• Title/Summary/Keyword: two-phase partition chromatography

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Isolation and Purification of Berberine in Cortex Phellodendri by Centrifugal Partition Chromatography (Centrifugal Partition Chromatography에 의한 황백으로부터 Berberine의 분리 및 정제)

  • Kim, Jung-Bae;Bang, Byung-Ho
    • The Korean Journal of Food And Nutrition
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    • v.27 no.3
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    • pp.532-537
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    • 2014
  • Cortex Phellodendri (CP) is derived from the dried bark of Phellodendron amurense. It has been widely used as a drug in traditional Korea medicine for treating diarrhea, jaundice, swelling pains in the knees and feet, urinary tract infections, and infections of the body surface. Many analytical methods have been used to study oriental herbal medicines, such as thin-layer chromatography, column liquid chromatography, and high performance liquid chromatography (HPLC). In this study, preparative centrifugal partition chromatography (CPC) was successfully carried out in order to separate pure compounds from a CP methanol extract. The optimum two-phase CPC solvent system was composed of n-butanol: acetic acid: water (4:1:5 v/v/v). The flow rate of the mobile phase was 3 mL/min in ascending mode with rotation at 1,000 rpm. The CPC-separated fraction and purification procedures were carried out by preparatory HPLC. The $^1H$ NMR spectrum revealed that the resonances at ${\delta}$ 4.10 and 4.20 ppm corresponded to three protons ($-OCH_3$), whereas those at ${\delta}$ 6.10 ppm corresponded to two protons ($-OCH_2O-$). Further, two aromatic protons (H-11 and H-12) conveys a doublet-doublet pattern. The H-11 doublet and H-12 doublet appear at ${\delta}$ 7.98 and 8.11, respectively. The $^{13}C$ NMR. spectrum showed a tetrasubstituted with a methylenedioxy group at C2 and C3, and two methoxy groups at C9 and C10. The chemical structure of the berberine was identified by $^1H$, $^{13}C$-nuclear magnetic resonance and electrospray ionization-mass spectroscopy spectral data analysis.

Effects of pH and Potassium Chloride in Solvent System of High-Speed Countercurrent Chromatography (pH 및 염화칼륨 첨가가 고속역류크로마토그래피의 용매시스템에 미치는 영향)

  • Lee, Chang-Ho;Lee, Boo-Yong;Lee, Hyun-Yu;Lee, Cherl-Ho
    • Korean Journal of Food Science and Technology
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    • v.29 no.6
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    • pp.1222-1227
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    • 1997
  • Effects of the physical properties of solvent system such as pH and polarity change by salt addition in solvent system were investigated by using high speed countercurrent chromatography apparatus (Model CCC-1000, Pharm-Tech Research Corp. USA). The changes of pH and interfacial tension in solvent system of high speed countercurrent chromatography did not significantly affect on retention of stationary phase, but induced remarkable changes in the partition coefficient of ginkgo flavonoids, kaempferol, quercetin and isorhamnetin. The partition coefficients of ginkgo flavonoid standard increase with an increased pH of solvent system and quercetin sharply increased at pH 10.0. Retention of stationary phase decreases with an increased concentration of KCl in butanol of solvent system. Interfacial tension between two phase in solvent system of hexane increases with an increased concentration of KCl. The polarity of solvent system significantly changes the partition coefficients of ginkgo flavonoid.

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Canola oil is an excellent vehicle for eliminating pesticide residues in aqueous ginseng extract

  • Cha, Kyu-Min;Lee, Eun-Sil;Kim, Il-Woung;Cho, Hyun-Ki;Ryu, Ji-Hoon;Kim, Si-Kwan
    • Journal of Ginseng Research
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    • v.40 no.3
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    • pp.292-299
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    • 2016
  • Background: We previously reported that two-phase partition chromatography between ginseng water extract and soybean oil efficiently eliminated pesticide residues. However, an undesirable odor and an unpalatable taste unique to soybean oil were two major disadvantages of the method. This study was carried out to find an alternative vegetable oil that is cost effective, labor effective, and efficient without leaving an undesirable taste and smell. Methods: We employed six vegetable oils that were available at a grocery store. A 1-mL sample of the corresponding oil containing a total of 32 pesticides, representing four categories, was mixed with 10% aqueous ginseng extract (20 mL) and equivalent vegetable oil (7 mL) in Falcon tubes. The final concentration of the pesticides in the mixture (28 mL) was adjusted to approximately 2 ppm. In addition, pesticides for spiking were clustered depending on the analytical equipment (GC/HPLC), detection mode (electron capture detector/nitrogen-phosphorus detector), or retention time used. Samples were harvested and subjected to quantitative analysis of the pesticides. Results: Soybean oil demonstrated the highest efficiency in partitioning pesticide residues in the ginseng extract to the oil phase. However, canola oil gave the best result in an organoleptic test due to the lack of undesirable odor and unpalatable taste. Furthermore, the qualitative and quantitative changes of ginsenosides evaluated by TLC and HPLC, respectively, revealed no notable change before or after canola oil treatment. Conclusion: We suggest that canola oil is an excellent vehicle with respect to its organoleptic property, cost-effectiveness and efficiency of eliminating pesticide residues in ginseng extract.

Isolation of Eckol from Ecklonia cava via Centrifugal Partition Chromatography (CPC) and Characterization of it's Anti-inflammatory Activity (고속원심분배 크로마토그래피를 이용한 감태(Ecklonia cava)로부터 Eckol의 분리 및 항염증 활성)

  • Kim, Yoon Taek;Lee, Ji-Hyeok;Ko, Ju-Young;Oh, Jae-Young;Lee, Won-U;Sok, Chang Hyun;Hong, Jin Tae;Jeon, You-Jin
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.48 no.3
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    • pp.301-307
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    • 2015
  • Phlorotannins and marine algal polyphenols, including dieckol, 6,6-bieckol, phloroglucinol, phlorofucofuroeckol-A, and eckol, were isolated from brown seaweeds. These compounds have beneficial bioactivities, and Ecklonia cava has become widely used for the extraction and isolation of phlorotannins. Eckol, in particular, has been to shown to have antioxidant, anti-inflammatory, anticoagulatory, and photoprotective properties. However, due to its low abundance in weaweed, the isolation and purification of eckol are difficult. Its limited availability renders the isolation and purification of eckol labor-intensive processes. Centrifugal partition chromatography (CPC) is an efficient technique for the isolation and purification of eckol. In this study, eckol was isolated from the ethyl acetate fraction of the 70% ethanol extract of E. cava using CPC with a two-phase solvent system of a n-hexane:EtOAc:methanol:water (2:8:3:7, v/v) solution. The purity and anti-inflammatory activity of the isolated eckol were verified by high-performance liquid chromatography and by assaying lipopolysaccharide-induced inflammatory responses in an immortalized murine BV2 microglial cell line, respectively. In conclusion, CPC is a useful technique for simple and efficient isolation of eckol from E. cava.

Polyacetylene Compounds from Panax Ginseng C. A. Meyer

  • Shim, Sang-Chul;Koh, Hun-Yeoung;Han, Byung-Hoon
    • Bulletin of the Korean Chemical Society
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    • v.4 no.4
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    • pp.183-188
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    • 1983
  • Two major and two minor polyacetylenes were isolated from fresh white Korean ginseng roots. The petroleum ether-ethyl ether fractions containing the polyacetylene compounds were collected through solvent fractionation, partition and silica gel column chromatography. Further separation of polyacetylenic fractions was proceeded by bonded normal phase HPLC utilizing a moderately nonpolar microparticulate column. The low pressure liquid chromatography was used for the semi-preparative separation. The chemical structures of the two major polyacetylenes separated were determined by UV, IR, $^1H$ NMR, $^{13}C$ NMR, mass spectra and elemental analysis. One of them is identified to be heptadeca-1-en-4, 6-diyne-3, 9, 10-triol, a new structure, and the other is heptadeca-1, 9-dien-4, 6-diyn-3-ol, known as panaxynol.

Isolation of Berberine from the Rhizome of $Coptis$ $chinensis$ by Centrifugal Partition Chromatography (향류분배 크로마토그라피법에 의한 황련($Coptis$ $chinensis$) 뿌리로 부터 Berberine의 분리)

  • Kim, Jung-Bae
    • The Korean Journal of Food And Nutrition
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    • v.24 no.4
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    • pp.617-621
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    • 2011
  • $Coptis$ $chinensis$ Franch rhizome is one of the important traditional Korea medicines with anti-inflammatory, anti-bacterial, anti-hypertensive and anti-cancer properties. The methanol extract of rhizome from the $Coptis$ $chinensis$ rhizome was purified by using preparative centrifugal partition chromatography (CPC) and HPLC method. The optimum two-phase CPC solvent system was composed of n-butanol:acetic acid:water at a ratio of 4:1:5. Berberine (16.8 mg) was successfully isolated by CPC and HPLC. The chemical structure of the compound was identified by (1 H)$^1H$, $^{13}C$-NMR and ESI-MS spectral data analysis.

Quantitative Analysis of Cinnamic Acid and Cinnamic Aldehyde in Traditionally Preparations by High Performance Liquid Chromatography (고속액체(高速液體)크로마토그라피에 의한 생약제제중(生藥製劑中)의 계피산(桂皮酸) 및 계피(桂皮)알데히드의 정량(定量))

  • Ryu, Kyung-Soo;Song, Bo-Wan
    • Korean Journal of Pharmacognosy
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    • v.11 no.2
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    • pp.75-80
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    • 1980
  • The decoctions and extracts were prepared on the traditionally prescribed four kinds (Kejigamcho-tang, Kejibanha-tang, Keji-tang, Kejiinsam-tang) of preparations containing Cinnamoni Raulus. The contents of cinnamic acid and cinnamic aldehyde in these preparations were determined by high performance liquid chromatography using reverse phase partition column, and 12% MeOH as eluting solvent. The sample was determined using the two wave length, 254nm and 280nm. This method was sucessfully applied to the analysis of cinnamic acid and cinnamic aldehyde of various preparations containing Cinnamons.

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Comparison of Triglyceride Composition between Red Pepper Seed Oils Harvested from the Chungsong and Youngyang Areas (청송.영양산 고추씨 기름의 Triglyceride 조성의 비교)

  • 김동수;전선미;정동윤;김현대;박영호
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.20 no.3
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    • pp.225-232
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    • 1991
  • A Study was carried out to elucidate the triglyceride compositions of the red pepper seed oils harvested from two different areas. The oil was extracted from the red pepper seed with nhexane. Each triglyceride of the oil was separated by thin layer chromatography (TLC) and fractonated by reverse phase high performance liquid chromatography (HPLC) on the basis of acyl carbon numbers, and partition number group(PN) and fatty acid composition of triglyceride were analyzed by gas liquid chromatography (GLC). From the results, it was found that the red pepper seed oils of the Chungsong and Youngyang areas consisted of 14 and 18 kinds of triglycerides, respectively. The red pepper seed oil of the Chungsong area consisted of (C18:2, C18:2, C18:2=41.0%), (C16:0, C18:2, C18:2=37.1%), and that of the Youngyang area consisted of (C18:2, C18:2, C18:2=41.0%), (C16:0, C18:2, C18:2=36.3%) and (C16:0, C16:2, C18:2=8.4%), as the major triglycerides.

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Studies on the Triglyceride Composition of Job's Tears (율무 지질의 Triglyceride 조성에 관한 연구)

  • Lee, Hee-Ja;Cho, Kwang-Yun;Bae, Jung-Surl;Jang, Soon-Wook
    • Korean journal of food and cookery science
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    • v.6 no.4 s.13
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    • pp.27-32
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    • 1990
  • Lipids of Job's tears (Yullmoo) were extracted by the mixture of chloroform: methanol (2:1, v/v) and from these lipids, triglycerides were separated by column chromatography (Sephadex G-25 column) and then confirmed by thin layer chromatography (TLC) and reconfirmed by gas chromatography (GC). The triglycerides were fractionated into 6 groups on the basis of their partition numbers (PN) by reverse phase high performance liquid chromatography (HPLC) on a column Shimpack CLC-ODS using tetrahydrofuran-acetonitril (25:75) mixture as a solvent. Each of these collected fractions gave one to two peaks in the GC chromatograms according to the acyl carbon number (CN) of the triglyceride and fatty acid composition of the triglycerides were also analyzed by GC. From the results, the major triglycerides of Job's tears lipids were estimated to be C18:1 C18:2 C18:2 (OLL, 38.2%), C16:0 C18:2 C18:3 (PLLn, 15.7%), C18:1 C18:1 C18:2 (OOL, 12.6%).

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Phytochemical analysis of Panax species: a review

  • Yang, Yuangui;Ju, Zhengcai;Yang, Yingbo;Zhang, Yanhai;Yang, Li;Wang, Zhengtao
    • Journal of Ginseng Research
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    • v.45 no.1
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    • pp.1-21
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    • 2021
  • Panax species have gained numerous attentions because of their various biological effects on cardiovascular, kidney, reproductive diseases known for a long time. Recently, advanced analytical methods including thin layer chromatography, high-performance thin layer chromatography, gas chromatography, high-performance liquid chromatography, ultra-high performance liquid chromatography with tandem ultraviolet, diode array detector, evaporative light scattering detector, and mass detector, two-dimensional high-performance liquid chromatography, high speed counter-current chromatography, high speed centrifugal partition chromatography, micellar electrokinetic chromatography, high-performance anion-exchange chromatography, ambient ionization mass spectrometry, molecularly imprinted polymer, enzyme immunoassay, 1H-NMR, and infrared spectroscopy have been used to identify and evaluate chemical constituents in Panax species. Moreover, Soxhlet extraction, heat reflux extraction, ultrasonic extraction, solid phase extraction, microwave-assisted extraction, pressurized liquid extraction, enzyme-assisted extraction, acceleration solvent extraction, matrix solid phase dispersion extraction, and pulsed electric field are discussed. In this review, a total of 219 articles published from 1980 to 2018 are investigated. Panax species including P. notoginseng, P. quinquefolius, sand P. ginseng in the raw and processed forms from different parts, geographical origins, and growing times are studied. Furthermore, the potential biomarkers are screened through the previous articles. It is expected that the review can provide a fundamental for further studies.