• Title/Summary/Keyword: XAD-4

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SENSITIVE DETERMINATION OF ELEVEN PHENOLIC ENDOCRINE-DISRUPTING CHEMICALS IN HUMAN URINE USING GAS CHROMATOGRAPHY/MASS SPECTROMETRY -SELECTED ION MONITORING

  • Kim, Hyub;Jang, Cheol-Hyeon
    • Environmental Engineering Research
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    • v.12 no.3
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    • pp.93-100
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    • 2007
  • I improved an analytical method for determining trace amounts of eleven phenolic endocrine-disrupting chemicals (11 phenolic EOCs) in human urine. The 11 phenolic EOCs were subjected to hydrolysis and then to solid phase extraction with a XAD-4 column. Alkylphenols, chlorophenols, and bisphenol A in XAD-4 column were eluted with acetonitrile, and the eluate was concentrated under a nitrogen stream, and then tert-butyldimethylsilylation. Separation and determination were done by gas chromatography, using mass spectrometry operating in the selective ion monitoring mode for quantitation. For tert-butyldimethylsily (TBDMS) derivatization the recoveries were $91.2{\sim}125.9%$, the limits of quantitation (LOQ) for the 11 phenolic EOCs in the nanogram-per-milliliter range ($0.025{\sim}1.000\;ng/mL$) were thus achieved by using 1 mL of urine, and the SIM responses were linear with the correlation coefficient varying by $0.9300{\sim}0.9943$. Based on the results for urine samples from unexposed individuals, 4-tert-octylphenol and pentachlorophenol were detected in hydrolysed urine sample. Other alkylphenols, chlorophenols and bisphenol A were not detected.

Utility of solid phase extraction for colorimetric determination of lead in waters, vegetables, biological and soil samples

  • Al-Mallah, Zakia;Amin, Alaa S.
    • Journal of Industrial and Engineering Chemistry
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    • v.67
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    • pp.461-468
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    • 2018
  • A highly sensitive, selective and rapid method for the determination of lead based on the reaction of lead (II) with 5-(4'-chlorophenylazo)-6-hydroxypyrimidine-2,4-dione (CPAHPD) and the solid phase extraction of the Pb(II)-CPAHPD complex with Amberlite XAD-2000 was developed, in the presence of pH 5.6 buffer solution and Triton X-114 medium. CPAHPD reacts with lead to form a violet complex with a molar ratio of 2:1 (CPAHPD to lead). This complex was enriched by the solid phase extraction with Amberlite XAD-2000. An enrichment factor of 500 was obtained by elution of the complex from the resin with a minimal amount of isopentyl alcohol(0.2 mL). In isopentyl alcohol medium,the molar absorptivity of the complex is $1.13{\times}10^6L\;mol^{-1}cm^{-1}$ at 647 nm. Beer's law is obeyed in the range of $5.0-160ng\;mL^{-1}$ in the measured solution. The relative standard deviation for 10 replicate samples of $50ng\;mL^{-1}$ level is 1.26%. The detection and quantification limits reaches 1.5 and $4.7ng\;mL^{-1}$ in the original samples. The presented procedure was successfully applied for determination of lead content in real samples such as vegetables, waters, biological and soil samples with satisfactory results.

Ecdysteroids from Melandrii Herba (왕불류행의 Ecdysteroid성분)

  • 김호경;전원경;고병섭
    • YAKHAK HOEJI
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    • v.45 no.5
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    • pp.455-459
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    • 2001
  • Melandrii Herba has been used for tympanitis, sore throat, dysentery and dehumidifying diuretic. From the BuOH fraction of methanol extracts, three ecdysteroids (ecdysterone, ecdysterone 22-acetate and inokosterone) were isolated by column chromatography using Amberlite XAD-4, ODS and Sephadex LH-20 gel and by HPLC method. The structures of these compounds were identified on the basis of spectroscopic methods.

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Study on the characterization of dissolved organic matters by XAD resin fractionation (XAD 수지분획에 의한 용존유기물질 특성 연구)

  • Park, Jeong-Min;Heo, Seong-Nam;Im, Tae-Hyo;Shin, Chan-Ki
    • Journal of environmental and Sanitary engineering
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    • v.22 no.4
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    • pp.23-32
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    • 2007
  • Changes in the characteristics of dissolved organic matter was studied at selected stations in the Nakdong river basin using physical and chemical methods. Characteristics of dissolved organic matters were analysed and assessed. Production of disinfection byproducts were also investigated. Distribution of the organic compounds according to the Molecular weight(MW) indicate that MWs higher than 100K were highest with cattle excrement wastewater and MW between 100-10K were highest with waters from forest streams. Low MW compounds (Jess than 1K) were highest with the effluents from environmental facilities. Results of resin fractionation study show that acidic hydrophobic substances(AHS) were dominant in many stations. The values were higher in the samples from mainstreams and sidestreams where the influence of organic matter is higher than the water from environmental facilities. Hydrophilic neutral substances(HoN) such as hydrocarbon, pesticides and detergents were higher in the wastewater treatment facilities. HoN values of water from the forest streams were 4.7% indicating there is no synthetic pollutant.

Conversion Patterns of Yellow Pigment from Gardenia jasminoides by Staphylococcus epidermidas and Lactobacillus plantarum (Staphylococcus epidermidas와 Lactobacillus plantarum에 의한 치자황색소의 변환양상)

  • Jeong, Hyung-Seok;Park, Keun-Hyung
    • Korean Journal of Food Science and Technology
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    • v.31 no.5
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    • pp.1184-1187
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    • 1999
  • The Gardenia jasminoides yellow pigment and converted pigments were completely separated by Amberlite XAD-4 column chromatography. These Pigments were gel filtrated on Sephadex LH-20 column chromatography. The characteristics of absorption spectra of eluate and fractionated pigments were investigated. The pigment converted by Lactobacillus plantarum showed a single blue color with an absorption peak at 588 nm and its molecular size was bigger than that of crocetin. The pigment, converted by Staphylococcus epidermidis, Showed blue-green color, which was composed of yellow color with an absorption peak at 418 nm and blue color at 588 nm. Molecular size of the yellow pigment was smaller than crocetin and that of blue color.

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Purification of Cephalosporin C Produced by Cephalosporium acrernoniurn (Cephalosporium acremonium 변이주가 생성하는 Cephalosporin C의 정제)

  • 이헌주;손영선;안동호;김현수;현형환
    • Microbiology and Biotechnology Letters
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    • v.20 no.2
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    • pp.178-182
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    • 1992
  • For an industrial-scale purification and production of cephalosporin C from a culture broth of Ceplzalos#mium nmemonium CSA-2.8A3 mutant, ultrafiltration, column chromatography, reverse osmosis, and spray drying were empolyed. Above 90% of yield and high purity of cephalosporin C were obtained through WA-30, HP-20, XAD-2000 and SK-1B column chromatographies. Especially, in the tendom operation of the columns, the recovery yield was increased up to 96%. The purified cephalosporin C was stable at $4^{\circ}C$ and in acidic condition, while it was unstable at room temperature and in alkaline condition at pH above 8.0. Cephalosporin C powder or a final product prepared by spray drying contained 85.554 of sodium cephalosporin C, 6.3%' of water, 4.63% of free $Na^+$ ions. and traces of metal ions.

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Study on desorption efficiency of naphthalene by adsorbing media and desorbing solvent (흡착관과 탈착용매에 따른 나프탈렌의 탈착효율에 관한 연구)

  • Choi, Jin Hee;Jo, Jihoon;Choi, Seong Bong;Lee, Kwon Seob;Shin, Hyun Hwa;Yang, Jeong Sun
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.19 no.4
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    • pp.403-411
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    • 2009
  • This study was performed to propose appropriate conditions suited to the analysis of naphthalene by comparing desorption efficiencies under various conditions. 1. As to influence by adsorbing media and desorbing solvent on desorption efficiency of naphthalene, when adsorbed by CCT, o-xylene gave the highest desorption efficiency of $73.96{\pm}0.53%$ while the lowest of $1.14{\pm}0.03%$ desorbed by ether. Both XAD-2 and Chromosorb 106 showed around 90% of desorption efficiencies for each solvent, especially desorption efficiencies more than 95% were achieved when adsorbed by Chromosorb 106 and desorbed by $CS_2$ or o-xylene. 2. Desorption efficiencies descended over the storage period in any condition(p<0.05). For all three adsorbing media, while desorption efficiencies showed no significant difference(p>0.05) between room temperature and refrigeration a day of loading, samples kept in room temperature had higher desorption efficiencies than refrigerated ones in 7 and 14 days with significant difference(p<0.05).Also, desorption efficiencies dropped drastically in 7 days, from that point the decreasing tendency went mild. 3. When respective 1 TLV and 0.1 TLV of naphthalene were spiked on CCT and desorbed by CS2($46.45{\pm}0.59%$ vs. $30.15{\pm}0.81%$), o-xylene($73.96{\pm}0.53%$ vs. $67.51{\pm}1.34%$), and ether($1.14{\pm}0.03%$ vs. N.D.) desorption efficiencies increased as the amount of loading increased(p<0.05).On the other hand, naphthalene spiked on XAD-2 and Chromosorb 106 indicated no significant difference(p>0.05) in desorption efficiencies between 1 TLV and 0.1 TLV. In conclusion, in order for favorable desorption efficiencies of naphthalene it is important to select appropriate adsorbing media and desorbing solvent accordingly. The result revealed that adsorbing media of XAD-2 and Chromosorb 106 outperformed CCT and desorbing solvents of $CS_2$ and o-xylene achieved over 90% of desorption efficiencies when adsorbed on XAD-2 and Chromosorb 106. Also, considering the tendency that desorption efficiencies of naphthalene decrease with time, the samples should be analyzed as soon as possible.

Analysis of didecydimethylammonium chloride (DDAC) aerosol in inhalation chamber (흡입챔버 내 didecyldimethylammonium chloride(DDAC) 에어로졸의 분석)

  • Yang, Jeong-Sun;Choi, Sung-Bong;Park, Sang-Yong;Lee, Sung-Bae
    • Analytical Science and Technology
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    • v.25 no.5
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    • pp.307-312
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    • 2012
  • To perform inhalation toxicity test by using experiment animals, we set up an analytical method to monitor didecyldimethylammonium chloride (DDAC) in aerosol nebulized into inhalation chambers by ion chromatography. DDAC was adsorbed by XAD-2 resin and analyzed with conductivity detector. Recovery of DDAC desorbed by acetonitrile from XAD adsorbent was 87.8%. The method detection limit (MDL) and the limit of quantitation (LOQ) were 2.97 ${\mu}g/m^3$ and 8.92 ${\mu}g/m^3$, respectively. Repeatability was calculated as RSD 7.8% in the range of 0~20 ${\mu}g/mL$. Time needed to analyze a sample was less than 5 minutes. Therefore, the analysis of DDAC by ion chromatography was practically useful in monitoring DDAC in inhalation chambers with rapidity and sensitivity manner to perform inhalation toxicity test using experimental animals.

Allelopathic Activity and Determination of Allelochemicals from Sunflower (Helianthus annuus L.) Root Exudates - 1. Allelopathic and Autotoxic Effects of Sunflower Root Exudates (해바라기(Helianthus annuus L.) 근분비물질(根分泌物質)의 타감작용(他感作用) 및 타감물질(他感物質)의 동정(同定) - 1. 해바라기 근분비물질(根分泌物質)의 타감작용(他感作用) 및 자가억제작용(自家抑制作用))

  • Park, K.H.;Moody, K.;Kim, S.C.;Kim, K.U.
    • Korean Journal of Weed Science
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    • v.12 no.1
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    • pp.52-60
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    • 1992
  • There was no significant difference in the final germination percentages(Experiment 1-3) as affected by sunflower root exudates between the control and the treated for the test species. In general(Experiment 1), however, germination onset was delayed the treated bottles. Germination rate was, also, reduced for both radish(Raphanus sativus L.) and rice(Oryza sativa L.). Therefore, the germination index was low in the treated bottles but germination gradually increased with time in the greated bottles in all test species so that the final germination percentages were similar between treatments. The root exudates of sunflower had significant inhibitory effects(Experiment 1-3) on the lengths of the shoots and roots of all the test species. Fresh weight was also significantly reduced in all test species. Sunflower seedlings(Experiment 3) in the treated(with the XAD-4 resin column) were larger and healthier than those in the control (without XAD-4 resin column) because of the removal of allelochemicals. The fresh weight of sunflower seedlings was markedly inhibited by sunflower root exudates. These mean that sunflower probably is an autotoxic crop.

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Group Separation of Water-soluble Organic Carbon Fractions in Ash Samples from a Coal Combustion Boiler

  • Park, Seung-Shik;Jeong, Jae-Uk;Cho, Sung-Yong
    • Asian Journal of Atmospheric Environment
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    • v.6 no.1
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    • pp.67-72
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    • 2012
  • The chemical characterization of water-soluble organic carbon in ash emitted from a coal combustion boiler has not been reported yet. A total of 5 ash samples were collected from the outlet of an electrostatic precipitator in a commercial 500 MW coal-fired power plant, with their chemical characteristics investigated. XAD7HP resin was used to quantify the hydrophilic and hydrophobic water-soluble organic carbons (WSOC), which are the fractions of WSOC that penetrate and remain on the resin column, respectively. Calibration results indicate that the hydrophilic fraction includes aliphatic dicarboxylic acids and carbonyls (<4 carbons), amines and saccharides, while the hydrophobic fraction includes aliphatic dicarboxylic acids (>4-5 carbons), phenols, aromatic acids, cyclic acid and humic acid. The average mass of the WSOC in the ash samples was found to depend on the bituminous coal type being burned, and ranged from 163 to 259 ${\mu}g$ C/g of ash, which corresponds to 59-96 mg C of WSOC/kg of coal combusted. The WSOC mass accounted for 0.02-0.03 wt% of the used ash sample mass. Based on the flow rate of flue gas produced from the combustion of the blended coals in the 500 MW coal combustion boiler, it was estimated that the WSOC particles were emitted to the atmosphere at flow rates of 4.6-7.2 g C/hr. The results also indicated that the hydrophilic WSOC fraction in the coal burned accounted for 64-82% of the total WSOC, which was 2-4 times greater than the mass of the hydrophobic WSOC fraction.