• Title/Summary/Keyword: trimethylsilyl

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Studies on Phytotoxin in Intensively Cultivated Upland Crops -I. Identification of phytotoxin in soil and effects of phytotoxin application to the toxicity of hot-pepper plant (연작재배지토양(連作栽培地土壤)의 식물독소(植物毒素)에 관(關)한 연구(硏究) -제(第)1보(報) 토양중(土壤中) 식물독소(植物毒素)의 분리정량(分離定量) 및 식물독소(植物毒素) 첨가(添加)가 고추 유식물(幼植物)에 미치는 영향(影響))

  • Lee, Sang Kyu;Suh, Jang Sun;Kim, Young Sig;Park, Jun Kyu
    • Korean Journal of Soil Science and Fertilizer
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    • v.20 no.1
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    • pp.63-67
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    • 1987
  • A laboratory experiment was conducted to find out the concentration of phytotoxin in intensively cultivated hot-pepper, garlic and chinese cabbage, and effects of these phytotoxin to the germination and growth of young hot-pepper plant. Also this experiment presents describes of the bio-assay method and results of phytotoxin application to the toxicity of hot-pepper plant. The results obtained were summarized as follows; 1. A series of non-volatile (aromatic) phenolic compounds such as hydroquinone, benzoic-, p-hydroxybenzoic, and vanillic acid were quantitatively and qualitatively analysed using BSA(N, O-bis(trimethylsilyl)acetamide) by means of gas chromatography method. 2. Phytotoxin as hydroquinone, benzoic-, p-hydroxybenzoic- and vanillic acid were determined in intensively cultivated hot- pepper, garlic and chinese cabbage. Highest concentration of phytotoxin was obtained in hot-pepper cultivated soil. 3. Direct toxic action of the applied phytotoxin to the germination and young hot-pepper plant growth was observed at the levels of 200 ppm. Benzoic acid was obtained the highest toxicity to the young hot-pepper plant growth. 4. Mode of actions of phytotoxins to the young hot-pepper plant growth were observed as stunting of stem elongation, discoloration of leaf and oxygen depletion from consideration as causes of symptom.

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Studies on the Removal of Volatile Organic Compounds in Wastewater using PTMSP/PDMS-PEI Composite Membrane by Pervaporation (PTMSP/PDMS-PEI 복합막을 이용한 폐수중의 휘발성 유기화합물 제거에 관한 연구)

  • Kweon, Chang-Oh;Paik, Gwi-Chan;Chun, Kyung-Soo
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.12 no.8
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    • pp.3532-3540
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    • 2011
  • In order to improve flux of PTMSP/PDMS dense membrane, PTMSP/PDMS-PEI composite membrane with PEI support was prepared by phase inversion process and dip coating. These membranes were evaluated in terms of the removal of volatile organic compounds such as PCE, TCE, chloroform, 1,1,1-trichloroethane from wastewater by pervaporation. The selectivity and flux of PTMSP/PDMS dense membranes was in the range of 216.2 to 2394.4 and 244.3 to 428.2g/m2h, respectively. And pervaporation property of PTMSP/PDMS-PEI composite membrane was in the range of 215.5 to 2404.2 and 390.4 to 728.6g/m2h, respectively. PTMSP/PDMS-PEI composite membrane has remarkably greater flux than dense membranes with similar selectivity. It was possible for polymeric membranes used in this study to remove PCE selectively which is dissolved small quantity in water among other separable solutes. PTMSP/PDMS-PEI composite membrane showed the best performances among the silicone polymeric membranes, and has better durability and mechanical strength than dense membranes. PTMSP/PDMS-PEI composite membrane should be a useful candidate for the removal of volatile organic compounds dissolved in wastewater.

Simultaneous Determination of Urinary Phytoestrogens and Estrogens by Gas Chromatography/Mass spectrometry (GC/MS에 의한 뇨 중 Phytoestrogen과 Estrogen의 동시 분석)

  • Yang, Yoon Jung;Lee, Seon Hwa;Chung, Bong Chul
    • Analytical Science and Technology
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    • v.11 no.5
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    • pp.374-385
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    • 1998
  • Phytoestrogens are biologically active compounds derived from plants foods. It had been suggested that phytoestrogens, by inhibiting aromatase in peripheral and/or cancer cells and lowering estrogen levels, may play a protective role as antipromotional compounds during growth of estrogen-dependent cancers. Therefore, simultaneous analysis of estrogens and phytoestrogens is necessary to elucidate the possible involvement of phytoestrogens in estrogen metabolism. In this view, we developed a simple and reproducible procedure to quantitatively determine estrogen and phytoestrogen metabolites. The proposed method consisted of solid phase extraction using preconditioned Serdolit AD-2 resin, enzyme hydrolysis with ${\beta}$-glucuronidase/arylsulfatase from Helix pomatia, liquid-liquid extraction and TMS-ether derivatization. And the final determination was carried out by gas chromatography/mass spectrometry (GC/MS) in selected ion monitoring mode (SIM). The precision and accuracy of this method was evaluated through within-a-day and day-to-day test. Recovery range and detection limit were 71.96~105.66%, 2~4 ng/mL, respectively. Using this method, 17 estrogen and 5 phytoestrogen compositions in urine of normal subjects were analyzed. It was found that amounts and relative distribution of urinary phytoestrigens and estrogens showed different pattern in male and female subjects.

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Analysis of ambers with different origin by IR and py/GC/MS (산지별 호박(amber)의 IR 및 py/GC/MS 특성 분석)

  • Park, Jong-Seo;Lim, Yu-Jin
    • Analytical Science and Technology
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    • v.24 no.4
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    • pp.256-265
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    • 2011
  • Ambers have been used as a gemstone and a religious object since the ancient times and found in several archaeological sites in Korea. To prepare an enhanced conservation measures, we surveyed the chemical and spectroscopic properties of the ambers according to the provenance. Total 14 amber samples were collected from 6 different provenances including Baltic, Chiapas, Colombian, Dominican, Fushun and Madagascar amber. Infrared (IR) spectroscopic analysis was conducted for the non-destructive examination of the amber samples. They were also analyzed with pyrolysis/GC/MS (py/GC/MS) at the pyrolysis temperature of $300^{\circ}C$ with the on-line derivatization to trimethylsilyl ester. Baltic shoulder corresponding to the absorption at $1250cm^{-1}{\sim}1150cm^{-1}$ appeared in the IR spectrum of Baltic amber. IR spectra of the other ambers also showed somewhat distinctive characteristic peaks. In py/GC/MS analysis peaks assignable to succinic acid, dehydroabietic acid and pimaric acid were detected, which are known to be the components of the amber. In the meanwhile, the presence of compounds appearing in certain amber will be applied to differentiate the provenances of amber relics if their fragments are available for the analysis. These results are expected to help the confirmation of archaeological amber relics and archaeometric interpretation of provenances and manufacturing techniques.

Pretreatment method of urinary thiodiglycolic acid as metabolite of vinyl chloride (염화비닐의 요중 대사물질인 thiodiglycolic acid의 분석을 위한 전처리 조건)

  • Hong, Joo Youn;Kim, Chi Nyon;Jung, Jae Hoon;Chang, Jung Hwan;Roh, Jaehoon
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.9 no.1
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    • pp.23-40
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    • 1999
  • The analysis of thiodiglycolic acid in urine has been used as an index of biological exposure to vinyl chloride. Unfortunately thiodiglycolic acid has a strong hydrophilic character, because it has two carboxylic groups, so that it can only be extracted with organic solvent with a great difficulty. Underivatized thiodiglycolic acid tends to tail because of non-specific interaction with the inert support. Therefore, esterification is the obvious first choice for derivatization of thiodiglycolic acid, particularly for gas chromatography. In this study, the focus of interest is to compare two method of esterifications (methylation and silylation). Methylation is to make the methyl ester of thiodiglycolic acid by reaction with diazomethane. Silylation is to make the trimethylsilyl ester of thiodiglycolic acid by reaction with N-trimethylsily-ldiethylamine. The results and conclusions are as the following: 1. The detection limit (sensitivity) of methylated thiodiglycolic acid was $5.00{\mu}g/m{\ell}$ and silylated thiodiglycolic acid was $3.07{\mu}g/m{\ell}$ by gas chromatography with flame ionization detector. 2. The optimal liquid-liquid extraction of thiodiglycolic acid was as following: To each of the tubes, $15m{\ell}$ of urine, concentrated sulfuric acid (pH 1 - 2) and 5 gsodium sulfate were added. The samples was extracted three times with $5m{\ell}$ ethylacetate each time. 3. The methylated thiodiglycolic acid was more stable than silylated thiodiglycolic acid in extractional solvent which contained humidity. 4. The precision (pooled coefficient of variation for 4 days) of the analysis was 0.07324 in methylated thiodiglycolic acid with external standard calibration, and 0.07033 in methylated thiodiglycolic acid with internal standard calibration. 5. The precision (pooled coefficient of variation for 4 days) of the analysis was 0.10914 in silylated thiodiglycolic acid with external standard calibration, and 0.13602 in silylated thiodiglycolic acid with internal standard calibration. From the above results, the analysis of methylated thiodiglycolic acid was more sensitive (limit of detection) than silylated thiodiglycolic acid by gas chromatography. However, the methylated thiodiglycolic acid was stable in the humidity and was separated sharply on chromatogram. Also, analysis of methylated thiodiglycolic acid was more precise (pooled coefficient of variation for 4 days) than silylated thiodiglycolic acid. In conclusion, it is established that the analysis of methylated thiodiglycolic acid is appropriate for biological monitoring of exposure to vinyl chloride.

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Structure Analysis of Water-soluble Polysaccharides Extracted from The Unripe Fruit of Cudrania tricuspidata (꾸지뽕나무 열매에서 추출한 수용성 다당류의 구조분석)

  • Kim, Seok Ju;Lee, Kyung-Tae;Youe, Won-Jae;Lee, Sung-Suk;Kim, Yong Sik
    • Journal of the Korean Wood Science and Technology
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    • v.42 no.6
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    • pp.740-746
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    • 2014
  • The unripe fruit of cudrania tricuspidata was extracted with 50% ethanol. The crude water-soluble extracts were separated by liquid-liquid separation with n-hexane, ethyl acetate and butanol followed by precipitation with ethanol, and then the water-soluble polysaccharide (F1) was isolated by the fractionation through gel permeation chromatography using preparative PLaquagel-OH column with water. The structure was characterized by monosaccharide composition with HPAEC-PAD, methylation analysis with GC-MS, FT-IR and HPLC. According to the data, F1 was com posed of glucose (22.84 mM), galactose (13.75 mM), arabinose (45.87 mM), xylose (7.49 mM). It was revealed which uronic acid and acetyl group were not attached in F1. And it is constituted of 1-linked arabinose, 1,4-linked arabinose, 1,3-linked glucose, 1,4-linked galactose, 1,4-linked glucose, 1,3,6-linked galactose, 1,3,6-linked glucose and the ratio was showed 1.1 : 1.0 : 4.9 : 7.5 : 3.0 : 3.1 : 1.4 : 1.5.

Comparison of the Analytical Method for 3-Monochloropropane-l,2-diol in Food (식품 중 3-monochloropropane-1,2-diol의 분석법 비교 연구)

  • Yoo, Seung-Seok;Oh, Chang-Hwan
    • Korean Journal of Food Science and Technology
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    • v.39 no.4
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    • pp.360-365
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    • 2007
  • The studies for the derivatization of 3-monochloropropane-1,2-diol (3-MCPD) were performed mainly as acylation with HFBI (heptafluorobutyrylimidazole), alkylation with PBA (phenylboric acid) and silylation with BSTFA (N,O-bis[trimethylsilyl]trifluoroacetamide). Also silylation with MTBSTFA(N-methyl-N-[tert.-butyldimethylsilyl] trifluoroacetamide) and acylation with MBTFA (N-Methyl-bis[trifluoro-acetamide]) were also considered. Except the TBDMS derivative of 3-MCPD, all the derivatives were detected well. The derivatives of 3-MCPD with HFBI, PBA and BSTFA showed below 10 ${\mu}g/kg$ which was sensitive enough to satisfy Korea maximum residue limit 0.3 mg/kg. Among the tested adsorbents, Extrelut20 and Florisil were evaluated as the proper adsorbents to eliminate the soy sauce matrix for 3-MCPD. Ethyl acetate was the most efficient eluent with good recovery rate. The desired surrogate compound and internal standard were 1,2-butanediol and 1,2-dibromo-3-chloropropane, respectively. The limit of detection for PB-MCPD and TMS-MCPD were 10.16 and 7.06 ${\mu}g/kg$ on GC/MSD, respectively. HFB-MCPD derivative showed the lowest detection limits 2.98 and 5.32 ${\mu}g/kg$ by GC/ECD and GC/MSD, respectively.

Changes of Some Physicochemical Properties of Yoghurt made from ${\beta}$-Galactosidase-treated Commercial Milks (${\beta}$-Galactosidase 처리 시유로 제조한 요구르트의 이화학적 성분 변화)

  • Lee, In-Seon;Kim, Sang-Hee;Ha, Jae-Ho;Kang, Kook-Hee
    • Korean Journal of Food Science and Technology
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    • v.21 no.6
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    • pp.795-799
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    • 1989
  • This study was carried out to hydrolyze lactose in commercial milk by ${\beta}-galactosidase$ from Kluyveromyces fragilis and to compare some physicochemical properties of yoghurts made from control and lactase-treated commercial milks. Quantitative analysis of sugars was performed by gas liquid chromatograph (GLC) on trimethylsilyl (TMS) derivatives. In commercial milk, 94.6% of lactose was hydrolyzed after 2 hours incubation at $40^{\circ}C$ with 6.0 units/ml of ${\beta}-galactosidase$. pH, titratable acidity and viable cell number of yoghurt made from lactase-hydrolyzed (LH) commercial milk were 4.1, 1.04% and $6.5{\times}10^8/ml$ of Str. thermophilus, $8.9{\times}10^8/ml$ of L. bulgaricus after 8 hours incubation at $40^{\circ}C$, respectively, The total contents of amino acid were 2.63% in control and 2.19%. in LH yoghurt. The total contents of free amino acid were 26.95 mg% in control and 17.55mg% in LH yoghurt. Analysis of free fatty acids resulted in that the contents of short chain fatty acids in LH yoghurt were a little higher than those in control. Both in control and LH yoghurt, the palmitic acid content was highest and that was followed by oleic and myristic acid.

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Homolytic Reactions of Isonitriles (이소니트릴의 자유라디칼반응)

  • Sung Soo Kim
    • Journal of the Korean Chemical Society
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    • v.24 no.3
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    • pp.250-258
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    • 1980
  • Various radicals may add to isonitriles to give imidoyl radcals RN=CR'. This may be also generated via abstraction of imidoyl hydrogen from imine in the following manner: RN=CR' + R"${\cdot}{\rightarrow}$ RN=CR' + R"-H Imidoyl radicals would be stabilized via two pathways, ${\beta}$-cleavage and atom transfer reactions. ${\beta}$-Cleavage may occur in two directions depending upon structure of the radicals. Cyanide transfer and the "so-called" normal ${\beta}$-cleavage are the two modes of ${\beta}$-cleavage. Addition of t-butoxy radical to t-butyl isocyanide 7 generates an imidoyl radical t-Bu-N=C-O-Bu-t, which undergoes ${\beta}$-cleavage to give t-butyl isocyanate and t-butyl radical. Addition of phenyl radical to 7 forms the intermediate radical t-Bu-N=$C-C_6H_5$, which decomposes to give benzonitrile and t-butyl radical. The t-butyl radical generated from the ${\beta}$-cleavage adds to 7 giving the radical t-Bu-N=C-Bu-t, which cleaves only to pivalonitrile and t-butyl radical, inducing radical chain isomerization. Trimethylsilyl radical adds to 7 to give the intermediate t-Bu-N=$C-Si(CH_3)_3$, which collapses to $(CH_3)_3$SiCN and a t-butyl radical.

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Separation of Hydrogen-Nitrogen Gases by PTMSP/PDMS-Borosilicate Composite Membranes (PTMSP/PDMS-Borosilicate 복합막에 의한 수소-질소 기체 분리에 관한 연구)

  • Lee, Suk Ho;Lee, Hyun Kyung
    • Membrane Journal
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    • v.25 no.2
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    • pp.123-131
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    • 2015
  • The PTMSP/PDMS graft copolymer were synthesized from the PTMSP[poly(1-trimethylsilyl-1-propyne)] and the PDMS[poly(dimethylsiloxane)] and then the PTMSP/PDMS-borosilicate composite membranes were prepared by adding the porous borosilicates to the PTMSP/PDMS graft copolymer. The number-average molecular weight (${\bar{M}}_n$) and the weight-average molecular weight (${\bar{M}}_w$) of PTMSP/PDMS graft copolymer were 460,000 and 570,000 respectively, and glass transition temperature ($T_g$) of PTMSP/PDMS graft copolymer appeared at $33.53^{\circ}C$ according to DSC analysis. According to the TGA measurements, the addition of borosilicate to the PTMSP/PDMS graft copolymer leaded the decreased weight loss and the completed weight loss temperature went down. SEM observation showed that borosilicate was dispersed in the PTMSP/PDMS-borosilicate composite membranes with the size of $1{\sim}5{\mu}m$. Gas permeation experiment indicated that the addition of borosilicate to PTMSP/PDMS graft copolymer resulted in the increase in free volume, cavity and porosity resulting in the gradual shift of the mechanism of the gas permeation from solution diffusion to molecular sieving surface diffusion, and Knudsen diffusion. Consequently, the permeability of $H_2$ and $N_2$ increased and selectivity ($H_2/N_2$) decreased as the contents of borosilicate increased.