• Title/Summary/Keyword: extraction chromatography

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Extraction and separation of glabridin from licorice by reversed phase high performance liquid chromatography

  • Choi, Du Young;Row, Kyung Ho
    • Analytical Science and Technology
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    • v.19 no.6
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    • pp.455-459
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    • 2006
  • The extraction and separation of glabridin from licorice root by HPLC was performed in this work. First, by investigating the different extraction solvents, extraction methods and extraction times, a one-hour ultrasonic extraction procedure with ethyl acetate as the extraction solvent was optimized. Then the ethyl acetate extraction was applied to RP-HPLC for separation of glabridin. The column efficiencies and resolutions were experimentally investigated with different mobile phase compositions. Baseline separation of glabridin was obtained under the mobile phase composition of 50/50 vol.% (ACN/water). The retention time of glabridin was 20.3 min. The peak of glabridin was collected from the HPLC elution for several times and identified by LC/MS. Under the optimum extraction and HPLC separation methods, 1.26 g of glabridin per kg licorice root could be extracted.

A Study on the Isolative determination of Smithion and Malathion in the Human Blood by Gas Chromatography (Gas Chromatography에 의한 인체혈액중에서 스미치온 및 마라치온의 분리정량에 관한 연구)

  • 구성회;박성우;이영자
    • Journal of Environmental Health Sciences
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    • v.5 no.1
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    • pp.58-60
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    • 1978
  • This experiment was carried out to determine the amount of organophosphorous pesticides accumulated in farmer's blood during the farming season. The Blood had been collected for about 5ml from farmer's, and extraction was purified on a Avicel/Darco G-Co (1:10) column and determined by Gas Chromatography using AFID supported on 2% EGA. The Gas chromatographic detection yielded recoveries from the blood of 88% for smithion 94% for malathion. The amount of average contamination shows 0.045ppm for smithion. 0.054ppm for malathion.

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Ultrasonic-assisted Micellar Extraction and Cloud-point Pre-concentration of Major Saikosaponins in Radix Bupleuri using High Performance Liquid Chromatography with Evaporative Light Scattering Detection

  • Suh, Joon-Hyuk;Yang, Dong-Hyug;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2637-2642
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    • 2011
  • A new ultrasonic-assisted micellar extraction and cloud-point pre-concentration method was developed for the determination of major saikosaponins, namely saikosaponins -A, -C and -D, in Radix Bupleuri by high performance liquid chromatography with evaporative light scattering detection (HPLC-ELSD). The non-ionic surfactant Genapol X-080 (oligoethylene glycol monoalkyl ether) was chosen as the extraction additive and parameters affecting the extraction efficiency were optimized. The highest yield was obtained with 10% (w/v) Genapol X-080, a liquid/solid ratio of 200:1 (mL/g) and ultrasonic-assisted extraction for 40 min. In addition, the optimum cloud-point pre-concentration was reached with 10% sodium sulfate and equilibration at $60^{\circ}C$ for 30 min. Separation was achieved on an Ascentis Express C18 column (100 ${\times}$ 4.6 mm i.d., 2.7 ${\mu}M$) using a binary mobile phase composed of 0.1% acetic acid and acetonitrile. Saikosaponins were detected by ELSD, which was operated at a $50^{\circ}C$ drift tube temperature and 3.0 bar nebulizer gas ($N_2$) pressure. The water-based solvent modified with Genapol X-080 showed better extraction efficiency compared to that of the conventional solvent methanol. Recovery of saikosaponins ranged from 93.1 to 101.9%. An environmentally-friendly extraction method was successfully applied to extract and enrich major saikosaponins in Radix Bupleuri.

Optimization of Extraction of Astaxanthin from Portunus trituberculatus by Ionic Liquids (이온성 액체를 사용한 꽃게 껍질에서 아스타크산틴 추출 조건의 최적화)

  • Lee, Yu Jin;Lee, Yu Ri;Tang, Baokun;Row, Kyung Ho
    • KSBB Journal
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    • v.28 no.4
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    • pp.238-243
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    • 2013
  • Astaxanthin is one of the carotenoid with strong antioxidant. The conditions of extraction of astaxanthin from Portunus trituberculatus were optimized in this work. Six factors of conditions such as, extraction method, extraction solvent, ratio of solvent to raw material, temperature, and time, were investigated. For the increase of the extraction yield, ionic liquids were used as additives in the extraction solvent. The optimum extraction conditions were found: heat reflux extraction, Dichloromethane/methanol (25:75, v/v) as solvent, 1:30 of the ratio of solvent raw material, $80^{\circ}C$, 90 min, and ionic liquid as additive. As a result, 45.81 ${\mu}g/g$ of astaxanthin was extracted from waste.

Comparison of Static and Dynamic Solvent Extraction of Polychlorinated Dibenzofurans from Fly Ash

  • Yang, Jeong Soo;Jeong, Jang Hwan;Yu, Euy Kyung
    • Analytical Science and Technology
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    • v.17 no.4
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    • pp.295-301
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    • 2004
  • In this study, static and dynamic solvent extractions are compared for more efficient extraction of polychlorinated dibenzofurans (PCDFs) from fly ash. Static solvent extraction rather than dynamic extraction showed a higher recovery of PCDFs, which was adsorbed strongly with fly ash. The effects of parameters, such as temperature, toluene-isopropyl alcohol mixture, static and dynamic time flow rate, and solvent volume on the extraction were investigated and the variations in average recoveries of PCDFs were explained. In both extractions, temperature was an effective parameter because the higher temperature gave the higher recoveries. In dynamic solvent extraction, dynamic time was more effective than flow rate and solvent volume for the extraction of PCDFs from fly ash. Multi-layer column chromatography on neutral and acidic silica gel with n-hexane was used for cleaning up the extracts. The quantification of the PCDFs extracted was performed using HPLC-UV.

Characterization of Squalene Synthase Inhibitor Isolated from Curcuma longa (울금(Curcuma longa)으로부터 분리한 squalene synthase 저해물질의 특성)

  • Choi, Sung-Won;Yang, Jae-Sung;Lee, Han-Seung;Kim, Dong-Seob;Bai, Dong-Hoon;Yu, Ju-Hyun
    • Korean Journal of Food Science and Technology
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    • v.35 no.2
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    • pp.297-301
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    • 2003
  • An inhibitor of squalene synthase, a key enzyme in the cholesterol biosynthetic pathways and a target for improved agents to lower plasma levels of low-density lipoprotein, was sequentially purified from Curcuma longa by acetone extraction, silica gel column chromatography, and sephadex LH-20 column chromatography. Active compound, YUF-01, was successfully purified and analyzed as $C_{20}H_{21}O_6$ by electron ionization mass spectrum. Through $^1H-NMR$ and $^{13}C-NMR$ analyses, YUF-01 was identified as curcumin, which showed strong inhibition of squalene synthase.

Purification of Isoflavone from Soybean Hypocotyls using Various Resins

  • Choi Yeon-Bae;Kim Kang-Sung
    • Journal of Environmental Health Sciences
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    • v.31 no.3
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    • pp.221-226
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    • 2005
  • Isoflavone was extracted with various concentration of aqueous methanol using whole hypocotyls as the starting material. Whole hypocotyls were preferred as the raw material because the residue could be easily removed from the solvent after the extraction process. Extraction yield was almost constant at the methanol concentration of $20-80\%$. Most of the isoflavone was extracted within 1 hr, and the extraction yield remained almost constant thereafter. When the concentration of methanol was $80\%$, the content of total solid was reduced due to the reduced extraction of contaminating protein as the result of protein insolubilization. Among resins tested, Diaion HP-20, Amberlite XAD-16, and Amberlite IRC-50 showed the highest capacity to absorb the compound. Open column chromatography with Diaion HP-20 showed that $80\%$ aqueous ethanol was most efficient as the eluting solvent with final recovery of the phytochemical being more than $95\%$. Maximum adsorption of the phytochemical occurred at the acidic pH 2-4. When the spatial velocity was increased to 15 and more, the degree of adsorption was decreased, whereas below spatial velocity of 15, the adsorption capacity of isoflavone to the resin was almost constant. The purity of the isoflavone purified by column chromatography was $78\%$.

Optimization of Disk Sorptive Extraction Based on Monolithic Material for the Determination of Aroma Compounds from Lantana camara L. by Gas Chromatography-Mass Spectrometry

  • Jang, Hye-Jin;Son, Hyun-Hwa;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.32 no.12
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    • pp.4275-4280
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    • 2011
  • Present study describes the optimization of disk type sorptive extraction using monolithic material (Mono Trap) for the analysis of volatile aroma compounds from Lantana camara L. in combination with gas chromatography/mass spectrometry (GC/MS). Monolithic material sorptive extraction (MMSE) is a new sampling technique using a monolithic hybrid adsorptive disk (O.D. 10 mm, 1 mm thickness) made of high purity silica and activated carbon having a large surface area chemically bonded with octadecyl silane (ODS). The experimental parameters that may influence the MMSE efficiency have been optimized. Linearity, accuracy, precision and detection limits were evaluated to assess the performance of the proposed method. The method was validated with real plant samples of Lantana camara L. Twenty eight compounds including the main representative compounds of ${\alpha}$-curcumene and ${\beta}$-caryophyllene were found in analyzed samples. Results proved that proposed method could be used as a good alternative for the analysis for such volatile aroma compounds in plant samples.