• Title/Summary/Keyword: Reversed-phase HPLC

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Properties and Activitiy Screening of Chromone Derivatives (크로몬 유도체의 물성 및 활성검색)

  • 김영로;이상현;김경순;정춘식;정재훈;김박광
    • YAKHAK HOEJI
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    • v.44 no.2
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    • pp.107-114
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    • 2000
  • We have synthesized 4-isonitroso-4H-1-benzopyran and 4-amino-2,3-dihydro -4H-1-benzopyran of chromone derivatives by using condensation method. Physico-chemical properties of these compounds were measured and analyzed by UV and HPLC method. The correlation coefficient of their methanol solutions by UV were 0.9992 and 0.9994, respectively. And oxime compound was resolved within 4 min and had a detection limit of 3 ng at S/N=3 by HPLC using a reversed phase column with three solvents(MeOH, $H_2O$, HAc). The amino compound was resolved within 4.5 min and had a detection limit of 10 ng at S/N=3 by HPLC under the same conditions. Anti-diabetic effect of chromone derivatives were investigated in the streptozotocin (STZ)-induced diabetic rats. Diabetes was induced in male Sprague-Dawley rats by injections of STZ (45 mg/kg, i.v). The investigation of the hair growth effect of isonitrosobenzopyran and 4-aminobenzopyran on the hair of black mouse (C57BL/6) was also carried out. The administraion of their ethanol solution to the black mouse (C57BU/6) through skin them promoted the growth of hair.

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Solid-Phase Extraction of Caffeine and Catechin Compounds from Green Tea by Caffeine Molecular Imprinted Polymer

  • Jin, Yinzhe;Row, Kyung-Ho
    • Bulletin of the Korean Chemical Society
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    • v.28 no.2
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    • pp.276-280
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    • 2007
  • In this work, caffeine and some catechin compounds + C, EC, EGC, and EGCG were extracted from green tea by using molecular imprinted polymers (MIP) as sorbent materials in a solid-phase extraction (SPE) process known as MISPE (molecular imprinted solid-phase extraction). For synthesis of MIP, caffeine was employed as the template, MAA as the monomer, EGDMA as the crosslinker, and AIBN as the initiator. A solution of caffeine (0.2 mg/mL in methanol) was utilized in the solid extraction cartridges following loading, washing, and elution procedures with acetonitrile, methanol, and methanol-acetic acid (90/10, %v/v) as the solvents, respectively. This solid-phase extraction protocol was applied for the extraction of caffeine and some catechin compounds from green tea. A comparison was made between the results obtained with the MIP cartridges and a traditional C18 reversed-phase cartridge. It was thereupon found that the recovery of caffeine by the MIPbased sorbent used in this work was almost two and four times greater than that by a commercially available C18 material. A quantitative analysis was conducted by high performance liquid chromatography (HPLC) using a C18 column (5 μm, 250 × 4.6 mm) with methanol/water (40/60, %v/v) as the mobile phase at a flow rate of 0.5 mL/min.

Quantitative Determination of Flavonoids from Stems of Spatholobus suberectus

  • Park, Jinseon;Park, So Yeon;Shim, Sang Hee
    • Natural Product Sciences
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    • v.19 no.2
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    • pp.145-149
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    • 2013
  • A simple reversed phase HPLC method was established for quantitative determination of liquiritigenin (1), genistein (2), isoliquiritigenin (3), and 7-hydroxyflavanone (4) from stems of Spatholobus suberectus Dunn (Leguminosae) using a binary gradient of $H_2O$ and MeOH as a mobile phase with UV detection at 280 nm. All calibration curves showed good linear regression ($r^2$ > 0.998) within test ranges. The detection limits of the four compounds were $0.43{\sim}1.63{\mu}g/mL$. The contents of four flavonoids (1 - 4) from the stem of S. suberectus were 6.54 mg/g, 1.66 mg/g, 6.65 mg/g, and 1.93 mg/g, respectively.

Oxidative Degradation Kinetics of Tocopherols during Heating

  • Chung, Hae-Young
    • Preventive Nutrition and Food Science
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    • v.12 no.2
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    • pp.115-118
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    • 2007
  • Tocopherols are important lipid-phase antioxidants that are subject to heat degradation. Therefore, kinetic analyses for oxidative degradation of tocopherols as a function of temperatures and times were performed. Alpha-, gamma- and delta-tocopherols dissolved in glycerol were heated at 100${\sim}$250$^{\circ}C$ for 5~60 min. Oxidized tocopherols were analyzed by HPLC using a reversed phase ${\mu}$-Bondapak C$_{18}$-column with two kinds of elution solvent systems in a gradient mode. The degradation kinetics for tocopherols followed a first-order kinetic model. The rate of tocopherol degradation was dependent on heating temperatures. The degradation rate constants for ${\gamma}$- and ${\delta}$-tocopherols were higher than those for ${\alpha}$-tocopherol. The experimental activation energies of ${\alpha}$-, ${\gamma}$- and ${\delta}$- tocopherols were 2.51, 6.05 and 5.34 kcal/mole, respectively. The experimental activation energies for the oxidative degradation of ${\gamma}$- and ${\delta}$-tocopherols were higher than that of ${\alpha}$-tocopherol.

Analysis of the Coumarin Constituents in Peucedanii Radix (식방풍중의 Coumarin성분의 확인 및 정량)

  • Shin, Kuk-Hyun;Kang, Sam-Sik;Chi, Hyung-Joon
    • Korean Journal of Pharmacognosy
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    • v.23 no.1
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    • pp.20-23
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    • 1992
  • A new method for the analysis of coumarin constituents in the roots of Peucedanum japonicum by high performance liquid chromatography was established. Among two coumarin constituents identified, peucedanol was confirmed to be applicable to a standard compound. A reversed phase system with a ${\mu}Bondapak$ C_{18}$, column using $H_2O-MeOH=5\;:\;4$ as a moble phase was developed. Peucedanol and a minor constituent, umbelliferone were detected at 333nm and the analysis was successfully carried out within 20 min.

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Determination of Byakangelicin in Angelicae dahuricae Radix by High Performance Liquid Chromatography (고속액체크로마토그라피에 의한 백지근 중 Byakangelicin의 정량)

  • Shin, Kuk-Hyun;Kang, Sam-Sik;Chi, Hyung-Joon
    • Korean Journal of Pharmacognosy
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    • v.21 no.3
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    • pp.239-241
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    • 1990
  • A new method for quantitative determination of byakangelicin in Angelicae dahuricae Radix by high performance liquid chromatography was established. A reversed-phase system with a ${\mu}Bondapak$ $C_{18}$ column using THF : dioxane : MeOH : HAc : 5% $H_3PO_4$ : $H_2O$=72.5 : 62.5 : 25 : 10 : 1 : 329 as a mobile phase was developed. Byakangelicin together with ter-O-byakangelicin and oxypeucedanin methanolate, and isooxypeucedanin as an internal reference were detected at 350 nm and the analysis was successfully carried out within 30 min.

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Determination of p-Methoxycinnamic Acid in Scrophulariae Radix by High Performance Liquid Chromatography (고속액체크로마토그라피에 의한 현삼근(玄蔘根) 중 p-Methoxycinnamic acid의 정량)

  • Lee, Sang-Hyun;Chi, Hyung-Joon;Shin, Kuk-Hyun
    • Korean Journal of Pharmacognosy
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    • v.30 no.3
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    • pp.328-331
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    • 1999
  • A new method for quantitative determination of p-methoxycinnamic acid in Scrophulariae radix by high performance liquid chromatography was established. A reversed-phase system with SPHERI-5 RP-18 5 micron $(250\;{\times}\;4.6\;mm)$ column using TFA (0.05%) and acetonitrile as a mobile phase was developed. p-Methoxycinnamic acid and N-(p-methoxycinnamoyl)-p-aminophenol as an internal reference were detected at 310 nm and the analysis was successfully carried out within 50 min.

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Determination of Icariin in Epimedii Herba by High Performance Liquid Chromatography (고속액체크로마토그라피에 의한 음양곽 중 Icariin의 정량)

  • Shin, Kuk-Hyun;Kang, Sam-Sik;Chung, Sun-Gan;Cho, Eui-Hwan
    • Korean Journal of Pharmacognosy
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    • v.20 no.1
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    • pp.21-24
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    • 1989
  • A new method for quantitative determination of icariin in Epimedii Herba by high performance liquid chromatography was established. A reversed-phase system with $a\;{\mu}Bondapak\;C_{18}$ column using methanol in water(15% to 70%, gradient elution) as a mobile phase was developed. Icariin and spinosin as an internal reference were detected at 350 nm and the analysis was successfully carried out within 30 min.

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Determination of Catecholamines and Their Metabolites in Rat Brain by High Performance Liquid Chromatography with Electrochemical Detector (HPLC-ECD에 의한 흰쥐 뇌 부위별 Catecholamine 및 대사산물의 신속정량법)

  • Ro, Ihl-Hyeob
    • YAKHAK HOEJI
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    • v.32 no.1
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    • pp.50-54
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    • 1988
  • A simple and sensitive method was studied for the simultaneous determination of catecholamine, indoleamine and their related metabolites by high performance liquid chromatography with electrochemical detector. Norepinephrine, dopamine, serotonin and their metabolites of 3,4-dihydroxyphenylacetic acid, homovanillic acid, 5-indoleacetic acid were resolved from rat brain tissue homogenates by separation on reversed phase $C_{18}$ column with mobile phase consisting of monochloroacetate buffer (pH2.47), 1.42mM sodium octyl sulfonate and 7% acetonitrile. Both catechols and indoles can be eluted in 15min. The sensitivities of this method are sufficient for determination of at least 100 pg of neurochemical amines in brain samples, for example, frontal cortex, olfactory bulb, striatum, septum, hippocampus, thalamus, hypothalamus, medulla & pons and cerebellum. The highest level of dopamine was observed in striatum whereas norepinephrine and serotonin were in hypothalamus.

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Chiral Separation of $\beta$-Blockers after Derivatization with (-)-Menthyl chloroformate by Reversed-Phase High Performance Liquid Chromatography

  • Kim, Kyeong-Ho;Choi, Pok-Wha;Hong, Seon-Pyo;Kim, Hyun-Ju
    • Archives of Pharmacal Research
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    • v.22 no.6
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    • pp.608-613
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    • 1999
  • Optimum conditions of chiral derivatization reaction of $\beta$-blockers (acebutolol, arotinolol, betaxolol, bisoprolol, celiprolol, metoprolol and pindolol) with (-)-menthyl chloroformate were investigated for the resolution by HPLC. With more than 30 times molar excess of (-)-methyl chloroformate chiral derivatization reactions were completed within one hour at room temperature except arotinolol and celiprolol. Diastereomeric derivatives of $\beta$-blockers were well resolved on the ODS column using acetonitrile-methanol-water as a mobile phase.

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