• Title/Summary/Keyword: methanol separation column

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Isolation and Quantitative Analysis of Betulinic Acid and Alphitolic Acid from Zyziphi Fructus (대추로부터 베튜리닉 산과 알피톨릭 산의 분리 및 정량)

  • Bae, Gi-Hwan;Lee, Sang-Myeong;Lee, Eun-Sil;Lee, Jun-Seong;Gang, Jong-Seong
    • YAKHAK HOEJI
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    • v.40 no.5
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    • pp.558-562
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    • 1996
  • Betulinic acid and alphitolic acid, the triterpenoids of Zyziphi Fructus, were isolated with silica gel column chromatography and used as the standard substances for the analysis. The compounds were determined with HPLC and HPTLC. They were separated on reversed phase column (Nova-Pak C18) with 0.05M Na2HPO4-methanol (19:81) in HPLC and detected at 210nm. Separation on HPTLC precoated silica gel F254 plates was carried out with chloroform-methanol (6:1) and the separated compounds were reacted with p-anisaldehyde and detected at 540nm. The contents of betulinic acid and alphitolic acid in Zyziphi Fructus from four different regions in Korea were in the range of 2.9~3.8% and 3.2~3.9%, respectively.

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Phytochemical Constituents of Actinidia arguta (다래나무뿌리의 식물화학적 성분)

  • Whang, Joon-Ih;Zee, Ok-Pyo;Moon, Hyung-In
    • Korean Journal of Pharmacognosy
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    • v.31 no.3
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    • pp.357-363
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    • 2000
  • The root of Actinidia arguta was extracted with methanol and the methanol extract was suspended in $H_2O$ and successively partitioned with n-hexane, $CH_2Cl_2$, EtOAc and n-BuOH. Repeated column chromatographic separation of the EtOAc extract resulted in the isolation of two flavonoids (compounds 2 and 3) and two triterpenes (compounds 1 and 4) and $CH_2Cl_2$, extract to afford three lignans (compounds 5-7). Their structures have been established by spectroscopic, means to be (+)-tormentoside(1), (-)-catechin(2), (-)-epicatechin(3), (+)-uscaphic $acid-28-O-[\beta}-D-glucopyranoside$(4), (+)-pinoresinol(5), (+)-medioresinol(6), and (-)-syringaresinol(7).

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Antioxygenic and Peroxide-decomposing Activities of Antarctic Krill Lipids (Krill 지질(脂質)의 항산화성(抗酸化性)과 과산화물(過酸化物) 분해작용(分解作用))

  • Lee, Jong-Ho
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.13 no.3
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    • pp.326-333
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    • 1984
  • The oxidation rate of krill lipids is very slow and no peroxides are accumulated even after long storage. By means of various chromatographic techniques and mass spectrophotometry, the primary antioxidant has been identified as ${\alpha}$-tocopherol. The phospholipid fractions did not show any antioxidative activity but peroxide-decomposing properties of total lipids depended upon the phospholipid contents. The peroxide-decomposing activities of phospholipids were due to the presence of polar materials generated during the storage. The most peroxide-decomposing fractions of oxidized krill lecithin by DEAE-cellulose column chromatography was low-molecule fraction (mean molecular weight: 182) and high-molecule fraction (mean molecular weight: 1942) was the next. The separation of peroxide-decomposing properties from low-molecule fraction was achieved by partitioning between chloroform and methanol/water. The methanol/water fraction showed strong peroxide-decomposing activities and main component of this fraction was assumed hydroxyamine compounds derived from choline.

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Bilin and Bilinone Chlorophyll Catabolite Content in the Hamamelidaceae Autumnal Leaves

  • Djapic, Nina
    • Natural Product Sciences
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    • v.28 no.1
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    • pp.18-26
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    • 2022
  • In order to facilitate the quantification in autumnal Hamamelidaceae leaves, a HPLC method was used for the determination of two chlorophyll catabolites and their isomers: bilin-type (1) and bilinone-type (2) ones. The separation was done on a RP-C4 column with a gradient solvent system of 0.1% trifluoroacetic acid aqueous-methanol at the flow-rate of 0.2 mL/min and detected at 244 nm. The quantity of bilin-type (1) and bilinone-type (2) chlorophyll catabolite isomers from ten species of Hamamelidaceae autumnal leaves methanol extracts: Corylopsis pauciflora, Corylopsis spicata, Forthergilla major, Hamamelis intermedia, Hamamelis japonicum, Hamamelis japonicum var. flavopurpurscens, Hamamelis virginiana, Parrotiopsis jacquemontiana, Parrotia persica and X Sycoparrotia semidecidua were from 0.85 mg/g ~ 57.50 mg/g for bilin-type isomers (1) and 3.40 mg/g ~ 49.30 mg/g for bilinone-type isomers (2). The results obtained gave insight in quantitative bilintype (1) and bilinone-type (2) chlorophyll catabolite composition of the Hamamelidaceae plant species autumnal leaves.

Reversed-Phase Ion-Pair Chromatography of Aromatic Sulfonic Acids (방향족 슬폰산들의 역상 이온쌍 크로마토그래피)

  • Sam-Woo Kang;Hae-Beom Oh;Seung-Seok Lee
    • Journal of the Korean Chemical Society
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    • v.30 no.2
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    • pp.224-230
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    • 1986
  • Dodecyltrimethylammonium bromide (DTAB) was examined as a counter-ion in the separation of aromatic sulfonic acids on alkylmodified silica (ODS) column by reversed-phase ion-pair chromatography. The capacity factor of acids was investigated and separation was attempted. The capacity factor of samples was influenced by the several factors such as a concentration of counter-ion, concentration of methanol, kinds and concentration of electrolyte in mobile phase as well as kinds and position of functional group in samples. Some mixtures of samples were able to be separated under optimum condition.

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Separation and Determination of Cefatrizine ${\cdot}$ Propylene Glycol by High-performance Liquid Chromatography (High Performance Liquid Chromatography 를 이용한 Cefatrizine ${\cdot}$ Propylene Glycol 의 분리 및 정량)

  • Kwon, Shoon-Ja;Lee, Ki-Chang;Choe, Koang-Hoon
    • Journal of the Korean Applied Science and Technology
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    • v.6 no.1
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    • pp.27-30
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    • 1989
  • The fast separation and determination of cefatrizine${\cdot}$propylene glycol and inmpurities - TACA: 7-amino-3-(1,2,3-triazol-4-yl)thiomethyl-3-cephem-4-carboxylic acid and 7-ACA; 7-amino cephalosporanic acid - was performed by the high poerformance liquid chromatography using octadecyl siland (ODS) column. Methanol and ammonium phosphate buffer [$0.03M(NH_4)_2\;HPO_4$, (pH 7.5)] was used analyze, as eluent. The experimental value of the contents of cefatrizine${\cdot}$propylene glycol and impurities agree with the theoretical value of those.

A study on separation and characterization of matrix metalloproteinase-9 inhibitors from natural plants (천연 식물 추출물에서 Matrix Metalloproteinase-9 활성 억제제의 분리 및 특성화에 관한 연구)

  • Hur, Yong-Chul;Park, Sung-Woo;Kim, Tai-Jin
    • Analytical Science and Technology
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    • v.18 no.3
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    • pp.188-193
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    • 2005
  • Three different oriental natural plants (Angelicae Dahuricae Radix, Sanguisorba Officinalis L, Euonymus alatus) were extracted with 70% methanol under refluxing for 4 hr in order to investigate their inhibitory effect on Matrix Metalloproteinase-9 (MMP-9) by a modified gelatin zymography, where only euonymus alatus showed the inhibitory effect on the activity of Matrix MMP-9. The fraction was collected by using the mixture of ethyl acetate and hexane on silica gel column. Seven portions were obtained and three fractions of them (first, third and forth) showed inhibitory effect on the zymography. To verify the effect of these substances on cells, human hepatoma, Hep3B cells as a cancer model, and Chang liver cells as a normal model were selected. In order to examine the cell viability, $1{\mu}g/mL$ of each extract was treated on cells. Most of the methanol soluble fractions showed negligible toxicity on human liver cell line.

Simultaneous Separation Analysis of Some Metal Ions in Piperidinedothiocarbamate Chelates by Reversed-Phase Liquid Chromatography (역상 액체 크로마토그래피에 의한 몇가지 금속 이온들의 Piperidinedithiocarbamate 킬레이트 동시분리분석)

  • Lee, Won;Bahng, Seung-Hoon;Kim, Mi-Kyoung
    • Analytical Science and Technology
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    • v.13 no.1
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    • pp.27-33
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    • 2000
  • Simultaneous separation and analysis of Ni(II), Pd(II), Co(II), Cu(II) and Hg(II) in peperidinedithiocarbamate (PDTC) chelates were investigated by reversed phase liquid chromatography. The optimum conditions for the separation of PDTC metal chelates were examined with respect to the pH, extraction solvent, and mobile phase strength on Novapak $C_{18}$ column using methanol/water mixture as mobile phase. All metal PDTC chelates were eluted in an acceptable range of capacity factor value ($0{\leq}log\;k^{\prime}{\leq}1$). The linear calibration curves were obtained in the concentration range of $0{\sim}1.2{\mu}g/mL$ for five metal ions, and also good precision in the range of 1.96~3.41% RSD was obseved. Under the optimum conditions, trace metat ions in the composite water sample were successfully separated and determined with relative error of ${\pm}2.0%$.

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A HPLC-UV method for quantification of ivermectin in solution from veterinary drug products

  • Kim, Young-Wook;Jeong, Wooseog
    • Korean Journal of Veterinary Service
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    • v.45 no.3
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    • pp.243-248
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    • 2022
  • The HPLC conditions for analysis of ivermectin in solutions dosage forms of commercial anthelmintics are different for each product. The purpose of this study was to establish a standardized chromatographic method for the quantification of ivermectin in solution. The separation was achieved on Waters Xbridge C18 column (4.6×150 nm, 5 ㎛) using different kinds of mobile phase composed of water/methanol/acetonitrile (15/34/51, v/v and 19.5/27.5/53, v/v), with UV detection at wavelengths 245 nm and 254 nm. A total of five commercial ivermectin in solution samples were analyzed. In this study, the optimal chromatographic conditions for analysis of ivermectin in solution were mobile phase of water/methanol/acetonitrile (15/34/51, v/v) at a flow rate of 1.0 mL/min and a detection wavelength of 245 nm using a Waters Xbridge C18 column (4.6×250 nm, 5 ㎛) at a column temperature of 25℃. The linearity was observed in the concentration range of 50~150 ㎍/mL, with a correlation coefficient, r2= 0.99999. The limit of detection and the limit of quantification were 0.88 and 2.68 ㎍/mL, respectively. The accuracy (% recovery) was found to be 98.9 to 100.3%. Intra-day and Intermediate precisions with relative standard deviations were less than 1.0%. The content of ivermectin for five market samples ranged 91.2~102.7%. The proposed method was also found to be robust, therefore, the method can be used for the routine analysis of ivermectin in solutions dosage forms.

Separation of Glabridin from Licorice by RP-HPLC (RP-HPLC를 이용한 감초에서 Glabridin의 분리)

  • 정용안;이광진;권문주;노경호
    • KSBB Journal
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    • v.18 no.5
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    • pp.408-411
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    • 2003
  • By reversed-phase high-performance liquid chromatography, the extraction and separation of glabridin by from licoricce root was performed in this work. The column efficiencies and resolutions of glabridin were investigated with mobile phase composition on the reversed-phase chromatographic system. The glabridin collected from licorice root was identified by LC/MS. The mobile phase used to extract glabridin were composed of ethanol, methanol, acetone, and ethyl acetate. For one-hour ultrasonic extraction with solvent of ethyl acetate, the favorable content of glabridin was obtained as 1.26g/kg. The glabridin was well separated in the mobile phase composition of 50/50 vol. % (acetonitrile/water).