• Title/Summary/Keyword: XAD-4

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Phenolic Compounds from Phyllanthus ussuriensis (여우주머니의 Phenol성 화합물)

  • 함인혜;왕도미나;조은선;조형권;황완균
    • YAKHAK HOEJI
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    • v.45 no.3
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    • pp.237-244
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    • 2001
  • The herbaceous species of phyllanthus in this genus are used as hyperglycemic, diuretic, and malaria agent in the world. For the phytochemical studies and the investigation of medicinal resources in the Phyllanthus species, Phyllanthus ussuriensis (Euphorbiaceae) were used and the studies of constituents in this plant were carried out. From the aqueous fraction of methanolic extract, one flavonoid (quercetin-3-O-rutinoside), two gallotannins (gallic acid, methyl gallate), and two ellagitannins (corilagin, geraniin) were isolated through fractionation and repeated column chromatography using Amberlite XAD-4, ODS gel, and sephadex LH-20. The structures of these compounds were identified on the basis of spectroscopic evidences.

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On-line SPE-HPLC Method using Alumina Filtering to Selectively Extract Phenolic Compounds from Environmental Water

  • Lee, Sung-Kwang
    • Bulletin of the Korean Chemical Society
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    • v.31 no.12
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    • pp.3755-3759
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    • 2010
  • A on-line SPE (solid phase extraction)-HPLC preconcentration method was developed for the determination of phenolic compounds at trace levels in environmental water sample. XAD-4 and Dowex 1-X8 were used as sorbent in the on-line SPE-HPLC method for the selective enrichment of nine phenolic compounds, which are included in the priority pollutants list of the US EPA. Also alumina prefiltering considerably reduced the amount of interfering peaks due to humic substances that could accumulated due to the preconcentration step and prevent quantification of polar phenolic compounds in environmental water samples. This method was used to determine the phenolic compounds in tap and river water and superiority to the US EPA 625 method in its enrichment factor, pretreatment time, recoveries, and detection limit. The limits of detection were in the range of $0.3-0.9\;{\mu}g/L$ in tap water sample.

Preconcentration and Determination of Fe(III) from Water and Food Samples by Newly Synthesized Chelating Reagent Impregnated Amberlite XAD-16 Resin

  • Tokahoglu, Serife;Ergun, Hasan;Cukurovah, Alaaddin
    • Bulletin of the Korean Chemical Society
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    • v.31 no.7
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    • pp.1976-1980
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    • 2010
  • A simple and reliable method has been developed to selectively separate and concentrate trace amounts of Fe(III) ions from water and food samples by using flame atomic absorption spectrometry. A new reagent, 5-hydroxy-4-ethyl-5,6-di-pyridin-2-yl-4,5-dihydro-2H-[1,2,4] triazine-3-thione, was synthesized and characterized by using FT-IR spectroscopy and elemental analysis. Effects of pH, concentration and volume of elution solution, sample flow rate, sample volume and interfering ions on the recovery of Fe(III) were investigated. The optimum pH was found to be 5. Eluent for quantitative elution was 10 mL of 2 M HCl. The preconcentration factor of the method, detection limit (3s/b, ${\mu}gL^{-1}$) and relative standard deviation values were found to be 25, 4.59 and 1%, respectively. In order to verify the accuracy of the method, two certified reference materials (TMDA 54.4 lake water and SRM 1568a rice flour) were analyzed. The results obtained were in good agreement with the certified values. The method was successfully applied to the determination of Fe(III) ions in water and food samples.

Purification and Characterization of the Siderophore from Bacillus licheniformis K11, a Multi-functional Plant Growth Promoting Rhizobacterium. (다기능 PGPR균주 Bacillus licheniformis K11이 생산하는 항진균성 Siderophore의 정제와 특성)

  • Woo, Sang-Min;Woo, Jae-Uk;Kim, Sang-Dal
    • Microbiology and Biotechnology Letters
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    • v.35 no.2
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    • pp.128-134
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    • 2007
  • Previously, we isolated plant growth promoting rhizobacterium (PGPR) Bacillus licheniformis K11 which could produce auxin, cellulase and siderophore. The siderophore of B. licheniformis K11 $(siderophore_{K11})$ was determined to be a catechol type siderophore which is produced generally by Bacillus spp. B. licheniformis K11 could produce the siderophore most highly after 96 h of incubation under nutrient broth at $20^{\circ}C$ with initial pH 9.0. For the production of the $siderophore_{K11}$, trehalose and $NH_4Cl$ were the best carbon and nitrogen sources in Davis minimal medium, respectively. The $siderophore_{K11}$ was Produced in M9 medium (pH 9.0) after 4 days at $20^{\circ}C$, and purified from culture broth of B. licheniformis K11 by using Amberlite XAD-2, Sephadex LH-20 column chromatography, and reversed-phase HPLC. The $siderophore_{K11}$ had the biocontrol activity against spore germination of P. capsici and F. oxysporum on potato dextrose agar (PDA). The results indicate that the $siderophore_{K11}$ is an antifungal mechanism of B. licheniformis K11 against phytopathogenic fungi.

Anti-tumor Activity of the Extract of $Alpinia$ $officinarum$ using Hollow Fiber Assay (Hollow FiberAssay을 이용한 고량강 추출물의 항종양 효과)

  • Lee, Keyong-Ho;Rhee, Ki-Hyeong
    • The Korean Journal of Food And Nutrition
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    • v.24 no.4
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    • pp.496-500
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    • 2011
  • The purpose of this investigation was to evaluate anti-tumor activity and detect what compounds affect its activity form $Alpinia$ $officinarum$ Hance. Two fractions, methanol and ethylacetate, were isolated by Amberlite XAD-2 resin column chromatography from methanol extract of the rhizomes of $Alpinia$ $officinarum$. In hollow fiber assay, the methanol extract and methanol fraction were found to inhibit the tumor growth against colon tumor cell lines such as Colo-320, HCT116 and WiDr. Three diarylheptanoids [5-hydroxy-1,7-diphenyl-3-heptanone, 5-hydroxy-7-(4"-hydroxy-3"-methoxyphenyl)-1-phenyl-3-heptanone and 3,5-dihydroxy-1,7-diphenylheptane] and two flavonoids [galangin and kaempheride] were isolated and identified from the methanol fraction, which is higher activity than ethylacetate fraction. Among these diarylheptanoids and flavonoids, 3,5-dihydroxy-1,7-diphenylheptane, galangin and kaempheride as active components on anti-tumor activity were mainly posited in methanol fraction.

Formation of Furans during the Acid Hydrolysis of Agar and Their Removal by Treatments of Lime, Steam-stripping and Hydrophobic Resins (한천의 산 당화에 의한 Furan화합물의 생성 및 제거)

  • Kim, Na-Hyun;Lee, Jae-Won;Seo, Yung-Bum;Yoon, Min-Ho
    • Korean Journal of Agricultural Science
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    • v.36 no.2
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    • pp.225-232
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    • 2009
  • The ratio of saccharification and formation of furans during the acid hydrolysis of agar with oxalic acid and sulfuric acid were examined base on the contents of the agar and acids. The ratio of saccharification in oxalic acid appeared to be 51~59% somewhat higher than 49~61% of sulfuric acid. Formation of the furans during the acid hydrolysis increased proportional to the contents of agar and acid. The relative formation ratio was high 10~47% for furfural (FUR) and 15~29% for hydroxy-methyl furfural (HMF) in 0.5~1.25% sulfuric acid rather than those of oxalic acid. When comparing the removal efficiency of the furans using an alkali treatment, steam stripping and hydrophobic resins, FUR was eliminated 60% by the alkali treatment, 62~90% by steam stripping and 71~75% by Amberlite XAD4 and 7HP, while HMF was removed to low levels of 10.5%, 4~17% and 13~25%, respectively. The loss of reducing sugar was also observed in process of the removal of furans, and the loss rate was the level of 2~4% in alkali treatment, 11~16% in steam stripping and 7~9% in Amberlite resins.

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Cell Culture Microbioassay for the Water Pollution Monitoring (세포배양 생화학적 기법에 의한 수환경오염 평가)

  • 오승민;정규혁
    • Toxicological Research
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    • v.16 no.4
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    • pp.285-291
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    • 2000
  • So far, investigation of environmental pollution has been achieved in field study. This remains the most exhaustive approach, current dimensions of environmental researches and their inherent complexity require that relatively inexpensive and simple laboratory procedures are developed to make possible the screening of large numbers of sites and samples. At this point. microbioassay has been high-lighted. The purpose of this study is to evaluate the water pollution using microbioassay. Two microbioassay methods were optimized and validated for the sensitive and quantitative determination of total toxic effects in the water. EROD(Ethoxyresorufin-O-deethylase) microbioassay was focused to detect PARs, PCBs and dioxinlike components in the water and E-screen assay to xenoestrogens. The EROD microbioassay was executed in rat hepatoma cell line, H4IIE and E-screen assay in MCF7-BUS cell line. Kumho river was selected for this study. 5ι of river water was extracted using combined solid-phase extraction in static adsorption mode with soxhlet extraction. Pollutants adsorbed to the XAD-4 resin were recovered by elution with ethyl acetate and methylene chloride (1 : 9). Toxic effects of extracts were determined by EROD-microbioassay and E-screen assay. EROD activities of water samples were 7.24-72.24 ng/ι MEQ. The estrogenic effect of various water samples is quantitatively evaluated by EEQ. The EEQ of samples range from 0.05 to 6.07 ng-EEQ/ι. These results suggested that Kumho river was highly polluted with organic toxic chemicals.

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Sensitive Determination of Alkylphenols, Chlorophenols, and Bisphenol A using GC/MS-SIM in Paper Materials (기체 크로마토그래피/질량분석기를 이용한 종이류 중 알킬페놀류, 클로로페놀류 및 비스페놀 A 정량)

  • Kim, Hyub;Kim, Jin-Ho
    • Environmental Analysis Health and Toxicology
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    • v.18 no.1
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    • pp.45-55
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    • 2003
  • The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrom-etry-selected ion monitoring (GC/MS-SIM) mode followed by two work-up methods for comparison; isoBOC derivatization method and TBDMS derivatization method. Eleven phenols in paper samples were extracted with acetonitrile. Also, solid -phase extraction (SPE) with XAD -4 and subsequent conversion to isobutoxycarbonyl derivatives or tert.-butyldimethylsilyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The SIM responses were linear with the correlation coefficient varying 0.9717 ∼ 0.9995 (isoBOC derivatization), and 0.9842 ∼ 0.9980 (TBDMS derivatization). The recoveries were 82.4 ∼ 108.8%) by area ratio of phenanthrene -d$\_$10/ vs bisphenol A-d$\^$l6/. (isoBOC derivatization and TBDMS derivatization) The range of concentrations was respectively, 0.95 ∼ 1.44 ng/g in 2,4-dichlorophenol, 1.01 ∼ 1.17 ng/g in t-butylphenol,2.17 ∼ 5.84 ng/g in pentachlorophenol, 12.68 ∼ 14.88 ng/g in nonylphenol and 30.84 ∼ 153.72 ng/g in bisphenol A.

Part-Per-Trillion Level Determination of Alkylphenols, Chlorophenols and Bisphenol A using GC/MS-SIM in Tap Water Samples (GC/MS-SIM 방법에 의한 수돗물 중 알킬페놀, 플로로페놀과 비스페놀 A의 ppt 정량)

  • Kim, Hyub
    • Environmental Analysis Health and Toxicology
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    • v.18 no.3
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    • pp.199-208
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    • 2003
  • A new technique was proposed for the determination of alkylphenols, chlorophenols and bisphenol A in tap water samples. The sample preparation consists of a solid phase extraction (SPE) of alkylphenols, chlorophenols and bisphenol A from a water sample with XAD-4 and subsequent conversion to isobutyloxycarbonyl (isoBOC) derivatives or tert-butyldimethylsilyl (TBDMS) derivatives for sensitive analysis with the CC/MS SIM mode. The recoveries were 86.6 ∼ 105.2% (isoBOC derivatization) and 97.6∼484.5% (TBDMS derivatization), respectively. The limit of quantitation of alkylphenols, chlorophenols and bisphenol h for SIM were 0.001∼0.050 $\mu\textrm{g}$/1 (isoBOC derivatization) and 0.003∼0.050 $\mu\textrm{g}$/1 (TBDMS derivatization). The SIM responses were linear with the correlation coefficient varying 0.9755∼0.9981 (isoBOC derivatization), and 0.9908∼0.9996 (TBDMS derivatization). When these methods were applied to tap water samples, the range of concentrations were 22.8∼31.3 ng/1 in 2,4-dichlorophenol, 28.6∼70.3 ng/1 in pentachlorophenol, 15.2∼17.4 ng/1 in t-butylphenol, 10.8∼13.2 ng/1 in t-octylphenol and 17.6∼36.3 ng/l in bisphenol A, respectively.

Application of Adsorption Sampling and Thermal Desorption with GC/MS Analysis for the Measurement of Low-Molecular Weight PAHs in Ambient Air (환경대기 중 저분자 PAHs 측정을 위한 흡착-열탈착-GC/MS 방법의 적용)

  • Seo, Seok-Jun;Seo, Young-Kyo;Hwang, Yoon-Jung;Jung, Dong-Hee;Baek, Sung-Ok
    • Journal of Korean Society for Atmospheric Environment
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    • v.30 no.4
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    • pp.362-377
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    • 2014
  • Polycyclic aromatic hydrocarbons (PAHs) have been of particular concern since they are present both in the vapor and particulate phases in ambient air. In this study, a simple method was applied to determine the vapor phase PAHs, and the performance of the new method was evaluated with a conventional method. The simple method was based on adsorption sampling and thermal desorption with GC/MS analysis, which is generally applied to the determination of volatile organic compounds (VOCs) in the air. A combination of Carbotrap (300 mg) and Carbotrap-C (100 mg) sorbents was used as the adsorbent. Target compounds included two rings PAHs such as naphthalene, acenaphthylene, and acenaphthene. Among them, naphthalene was listed as one of the main HAPs together with a number of VOCs in petroleum refining industries in the USA. For comparison purposes, a method based on adsorption sampling and solvent extraction with GC/MS analysis was adopted, which is in principle same as the NIOSH 5515 method. The performance of the adsorption sampling and thermal desorption method was evaluated with respect to repeatabilities, detection limits, linearities, and storage stabilities for target compounds. The analytical repeatabilities of standard samples are all within 20%. Lower detection limits was estimated to be less than 0.1 ppbv. In the results from comparison studies between two methods for real air samples. Although the correlation coefficients were more than 0.9, a systematic difference between the two groups was revealed by the paired t-test (${\alpha}$=0.05). Concentrations of two-rings PAHs determined by adsorption and thermal desorption method consistently higher than those by solvent extraction method. The difference was caused by not only the poor sampling efficiencies of XAD-2 for target PAHs and but also sample losses during the solvent extraction and concentration procedure. This implies that the levels of lower molecular PAHs tend to be underestimated when determined by a conventional PAH method utilizing XAD-2 (and/or PUF) sampling and solvent extraction method. The adsorption sampling and thermal desorption with GC analysis is very simple, rapid, and reliable for lower-molecular weight PAHs. In addition, the method can be used for the measurement of VOCs in the air simultaneously. Therefore, we recommend that the determination of naphthalene, the most volatile PAH, will be better when it is measured by a VOC method instead of a conventional PAH method from a viewpoint of accuracy.