• Title/Summary/Keyword: NMR study

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Synthesis Characterization and Biodistribution of $^{99m}Tc$-Ethyl-3-Isocyanobutyrate as a New Myocardial Perfusion Agent (새로운 심관관류 영상 화합물로서 $^{99m}Tc$-Ethyl-3-Isocyano-butyrate의 합성, 표지 및 체내동태에 대한 연구)

  • Lee, Myung-Chul;Cho, Jung-Hyuck;Lee, Dong-Soo;Lim, Sang-Moo;Oh, Seung-Joon;Chung, Soo-Wook;Lee, Kyung-Han;Jeong, Jae-Min;Chung, June-Key;Koh, Chang-Soon
    • The Korean Journal of Nuclear Medicine
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    • v.27 no.2
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    • pp.223-232
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    • 1993
  • Technetium labeled isonitrile analogues are widely used as myocardial perfusion imaging agents. We synthesized and characterized a new isonitrile compound, ethyl 3-isocyanobutyrate(EIB). Proton and $^{13}C$ NMR spectroscopy and thin layer chromatography with a $C_{18}$ coat was performed. EIB was easily labeled with $^{99m}TcO_4^-$- with sodium dithionite. The labeling efficiency measured by RP-HPLC was over 95%. The labeled product was stable with dilution in normal saline and with prolonged incubation at room temperature. There was no formation of secondary products or free $^{99m}TcO_4^-$. In vivo kinetics study of $^{99m}Tc$ (I) labeled EIB in rabbits showed adequate myocardial uptake, good contrast against lung background, and relatively rapid liver clearance. The heart to lung ratio was over 2.5 and the heart to liver ratio was approximately from 0.4 to 5 at 60 minutes post injection. Hepatic clearance of $^{99m}Tc-MIBI$ was faster ($t_{1/2}$=6 minutes) than that of $^{99m}Tc-MIBI$. In vivo kinetics observed in dog was similar to that in rabbit but there was faster gallbladder filling, and thus lower liver background. SPECT imaging of the canine myocardium showed favorable imaging characteristics. However, biodistribution in mice demonstrated a myocardial % injected dose/organ of less than 0.1%. This was thought to be due to interspecies difference in plasma esterase activity. In human plasma, $^{99m}Tc$ ( I ) labeled EIB was stable for at least 2 hours, without production of secondary products by HPLC. We conclude that ethyl 3-isocyanobutyrate may be a potential new myocardial perfusion imaging agent and deserves further investigation as to its usefulness for clinical use.

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Preparation and Characterization of Cy5.5-conjugated Biocompatible Polymeric Micellar Nanoparticles for Optical Imaging (광학 영상을 위한 Cy5.5가 결합된 생체적합성 고분자 마이셀 나노입자의 제조 및 특성분석)

  • Kim, Hyo-Jeong;Kim, Byung-Jin;Lee, Ha-Yeong;Jung, Suk Hyun;Jeong, Seo-Young;Yuk, Soon-Hong;Shin, Byung-Cheo;Seong, Ha-Soo;Choi, Youn-Woong;Ha, Dae-Chul;Choi, Sun-Hang;Lee, Soo-Min
    • Journal of Pharmaceutical Investigation
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    • v.39 no.6
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    • pp.393-400
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    • 2009
  • PHEA (hydroxyethyl-aspartamide)-mPEG (methoy-polyethyleneglycol)-$C_{16}$ (hexadecylamine)-ED (ethylenediamine) was prepared as a drug delivery carrier. The structure and molecular weight of polymers were characterized by $^1H$-NMR and gel permeation chromatography. Micelle size and shape were measured by electro-photometer light scattering and transmission electron microscope. The mean diameter of micelles was 23 nm in aqueous solution. To evaluate the potential of these polymeric micelles as a drug carrier, PSI-mPEG-$C_{16}$-ED was conjugated with Cy5.5 for Near-Infrared Fluorescent (NIRF) based optical imaging. PSI-mPEG-$C_{16}$-ED-Cy5.5 was injected intravenously into mice (n=5) and in vivo NIRF imaging was performed during 48 h after injection. The biodistribution study at 24 h after injection showed the longcirculation property of PSI-mPEG-$C_{16}$-ED-Cy5.5. Therefore, PSI-mPEG-$C_{16}$-ED micelles could be a promising drug carrier and imaging agent.

Inhibition of Low Density Lipoprotein-oxidation, ACAT-1, and ACAT-2 by Lignans from the Bark of Machilus thunbergii

  • Shrestha, Sabina;Park, Ji-Hae;Lee, Dae-Young;Cho, Jin-Gyeong;Lee, Do-Gyeong;Cho, Moon-Hee;Jeong, Tae-Sook;Kang, Hee-Cheol;Baek, Nam-In
    • Journal of Applied Biological Chemistry
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    • v.54 no.1
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    • pp.63-66
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    • 2011
  • The bark of Machilus thunbergii was extracted with 80% aqueous methanol (MeOH), and the concentrated extract was partitioned using ethyl acetate (EtOAc), butanol (n-BuOH), and $H_2O$, successively. From the EtOAc fraction, five lignans were isolated through the repeated silica gel, octadecyl silica gel (ODS) and, Sephadex LH-20 column chromatography. Based on nuclear magnetic resonance (NMR), mass spectroscopy (MS), and infrared spectroscopy (IR) spectroscopic data, the chemical structures of the compounds were determined to be machilin A (1), machilin F (2), licarin A (3), nectandrin A (4), and nectandrin B, (5). This study presents comparative account of five lignans from M. thunbergii bark contributing inhibition of low density lipoprotein (LDL), ACAT-1, and ACAT-2. Compounds 2-5 showed varied degree of antioxidant activity on LDL with $IC_{50}$ values of 2.1, 11.8, 15.3, and $4.1{\mu}M$. Compounds 1, 2, and 3 showed inhibition activity on ACAT-1 with values $63.4{\pm}6.9%$ ($IC_{50}=66.8{\mu}M$), $53.7{\pm}0.9%$ ($IC_{50}=109.2{\mu}M$), and $78.7{\pm}0.2%$ ($IC_{50}=40.6{\mu}M$), respectively, at a concentration of 50 mg/mL, and on ACAT-2 with values $47.3{\pm}1.5%$ ($IC_{50}=149.7{\mu}M$), $39.2{\pm}0.2%$ ($IC_{50}=165.2{\mu}M$), and $52.1{\pm}1.0%$ ($IC_{50}=131.0{\mu}M$, respectively, at a concentration of 50 mg/mL.

Chemical Constituents of Domestic Quercus spp. Barks (국내산 참나무속 수종 수피의 추출성분)

  • Kim, Jin-Kyu;Kwon, Dong-Joo;Lim, Soon-Sung;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
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    • v.38 no.4
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    • pp.359-374
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    • 2010
  • This study was carried out to investigate the chemotaxonomical correlation and chemical constituents of domestic Quercus spp. barks. The barks of Q. mongolica, Q. aliena, Q. serrata, Q. acutissima, Q. dentata, and Q. variabilis were collected in the experimental forest of Kangwon National University. The combined extracts were successively fractionated with n-hexane, methylene chloride and ethyl acetate using a separation funnel. A portion of the ethyl acetate and H2O soluble materials of each species were chromatographed on a Sephadex LH-20 column using various aqueous MeOH and EtOH-hexane as washing solvents. Spectrometric analysis such as NMR and MS, including TLC, were performed to characterize the structures of the isolated compounds. Ellagic acid (0.03 g), (+)-catechin (4.59 g), taxifolin (3.35 g), and glucodistylin (20.52 g) were isolated from Q. mongolica bark. Gallic acid (0.18 g), (+)-catechin (8.52 g), (+)-gallocatechin (0.09 g), taxifolin (0.54 g), and glucodistylin (3.28 g) were characterized from Q. acutissima bark. Gallic acid (0.38 g), ellagic acid (0.11 g), (+)-catechin (2.01 g), (+)-gallocatechin (0.12 g), and glucodistylin (0.39 g) were identified from Q. dentata bark. Ellagic acid (1.51 g), (+)-catechin (21.91 g), and glucodistylin (3.91 g) were purified from Q. aliena bark. Ellagic acid (0.84 g), (+)-catechin (0.82 g), taxifolin (4.02 g), and glucodistylin (21.50) were isolated from Q. serrata bark. Gallic acid (0.24 g), caffeic acid (0.05 g), (+)-catechin (0.32 g), and glucodistylin (0.65 g) were purified from Q. variabilis bark. (+)-Catechin and glucodistylin were isolated from all the barks. Glucodistylin can be a taxonomic index on Quercus spp.

Information Requirements, IS Planning Typology, and IS Planning Effectiveness : An Empirical Study (정보요구, 정보시스템 기획유형, 그리고 정보시스템 기획 효과성에 관한 실증적 연구)

  • 문태수
    • Proceedings of the Korea Association of Information Systems Conference
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    • 1997.10b
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    • pp.111-136
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    • 1997
  • 정보시스템 기획(IS planning)은 경영환경의 변화로부터 야기되는 조직의 정보요구 를 제대로 파악함으로써 새로운 정보시스템의 구축이나 실행과정에 반영하는 중요한 과업중 의 하나이다. 하지만, 아직까지 정보요구를 반영한 정보시스템 기획유형에 관한 연구나 정 보시스템 기획의 효과성에 관한 영향에 대한 실증적인 연구가 없었다. 그리하여, 본 연구에 서는 기업의 경쟁력 강화 목표를 달성하기 위해 필요한 정보시스템의 효율적인 관리와 활용 을 위하여 정보시스템 기획에 관한 상황 이론적 접근을 시도하였다. 본 연구는 과업환경을 중심으로 발생하는 정보요구의 유형에 따라 정보시스템 계획을 어떻게 추진하는 것이 바람 직한 것인지를 파악하고, 정보시스템을 기획 시 정보요구 수준과의 적합성(fitness)에 따라 정보시스템 기획의 효과성은 어떻게 달라지는 지를 파악하고자 한다. 이를 위하여 본 연구 에서 사용된 Construct와 변수들은 기존의 정보시스템 기획관련 문헌을 이용하였다. 본 연 구를 위하여 국내 매출액 1000대 기업을 대상으로 설문지를 우송하였으며, 그 중 187부가 회수되었다. 자료분석의 결과, 정보요구 수준과 정보시스템 기획유형간의 관련성은 긍정적 으로 관련되어 있었으며, 정보요구 수준에 따른 기획의 효과성에는 차이가 없었으나, 정보 시스템 기획유형에 따른 기획의 효과성은 유의한 차이가 있었다. 특히, 정보요구 수준과 정 보시스템 기획유형간의 적합성에 의한 정보시스템 기획의 효과성에 대한 t-test결과는 적합 한 조직(fit organization)보다는 적합하지 않은 조직(unfit organization)의 성과가 더 높은 것으로 나타났다.성 형질전환 계통의 식물체 내에서의 바이러스 증식 및 이동과 관련된 저항성 기작, 여러 가지 PVY 계통에 대한 저항성 유무, 수량, 생육 특성 및 주요 화학 성분 함량 등을 발표하고자 한다.-glucose로 구성된 다당류 이었다. 아미노산은 Asp 및 Glu의 산성 아미노산과 Ala, Leu 등의 함량이 높게 나타났으며, 비알칼리 추출물에서 Ser과 Thr의 함량이 높게 나타났다. 다당류 T-AS는 평균 분자량이 2,000 kD와 12kD에서 주 peak를 나타냈으며, 수용성 분획의 평균 분자량은 12kD이고 비수용성 분획은 36~2,000 kD의 평균 분자량 분포를 갖는 것으로 나타났다. IR과 NMR 분석 결과 890 cm-1에서 흡수 peak를 나타내어 $\beta$-(1,3)0glucan과 $\beta$-(1,6)-glucan의 구조를 갖는 다당류로 확인 되었다. T-AS 분획은 C:H:O:N의 함량비가 38.9:5.7:49.6:1.84%이며, 이 물질의 융점은 163 $^{\circ}C$로 연한 갈색을 나타낸다. 분리된 GLG의 항암활성 기전 규명을 위해, in vivo 항암실험, 항보체 활성능, 항체 생성능, serum protein 분비능, 대식세포의 탐식능과 활성능 및 세포간 물질 분비 등의 상관관계를 조사하였다. 다당류 GLG 분획물들 가운데 항보체의 활성이 높았던 분획은 sarcome 180에 대한 항암 활성이 높게 나타났다. 다당류 T-AS의 보체 활성화 기작은 classical과 alternative complement pathway의 양 경로를 통해 활성화 되었다. T-AS 분획은 mouse내의 특정

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Complex Formation of Transition and Post-Transition Metal Ions with 1,15-Diaza-3,4 : 12,13-dibenzo-5,8,11-trioxacyclooctadecane (전이 및 중금속이온과 1,15-diaza-3,4 : 12,13-dibenzo-5,8,11-trioxa-cyclooctadecane과의 착물형성)

  • Kim, Si-Joong;Lee, Myung-Jae;Koo, Chang-Hyung;Woo, Kyoun-Ja
    • Journal of the Korean Chemical Society
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    • v.35 no.6
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    • pp.645-652
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    • 1991
  • The stability constants$(K_f)$ of the complexes of some transition and post-transition metal ions (Co(Ⅱ), Ni(Ⅱ), Cu(Ⅱ), Zn(Ⅱ), Cd(Ⅱ), Pb(Ⅱ), Hg(Ⅱ)) with $N_2O_3$-donor macrocyclic ligand, 1,15-diaza-3,4 : 12,13-dibenzo-5,8,11-trioxacyclooctadecane ($NtnOdienH_4$), have been determined by potentiometry in aqueous solution at $25^{\circ}C$. Log $K_f$ values of the complexes were : Co(Ⅱ): 3.83, Ni(Ⅱ) : 4.56, Cu(Ⅱ) : 7.74, Zn(Ⅱ) : 4.98, Cd(Ⅱ) : 3.91, Pb(Ⅱ) : 6.65, and Hg(Ⅱ) : 14.87. The order of stabilities of transition metal complexes was the same as the natural order of stability proposed by Williams-Irving. In post-transition metal complexes, the order of stabilities was Cd(Ⅱ) < Pb(Ⅱ) < Hg(Ⅱ), and the covalent character in metal ion-donor atoms bonds appeared a dominant factor in the stability. In methanol solution, each metal ion forms 1 : 1 complex, while Ni(Ⅱ) ion forms both 1 : 1 and 1 : 2 complexes. It was confirmed by $^1H-$ and $^{13}C-$NMR spectral study that the nitrogen atoms in the ligand were major contributors for the complexation of post-transition metal ions with the ligand. It was shown, by elementry analysis, electrical conductivity and magnetic susceptibility measurements, and spectral analysis, that solid Cu(Ⅱ)-and Zn(Ⅱ)-complexes have a distorted octahedral and a tetrahedral structure, respectively.

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Isolation and HPLC-DAD validation of xanthoangelol in Lespedeza bicolor extract (싸리나무 추출물의 Xanthoangelol 분리 및 HPLC-DAD 밸리데이션)

  • Woo, Hyun Sim;Kim, Yeong-Su;Oh, Yu Jin;Cho, Hae Jin;Song, Se-Kyu;Kim, Dae Wook
    • Korean Journal of Food Science and Technology
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    • v.52 no.1
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    • pp.26-30
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    • 2020
  • This study was undertaken to determine the characteristics of xanthoangelol, the major chalcone constituent derived from the extracts of different parts of Lespedeza bicolor. Xanthoangelol was isolated from the root extract using column chromatography and used as a standard for quantitative analysis. The structure of the isolated compound was established based on spectroscopic evidence. The HPLC-DAD method was validated for specificity, linearity, precision, accuracy, limit of detection, and limit of quantitation. The calibration curve of xanthoangelol had significant linearity (R2>0.9999). Limit of detection and limit of quantitation 0.018 and 0.059 ㎍/mL, respectively. The relative standard deviation values of precision test, and intra- and inter-day tests were less than 0.22 and 0.40%, respectively. In the recovery test, the accuracy ranged from 98.98-102.78% with RSD values less than 0.13%. The method validation parameters indicate the applicability of the HPLC method for quality control of food or drug formulations containing L. bicolor.

Kinetic Study of Macrocyclic Ligand-Metal Ion Complexes (거대고리 리간드와 금속이온과의 착물에 관한 반응속도론적 연구)

  • Moon-Hwan Cho;Jin-Ho Kim;Hyu-Bum Park;Si-Joon Kim
    • Journal of the Korean Chemical Society
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    • v.33 no.4
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    • pp.366-370
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    • 1989
  • A new macrocyclic ligand 1,15,18-triaza-3,4;12,13-dibenzo-5,8,11-cycloeicosane (NdienOdien$H_4$ = $N_3O_3$) has been synthesized and identified by element analysis, NMR and IR spectrophotometry. Stepwise protonation constants of ligand are determined by potentiometry in 95% methanol solution(I = 0.1 mol $dm^{-3}$, $Me_4$NCl). log $K_1$;log $K_2$;log $K_3$ = 9.1;8.1;3.6.The kinetics of the acid-promoted dissociation reactions of complex cations of nickel(II) and copper(III) with NdienOdien and NdienOen macrocyclic ligands having, respectively, 17 and 20 ring members, have been studied spectrophotometrically in HCl$O_4$ NaCl$O_4$ aqueous solutions. From the temperature effect on kinetic constant ($k_{obs}$), the parameters of activation(${\Delta}H^{\neq}$, ${\Delta}S^{\neq}$) of dissociation reaction for $ML^{2+}$ with $H^+$ ion have been determined. We have proposed the possible mechanism of the reaction from the data obtained.

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New Ruthenium Complexes for Semiconductor Device Using Atomic Layer Deposition

  • Jung, Eun Ae;Han, Jeong Hwan;Park, Bo Keun;Jeon, Dong Ju;Kim, Chang Gyoun;Chung, Taek-Mo
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.363-363
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    • 2014
  • Ruthenium (Ru) has attractive material properties due to its promising characteristics such as a low resistivity ($7.1{\mu}{\Omega}{\cdot}cm$ in the bulk), a high work function of 4.7 eV, and feasibility for the dry etch process. These properties make Ru films appropriate for various applications in the state-of-art semiconductor device technologies. Thus, it has been widely investigated as an electrode for capacitor in the dynamic random access memory (DRAM), a metal gate for metal-oxide semiconductor field effect transistor (MOSFET), and a seed layer for Cu metallization. Due to the continuous shrinkage of microelectronic devices, better deposition processes for Ru thin films are critically required with excellent step coverages in high aspect ratio (AR) structures. In these respects, atomic layer deposition (ALD) is a viable solution for preparing Ru thin films because it enables atomic-scale control of the film thickness with excellent conformality. A recent investigation reported that the nucleation of ALD-Ru film was enhanced considerably by using a zero-valent metallorganic precursor, compared to the utilization of precursors with higher metal valences. In this study, we will present our research results on the synthesis and characterization of novel ruthenium complexes. The ruthenium compounds were easy synthesized by the reaction of ruthenium halide with appropriate organic ligands in protic solvent, and characterized by NMR, elemental analysis and thermogravimetric analysis. The molecular structures of the complexes were studied by single crystal diffraction. ALD of Ru film was demonstrated using the new Ru metallorganic precursor and O2 as the Ru source and reactant, respectively, at the deposition temperatures of $300-350^{\circ}C$. Self-limited reaction behavior was observed as increasing Ru precursor and O2 pulse time, suggesting that newly developed Ru precursor is applicable for ALD process. Detailed discussions on the chemical and structural properties of Ru thin films as well as its growth behavior using new Ru precursor will be also presented.

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Phase Behavior and Structural Analyses of the THF + H2 Binary Clathrate Hydrate (THF + H2 이성분계 크러스레이트 하이드레이트의 상거동 및 구조 분석)

  • Cha, Jong-Ho;Park, Youngjune;Cha, Min-Jun;Yeon, Sun-Hwa;Lee, Huen
    • Korean Chemical Engineering Research
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    • v.46 no.6
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    • pp.1095-1099
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    • 2008
  • In this study, we investigated that hydrate formation and phase behavior of the $THF+H_2$ binary clathrate hydrates. In order to confirm the binary clathrate hydrate formation we employed the Raman and NMR spectroscopies that are known to be quite powerful tools, particularly for examining the cage occupancy pattern of guest molecules. In addition, we traced the P-T profiles from clathrate hydrate formation and dissociation process, which made it possible for the resulting phase equilibrium boundary to be clearly established. In the binary clathrate hydrate matrix we further identified that the relatively large THF molecules can only occupy the large $5^{12}6^4$ cavities, while the small $H_2$ molecules are entrapped in the empty $5^{12}$ cavities in structure-II, making the hydrate to be stable above 273 K even at relatively low pressure condition. Considering that pure $H_2$ hydrate can be produced at the extreme pressures higher that 1,000 bar, we can conclude that the water-soluble second guest inclusion induces $H_2$ storage and transportation to be readily achievable under much milder conditions.