• Title/Summary/Keyword: XAD-2

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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.

Determination of 11 Phenolic Endocrine Disruptors using Gas Chromatography/Mass Spectrometry-Selected Ion Monitoring in Five Selected Wastewater Influents

  • Kim, Hyub
    • Environmental Engineering Research
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    • v.13 no.4
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    • pp.216-223
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    • 2008
  • An efficient method for the simultaneous determination of eleven phenolic endocrine-disrupting chemicals (EDCs) present in wastewater influent samples was described. The 11 phenolic EDCs including alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) following two work-up methods for comparison; isobutoxycarbonyl (isoBOC) derivatization and tert-butyldimethylsilyl (TBDMS) derivatization. The wastewater influent samples containing the 11 EDCs were adjusted to pH 2 with $H_2SO_4$ and then cleaned up with n-hexane. Next, they were subjected to solid-phase extraction (SPE) with XAD-4 resin and subsequently converted to isoBOC or TBDMS derivatives for sensitivity analysis with gas chromatography/mass spectrometry-selected ion monitoring (GC/MSSIM). Following isoBOC derivatization and TBDMS derivatization, the recoveries were 86.6-105.2% and 97.6-142.7%, the limits of quantitation (LOQ) for the 11 phenolic EDCs for SIM was 0.001-0.050 ng/mL and 0.003-0.050 ng/mL, and the SIM responses were linear with the correlation coefficient varying by 0.9717-0.9995 and 0.9842-0.9980, respectively. When these methods were applied to five selected wastewater influent samples, for isoBOC derivatization and TBDMS derivatization the ranges of concentration detected were 0.2-99.6 ng/mL and 0.4-147.4 ng/mL, respectively.

Exposure Assessment to Asbestos and Diesel Engine Exhaust Particulate Matter in Urban Bus Garage (버스 정비 작업자에 대한 석면 및 디젤 엔진 배출물질 노출 평가)

  • Lee, Naroo;Yi, Gwangyong
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.26 no.2
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    • pp.219-224
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    • 2016
  • Objectives: Lung cancer occurred with worker working in an urban bus garage. A survey was conducted to investigate whether lung cancer had causal relationship with work. Exposure to asbestos and diesel engine exhaust were suspected. Methods: Airborne asbestos was sampled on membrane filter and analyzed using phase-contrast microscopy. Airborne diesel exhaust was sampled using quartz filter and analyzed with thermal-optical analyzer. Polynuclear aromatic hydrocarbons was sampled using PTFE filter and XAD-2 tube and analyzed with gas chromatography-mass selective detector. Results: Airborne asbestos concentration was under 0.01 fiber/cc. Worker who warmed up an engine of urban bus for 2 hours was exposed to elemental carbon concentration, $15.5{\mu}g/m^3$. Only naphtalene among polynuclear aromatic hydrocarbons was detected. Conclusions: It was difficult to conclude about worker exposure to asbestos because working hour related asbestos was too short. In reviewing papers, the exposure to asbestos over 0.01 fiber/cc during exchange brake lining was found. It was identified that worker's occupational exposure to diesel exhaust based on elemental carbon was higher than the other occupational exposure to diesel exhaust.

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.

Characterization of an Elastase Inhibitor Produced by Streptomyces lavendulae SMF11

  • Lee, Hyun-Sook;Jin, Wook;Kang, Sung-Gyun;Hwang, Yoon-Sook;Kho, Yung-Hee;Lee, Kye-Joon
    • Journal of Microbiology and Biotechnology
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    • v.10 no.1
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    • pp.81-85
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    • 2000
  • An elastase inhibitor, SMFEI02, was isolated from culture broth of Streptomyces lavendulae SMF11. The inhibitor was purified by ultrafiltration followed by XAD-7 column and Dowex-1 anion-exchange chromatographies, and preparative HPLC. The molecular formula was determined to be $C_{14}H_{16}N_2O_2$ (MW244) by HRFAB-MS analysis. The inhibitor was identified to be a diketopiperazine cyclo(S-Phe-S-Pro) by the optical rotation value and MNR spectral data, and showed inhibitory activities for trypsin, chymotrypsin, cathepsin B, and papain as well as elastase with the Ki values ranging from 1.78mM to $2.86{\;}\mu\textrm{m}$. The inhibition showed a competitive mode for elastase, chymotrypsin, and cathepsin B, whereas it showed a noncompetitive mode for trypsin and papain.

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Isolation of Herbicidal Compounds from Pulsatilla koreana Roots (백두옹(Pulsatilia koreana Nakai) 뿌리로부터 제초활성물질의 분리)

  • 정형진
    • Korean Journal of Plant Resources
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    • v.9 no.1
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    • pp.47-54
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    • 1996
  • To search herbicidal compounds in Pulsatilla koreana Nakai, methanol extract of P. koreana roots was purified by sequences of XAD-7 column chromatography, silica gel adsorption column chromatography, silica gel flash column chromatography, preparative layer chromatography and preparative high performance liquid chromatography(Prep, HPLC).The final Prep. HPLC gave two herbicidally-active fractions. These fractions treatment at 100ppm inhibited the root length of Echinochloa crus-galli seedlings by 48% and 60% as compared with the control, respectively. Components in the two active fractions were analyzed by GC-MS Spectrometry. These compounds, which were isolated from P. koreana roots, were identified as several fatty esters, hydrocarbons, squalene, evidonol, and a diazepin analogue.

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Constituents of Sanguisorba hakusanensis Leaves (산오이풀 잎의 성분)

  • Kwon, Won-Jun;Whang, Wan-Kyunn;Kim, Il-Hyuk
    • YAKHAK HOEJI
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    • v.40 no.3
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    • pp.262-272
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    • 1996
  • The constituents of Sanguisorba hakusanensis leaves (Rosaceae), of which the roots have been used as an astringent, hemostatics and antiphlogistics, were studied phytoche mically. From water fraction of the MeOH extract, gallic acid 3-O-${\beta}$-D-(6'-O-galloyl)-glucopyranoside(I), quercetin-3-O-${\beta$-D-galactopyranoside(II), quercetin-3-O-${\alpha}$-L-arabinopyranoside(III) and $2{\alpha},\;3{\beta},\;19{\alpha}$, 23-tetrahydroxyurs-12-en-28-oic acid 28-O-${\beta}$-D-glucopyranoside(IV) were isolated by column chromatographic separation using Amberlite XAD-2, ODS-gel and Sephadex LH-20. The structure of these compounds were elucidated by spectroscopic parameters of $^1H$-NMR, $^{13}C$-NMR, $^1H-^1H$ COSY, $^{13}C-^1H$ COSY, EI-Mass, FAB-Mass, IR, UV and by comparison with authentic samples.

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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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Identification of an antagonistic bacteria and its antibiotic substance against Colletotrichm orbiculare causing anthracnose on cucumber

  • Chae, Hee-Jung;Moon, Surk-Sik;Ahn, Jong-Woong;Chung, Young-Ryun
    • Proceedings of the Korean Society of Plant Pathology Conference
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    • 2003.10a
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    • pp.102.1-102
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    • 2003
  • A bacterial strain YC4963 with antifungal activity against Colletotrichum orbiculare, a causal organism of cucumber anthracnose was isolated from the rhizosphere soil of Siegesbeckia pubescens (Siegesbeckia pubescens Makino;Family:Compositae) in Korea. Based on physiological and biochemical characteristics and 16S ribosomal DNA sequence analysis, the bacterial strain was identified as Pseudomonu aureofaciens. The bacteria also inhibited mycelial growth of several plant fungal pathogens such as Botrytis cinerea, Fusarium oxysporum and Rhizoctonia solani on PDA and 0.1 TSA media. The antibiotic activity was found from the culture filtrate of TSB(tryptic soy broth) and its active compounds were quantitatively bound to XAD adsorber resin. The antibiotic spectrum was broad and growth of C. orbiculare and F. oxysporum, B. cinerea were inhibited at very low concentration. The chemical data from various chromatographic procedures showed that active fraction consisted of at least two phenazine derivatives. However, the metabolites had no inhibitory effect on Pythium ultimum which was reported to be sensitive to phenazine antibiotics. The compounds responsible for the activity are now under investigation.

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Escherichia coli에서 발현된 재조합 인간 상피세포 증식인자의 정제 및 특성

  • 박세철;유광현
    • Microbiology and Biotechnology Letters
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    • v.24 no.4
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    • pp.478-484
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    • 1996
  • Recombinant human epidermal growth factor (rhEGF) was produced by E. coli BL21 harboring a plasmid pYHB101. The maximum production was 68.7 mg/l when the E. coli strain was cultured at 25$\circ$C for 48 hours in the modified MBL medium containing 10 g/l glucose with 1 mM IPTG induction at 2 hours after inoculation. The rhEGF was purified upto 267 folds by Amberlite XAD- 7 chromatography, ultrafiltration, and DEAE Sepharose fast flow ion exchange chromatography with an overall yield of 66.6%. The purified rhEGF was further separated into two fractions by HPLC. The N-terminal amino acid sequence of the second fraction was Asn-Ser-Asp-Ser-Glu-Cys-Pro-Leu-Ser-His. The effect of rhEGF on the DNA synthesis was examined using in vitro biological assay based on the incorporation of 5'-bromo-2'- deoxy-uridine (BrdU). The purified rhEGF shows no difference with natural human epidermal growth factor (nhEGF) in N-terminal amino acids residues and biological activity. From the results, we concluded that rhEGF produced from E. coli harboring the plasmid pYHB101 was apparently the same as nhEGF.

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