• 제목/요약/키워드: XAD-4

검색결과 122건 처리시간 0.025초

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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    • 제12권3호
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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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    • 제67권
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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.

왕불류행의 Ecdysteroid성분 (Ecdysteroids from Melandrii Herba)

  • 김호경;전원경;고병섭
    • 약학회지
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    • 제45권5호
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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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XAD 수지분획에 의한 용존유기물질 특성 연구 (Study on the characterization of dissolved organic matters by XAD resin fractionation)

  • 박정민;허성남;임태효;신찬기
    • 환경위생공학
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    • 제22권4호
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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.

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

  • 정형석;박근형
    • 한국식품과학회지
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    • 제31권5호
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    • pp.1184-1187
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    • 1999
  • 치자황색소로부터 미생물에 의해 변환된 색소의 색조차이를 규명하고자 L. plantarum과 S. epidermidis에 의해 변환된 색소를 Amberlite XAD-4 column chromatography로 정제 한 다음 Sephadex LH-20 column의 gel filtration 용출양상과 분리된 색소의 분광학적 특성을 조사 하였다. L. plantarum에 의해 변환된 색소는 crocetin보다 큰 분자크기를 갖고 588 nm에서 홉수극대를 갖는 단일의 청색소를 생성하며, S. epidermidis에 의해 변환된 색소는 L. plantarum에 의해 생성되는 588 nm에 흡수극대를 갖는 청색소와 함께 crocetin 보다 작은 분자크기와, 413 nm에서 흡수극대를 갖는 황색소를 동시에 생성함으로서 청녹색을 띠는 것임이 밝혀졌다.

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

  • 이헌주;손영선;안동호;김현수;현형환
    • 한국미생물·생명공학회지
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    • 제20권2호
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    • pp.178-182
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    • 1992
  • Cephalosporium acremonium CSA-2.8A3 변이주로 부터 생성된 cephaloporin C를 정제하여 산업적 이용을 위해 ultrafiltration으로 균체를 제거하고 수종의 수지공정을 통하여 소디움염 형태의 cephalosporin C를 정제하였으며 역삼투막에 의한 농축과 분무건조를 행하였다. WA-30, HO-20, XAD-2000, SK-1B column chromatography를 통해 90% 이상의 높은 수율과 순도를 얻을 수 있었고, 특히 상기 수지들을 직렬로 연결하여 사용합으로써 수율은 96%까지 올릴 수 있었다.

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

  • 최진희;조지훈;최성봉;이권섭;신현화;양정선
    • 한국산업보건학회지
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    • 제19권4호
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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.

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

  • 양정선;최성봉;박상용;이성배
    • 분석과학
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    • 제25권5호
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    • pp.307-312
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    • 2012
  • 4급 암모늄 계열의 대표적인 살균제인 didecyldimethylammonium chloride(DDAC)는 흡입 경로에 의해 폐 섬유화 등의 폐질환을 일으킬 가능성이 높은 물질로, 흡입독성시험을 위하여 전신 흡입노출 챔버 내에 에어로졸 형태로 분무된 DDAC의 포집 및 분석방법을 검토하였다. DDAC의 포집 회수율은 아세토니트릴을 사용하여 탈착한 XAD 흡착제의 회수율이 87.8%로 실리카겔의 경우보다 우수한 것으로 나타났다. 이온크로마토그라프-전기전도도 검출기로 분석한 DDAC의 검출한계(MDL, method detection limit)는 0.18 ${\mu}g/mL$이었으며, 정량한계(LOQ, limit of quantitation)는 0.54 ${\mu}g/mL$였다. 공기 포집량 240 L를 기준으로 챔버 내 공기 중 농도로 환산하면 MDL이 2.97 ${\mu}g/m^3$, LOQ가 8.92 ${\mu}g/m^3$로, 챔버 내 발생 농도인 70~900 ${\mu}g/m^3$ 농도 수준의 모니터링에 적절하였다. 분석의 재현성은 0~20 ${\mu}g/mL$ 농도범위에서 상대오차 7.8% 내외였으며 시료 분석에 소요되는 시간은 5분 이내였다. 따라서 XAD를 사용한 DDAC의 포집 및 이온크로마토그라피를 이용한 분석방법은 실험동물을 사용한 전신 흡입노출 챔버 내 DDAC 농도의 신속하고 편리한 모니터링에 적절한 것으로 나타났다.

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) (Allelopathic Activity and Determination of Allelochemicals from Sunflower (Helianthus annuus L.) Root Exudates - 1. Allelopathic and Autotoxic Effects of Sunflower Root Exudates)

  • 박광호;;김순철;김길웅
    • 한국잡초학회지
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    • 제12권1호
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    • pp.52-60
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    • 1992
  • 해바라기의 타감작용(他感作用)(Allelopathy) 및 천연제초제(天然除草劑)로서의 개발가능성(開發可能性)에 관한 시험(試驗)을 1988-1991년(年)에 걸쳐 국제미작연구소(國際米作硏究所)(IRRI) : 농학(農學), 생화학부(生化學部) 및 국립(國立)필리핀 대학교(大學校) 화학과(化學科)(천연물(天然物) 연구실(硏究室))에서 수행(遂行)하여 얻은 결과중(結果中) 해바라기의 생육중(生育中) 뿌리에서 분비(分泌)되는 타감작용(他感作用) 및 자가억제작용(自家抑制作用)에 관(關)한 연구결과(硏究結果)는 다음과 같다. 1. 해바라기의 근분비물질(根分泌物質)은 대조구(對照區)에 비해 전체적인 발아율(發芽率)에는 유의적(有意的)인 차이(差異)가 인정되지 않았지만 발아시(發芽始)등에는 다소 큰 영향(影響)을 미쳤음. 2. 생물검정재료(生物檢定材料)의 지상부(地上部), 지하부(地下部) 생장(生長) 및 전체 생체중(生體重)에는 유의적인 감소(減少)가 있었음. 3. XAD-4 Resin올 부착한 시험(試驗) 3에서 해바라기는 대조구(對照區)에 비해 전반적인 생장량(生長量)이 많은 것으로 보아 자가억제작용(自家抑制作用)이 인정되었으며 이는 Resin에 의한 타감물질(他感物質)(Allelochemicals)의 판착효과(坂着效果)로 추정(推定)된다.

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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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    • 제6권1호
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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.