• Title/Summary/Keyword: trimethylsilyl

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Synthesis of Substrates for Gene Therapy Monitoring of HSV1-TK System (유전자 영상용 HSV1-TK 기질의 합성)

  • Choi, Tae-Hyun;Ahn, Soon-Hyuk;Choi, Chang-Woon;Lim, Sang-Moo;Awh, Ok-Doo
    • The Korean Journal of Nuclear Medicine
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    • v.36 no.2
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    • pp.102-109
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    • 2002
  • Purpose : In gene therapy, tumor cells expressing the herpes simplex virus thymidine kinase are sensitive to prodrugs. Potential prodrugs IVDU and IVFRU were synthesized and radiolabeled with radioiodine for noninvasive imaging of herpes simplex virus type 1 gene expression. Material and Methods : 5-(2-trimethysilyl) vinyl-2'-deoxyuridine and 5-(2-trimethylsilyl)vinyl-2'-fluoro-2'-deoxyuridine, precursors of 5-(2--iodo)viny l-2'-deoxy uridine(IVDU) and 5-(2-iodo)-2'-vinyl-2'-deoxy-2'-fluororibofuranosyl uracil(IVFRU), were synthesized from reaction of trans-1-trimethylsillyl-2-tri-n-butylstannylethylene with 5-iodo-2'-deoxyuridine and 5-iodo-2'-fluoro-2'-deoxyuridine, respectively, on the condition of Pd catalyst. These precursors were separated from reaction mixture by silica gel column chromatography method. Each precursor was radioiodinated with radioiodine by mixing with ICI oxidizing agent. These radioiodinated compounds were purified with HPLC. Radiohalogen exchange has been shown to be effective for the synthesis of products with lower specific activity. Similarly, carrier-added and high specific activity products have been isolated in respectable radiochemical yields using ICI method. Results : Synthetic yield of precursors, IVDU and IVFRU were 43% and 18%, respectively. Radiochemical purity of both compunds was over 98%. Conclusion : We synthesized precursors of IVDU and IVFRU for monitoring of HSV1-tk gene expression. Radiotracers were radioiodinated with high radiolabeling yield by ICI method.

Separation of $H_2$ and $N_2$ Gases by PTMSP-NaY Zeolite Composite Membranes (PTMSP-NaY Zeolite 복합막에 의한 수소-질소 기체 분리에 관한 연구)

  • Kim, Ok-Su;Hong, Se Ryeong
    • Membrane Journal
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    • v.24 no.4
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    • pp.285-291
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    • 2014
  • The PTMSP[Poly(1-trimethylsilyl-1-propyne)]-NaY zeolite composite membranes were prepared by adding 0~50 wt% NaY zeolite to PTMSP. In order to investigate the characteristics of these membranes, we used the analytical methods such as FT-IR, $^1H$-NMR, GPC, DSC, TGA, and SEM. Gas permeation experiments were carried out at $23{\sim}26^{\circ}C$, $2kgf/cm^2$, and the permselectivity of $H_2$ and $N_2$ gases through the composite membranes was studied as a function of the NaY zeolite contents. According to TGA measurements, when NaY zeolite was inserted within the PTMSP, thermal stability of PTMSP was enhanced. Based on SEM observation, NaY zeolite was dispersed in the PTMSP-NaY zeolite composite membrane with a size of $1.5{\mu}m$. The permeability of $H_2$ and $N_2$ through the PTMSP-NaY zeolite composite membranes increased as NaY zeolite content increased. On the contrary, the selectivity($H_2/N_2$) of the PTMSP-NaY zeolite composite membranes decreased as zeolite content increased.

Comparison of Liquid Chromatography-Mass/Mass Spectrometry (MS) and Gas Chromatography-MS for Quantitative Analysis of Indole-3-acetic acid and Indole-3-butyric acid from the Concentrated Liquid Fertilizer (Liquid Chromatography-Mass/Mass Spectrometry (MS)와 Gas Chromatography-MS를 이용한 농축 액상 비료제품 중 Indole-3-acetic acid 및 Indole-3-butyric acid 정량분석능 비교)

  • Kim, Jin Hyo;Park, Jong Min;Choi, Geun-Hyoung;Park, Yun-Ki;Im, Geon-Jae;Kim, Doo-Ho;Kwon, Oh-Kyung
    • Journal of Applied Biological Chemistry
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    • v.56 no.1
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    • pp.53-57
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    • 2013
  • In here, we investigated the quantitative analysis method of indole-3-acetic acid (IAA) and indole-3-butyric acid (IBA) with liquid chromatography-mass/mass spectrometry (LC-MS/MS) or gas chromatography-MS. Two ways of clean-up process were investigated for LC-MS/MS instrumental analysis of IAA, but both a simple dilution and hydrophile-lipophile balance (HLB) solid phase extraction (SPE) were not met the optimal recovery rates for quantitative analysis. On the other hand, the clean-up method for GC-MS was finally optimized through HLB-SPE from 250-folds diluted sample and methylation with trimethylsilyl chloride in methanol for 4 h. The limit of detection for methyl ester of IAA and IBA were both 1.4 mg/L, and recovery rates showed 93-107% from the concentrated liquid fertilizer.

Azomethine Yilde Forming Photoreaction of N-(Tributylstannyl)methylphthalimide (N-(트리부틸스탄일)메틸프탈이미드의 아조메틴 일리드 형성 광화학 반응)

  • Jeong, Ho-Cheol;Park, Ki-Hyun;Park, Hea-Jung;Cho, Dae-Won;Yoon, Ung-Chan
    • Journal of the Korean Chemical Society
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    • v.53 no.3
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    • pp.302-307
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    • 2009
  • Investigation was conducted to examine whether photochemical reaction of N-(tributylstannyl)- methylphthalimide generates an azomethine ylide intermediate in its excited state as its silyl derivative N-(trimethylsilyl)methylphthalimide which has been observed to form an azomethine ylide. The irradiation of N-(tributylstannyl)methylphthalimide in $D_2O-CH_3$CN generates mono-deuterated N-methylphthalimide as an exclusive product which supports the efficient generation of azomethine ylide intermediate and its trapping by water molecule through a proto-destannylation pathway. However the generated tributylstannyl subsitiuted ylide was not observed to be trapped with a dipolarophile such as methyl acrylate and acrylonitrile present in the reactions which is in contrast with the ylide from N-(trimethylsilyl)methylphthalimide.

Optical and electrical property of Indium-doped ZnO (IZO) grown by Atomic Layer Deposition (ALD) using Et2InN(TMS)2 as In precursor and H2O oxidant

  • Jo, Yeong-Jun;Jang, Hyo-Sik
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.421.1-421.1
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    • 2016
  • We studied indium-doped zinc oxide (IZO) film grown by atomic layer deposition (ALD) as transparent conductive oxide (TCO). A variety of TCO layer, such as ZnO:Al (AZO), InSnO2(ITO), Zn (O,S) etc, has been grown by various method, such as ALD, chemical vapor deposition (CVD), sputtering, laser ablation, sol-gel technique, etc. Among many deposition methods, ALD has various advantages such as uniformity of film thickness, film composition, conformality, and low temperature deposition, as compared with other techniques. In this study, we deposited indium-doped zinc oxide thin films using diethyl[bis(trimethylsilyl)amido]indium [Et2InN(TMS)2] as indium precursor, DEZn as zinc precursor and H2O as oxidant for ALD and investigated the optical and electrical properties of IZO films. As an alternative, this liquid In precursor would has several advantages in indium oxide thin-film processes by ALD, especially for low resistance indium oxide thin film and high deposition rate as compared to InCp, InCl3, TMIn precursors etc. We found out that Indium oxide films grown by Et2InN(TMS)2 and H2O precursor show ALD growth mode and ALD growth window. We also found out the different growth rate of Indium oxide as the substrate and investigated the effect of the substrate on Indium oxide growth.

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A study on the determination of residual Antibiotics and Synthetic Antibacterial Agents in Meat(III) Simultaneous Gas Chromatography/Mass Spectrometry Analysis of Erythromycin and Tylosin (식육중의 잔류 항생.항균제의 검정에 관한 연구(III) Macrolide계 항생물질인 Erythromycin과 Tylosin의 Gas Chromatography/Mass Spectrometry 동시분석)

  • 류재천;송윤선;양종순;서지원;김명수;박종세
    • Journal of Food Hygiene and Safety
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    • v.8 no.1
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    • pp.17-23
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    • 1993
  • In an attempt to quantitate and qualitate residual antibiotics and antibacterial agents n meat simultaneously, we studied a gas chromatogrphy-mass spectrometry (GC/MS) analysis. For a simultaneous analysis of macrolide antibiotics such as erythromycin and tylosin in meat, the homogenization with MeOH, defatting with n-hexane, extraction with CHCl3, elution with CHCl3 : MeOH=2:1 from Sep-Pak silica cartridge, acid gydrolysis, back extraction with CHCl3, and quantitation by selected ion monitoring(SIM) mode after trimethylsilyl derivatization were performed. The recoveries of erythromycin and tylosin (CV,%) at 10 ppm fortification level were 90.59(4.89) and 45.91(0.20) , and the detection limits of those were 0.02 and 2.0 $\mu\textrm{g}$/g beef, respectively. From these results, the developed analytical method using GC/MS-SIM mode allows excellent detection and quantitation of residual macrolide antibiotics in meats, using complementary method with bio-assay.

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Synthesis of D-1,3-Dioxolane and D-1,3-Oxathiolane Pyrimidine Nucleosides (D-1,3-Dioxolane 및 D-1,3-Oxathiolane 피리미딘 뉴크레오사이드의 합성)

  • Hong, Joon-Hee;Cha, Ma-Rie;Shin, Seong-Eun;Choi, Bo-Gil;Chung, Byung-Ho;Kim, Joong-Hyup;Lee, Chong-Kyo;Chung, Won-Keun;Chun, Moon-Woo
    • YAKHAK HOEJI
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    • v.38 no.6
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    • pp.703-711
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    • 1994
  • We synthesized D-1,3-dioxolanyl acetate from D-mannose using Frazer-Reide reaction and D-1,3-oxathiolanyl acetate from either D-mannose or D-galactose in good yields. These acetates were conjugated with various disilylated pyrimidine base using trimethylsilyl trifluoromethane sulfonate as a Lewis acid catalyst to obtain 32 different D-nucleosides.

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Photoaddition Reactions of N-Methylthiophthalimide with $\alpha$-Silyl-n-electron Donors via Single Electron Transfer-Desilylation and Hydrogen Atom Abstraction Pathways

  • Yoon, Ung-Chan;Oh, Sun-Wha;Moon, Seong-Chul;Hyung, Tae-Gyung
    • Journal of Photoscience
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    • v.9 no.1
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    • pp.17-22
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    • 2002
  • Studies have been conducted to explore photoaddition reactions of N-methylthiophthalimide with $\alpha$-silyl-n-electron donors Et$_2$NCH$_2$SiMe$_3$, n-PrSCH$_2$SiMe$_3$ and EtOCH$_2$SiMe$_3$. Photoaddition of $\alpha$-silyl amine Et$_2$NCH$_2$SiMe$_3$ to N-methylthiophthalimide occurs in $CH_3$CN and benzene to produce non-silicon containing adduct in which thiophthalimide thione carbon is bonded to $\alpha$-carbon of $\alpha$-silyl amine in place of the trimethylsilyl group. In contrast, photoaddition of EtOCH$_2$SiMe$_3$ to N-methylthiophthalimide generates two diastereomeric adducts in which thiophthalimide thione carbon is connected to $\alpha$-carbon of $\alpha$-silyl ether in place of u-hydrogen. Based on a consideration of the oxidation potentials of u-silyl-n-electron donors and the nature of photoadducts, mechanism for these photoadditions involving single electron transfer(SET) -desilylation and H atom abstraction pathways are proposed.

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Separation of Gas Based on PTMSP-silica-PEI Composites (PTMSP-silica-PEI 복합막에 의한 기체 분리에 관한 연구)

  • Kang Tae-Bum;Hong Se-Lyung
    • Membrane Journal
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    • v.16 no.2
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    • pp.123-132
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    • 2006
  • The PTMSP-silica-PEI composite membranes were synthesized from tetraethoxysilane (TEOS) and poly (1-trimethylsilyl-1-propyne) (PTMSP) by sol-gel process. The PTMSP-silica nanocomposite membranes were characterized by $^1H-NMR$, FT-IR, TGA, XPS, SEM, GPC and gas permeation measurements were accomplished with $H_2,\;O_2,\;N_2,\;CO_2,\;CH_4$. The gases permeability increased with increasing TEOS content. Both the permeability and selectivity of $H_2,\;CH_4$ increased to 15 wt% TEOS. While the permeability of $O_2,\;CO_2$ increased without decrease of selectivity.

Development of a GC-MS Diagnostic Method with Computer-aided Automatic Interpretation for Metabolic Disorders (GC-MS 크로마토그램의 컴퓨터 자동해석을 이용한 유전성 대사질환의 진단법 개발)

  • Yoon, Hye-Ran
    • Journal of The Korean Society of Inherited Metabolic disease
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    • v.6 no.1
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    • pp.40-51
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    • 2006
  • Purpose: A personal computer-based system was developed for automated metabolic profiling of organic aciduria and aminoacidopathy by gas chromatography-mass spectrometry and data interpretation for the diagnosis of metabolic disorders Methods: For automatic data profiling and interpretation, we compiled retention time, two target ions and their intensity ratio for 77 organic acids and 13 amino acids metabolites. Metabolites above the cut-off values were flagged as abnormal compounds. The data interpretation was a based on combination of flagged metabolites. Diagnostic or index metabolites were categorized into three groups, "and", "or" and "NO" compiled for each disorder to improve the specificity of the diagnosis. Groups "and" and "or" comprised essential and optional compounds, respectively, to reach a specific diagnosis. Group "NO" comprised metabolites that must be absent to make a definite diagnosis. We tested this system by analyzing patients with confirmed Propionic aciduria and others. Results: In all cases, the diagnostic metabolites were identified and correct diagnosis was founded to be made among the possible disease suggested by the system. Conclusion: The study showed that the developed method could be the method of choices in rapid, sensitive and simultaneous screening for organic aciduria and amino acidopathy with this simplified automated system.

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