-performance Liquid Chromatography

  • Rho, Taewoong;Yoon, Kee Dong
    • Natural Product Sciences
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    • v.24 no.4
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    • pp.288-292
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    • 2018
  • High-performance countercurrent chromatography (HPCCC) coupled with reversed-phase highperformance liquid chromatography (RP-HPLC) method was developed to isolate dihydrophaseic acid 3'-O-${\beta}$-D-glucopyranoside (DHPAG) from the extract of Nelumbo nucifera seeds. Enriched DHPAG sample (2.3 g) was separated by HPCCC using ethyl acetate/n-butanol/water system (6:4:10, v/v/v, normal-phase mode, flow rate: 4.0 mL/min) to give 23.1 mg of DHPAG with purity of 88.7%. Further preparative RP-HPLC experiment gave pure DHPAG (16.3 mg, purity > 98%). The current study demonstrates that utilization of CCC method maximizes the isolation efficiency compared with that of solid-based conventional column chromatography.

Use of HCI Program for Optimization of Operating Conditions in Analytical and Preparative Chromatography (분석 및 분리용 크로마토그래피에서 조업조건의 최적화를 위한 HCI 프로그램의 이용)

  • Lee, Ju-Won;Lee, Min-U;No, Gyeong-Ho
    • KSBB Journal
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    • v.14 no.4
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    • pp.408-413
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    • 1999
  • To separate mixtures analytically and preparatively by LC (Liquid Chormatography), the operating conditions of analytical chromatography should be determined. The HCI program was utilized to find the optimum operating condition accurately and rapidly, and to reduce the number of experiments. In an analytical chromatography, based on the resolution and analysis time, the experimental conditons of deoxyribonucleosides and phopholipids were fixed in terms of taxol was calculated, and the collection time was predicted for the mixture of 5'-IMP and 5'-GMP from the elution profile when and purity wer known.

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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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