• Title/Summary/Keyword: NMR 분광법

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Antioxidative Activity of Flavonoids Isolated from Jindalrae Flowers (Rhododendron mucronulatum Turcz.) (진달래꽃으로부터 분리된 플라보노이드 화합물의 항산화성에 관한 연구)

  • Kim, Mi-Ae;Jones, A. Daniel;Chung, Tae-Yung
    • Applied Biological Chemistry
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    • v.39 no.4
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    • pp.320-326
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    • 1996
  • Seven antioxidative flavonoids were isolated from Jindalrae flowers (Rhododendron mnonulatum Turcz.), an edible plant in Korea. These compounds were identified as afzelin, ampelopsin, catechin, myricetin, myricitrin, quercetin and quercitrin on the basis of IR, UV, FAB-MS, $^1H\;NMR,\;and\;^{13}C\;NMR$ data. These compounds were consisted of two flavonols, three flavonol glycosides, a flavane, and a dihydroflavonol. The flavonol glycosides (14.4 g) present in th ethyl ether and ethyl acetate fractions comprised up to 82% of their total flavonoid amount (17.6 g) finally recovered by means of polyamide C-200 column chromatography, preparative TLC, recrystallization, and Sephadex LH-20 column chromatography. The antioxidant activities were measured in an ethanol solution of linoleic acid in the presence of ferric thiocyanate. The antioxidant efficiency increased in the order of afzrlin<$\alpha-tocopherol$

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Isolation and Characterization of Humic Acids Present in the Soils at the Vicinity of Domestic Atomic Power Plants(NPPs) (국내 원자력 발전소 주변 토양 휴믹산의 추출 및 특성 규명)

  • Lee, Chang-Hoon;Shin, Hyun-Sang;Chung, Kun-Ho;Cho, Young-Hyun;Lee, Chang-Woo
    • Journal of Radiation Protection and Research
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    • v.28 no.3
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    • pp.165-172
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    • 2003
  • Humic acids present in the soils at the vicinity of domestic atomic power plants(NPPs), located in Yeongkwang(YK), Uljin(UJ), Kori(KR), Koseong(KS), Wolseong(WS) area were isolated, and characterized using elemental analysis and UV/Vis, IR, CPMAS $^{13}C$ NMR spectroscopic methods. The characteristics were compared with one another and with commercial humic acid (Aldrich Co.). Molecular size distributions of the humic acids were determined using a stirred cell ultrafiltration technique. The results of elemental analysis showed that soil humic acid from UJ contains higher oxygen content than humic acids from KR and KS (O/C ratios: 0.51 (UJHA) us. 0.45(KRHA), 0.43(KSHA)). The molecular size distribution revealed that the soil humic acids of UJ and YK contained a higher percentage of larger molecules of > 30,000 daltons, compared to those of KR and KS. The spectral features obtained from UV/vis., IR and CPMAS $^{13}C$ NMR showed that the aromatic character and oxygen containing functional groups in the humic acids from UJ and YK were relatively higher than those of KR and KS. These results indicate that the soil humic acids from UJ and YK were in a higher degree of humification, which may suggest higher affinity of the humic acids with radionuclides released in the soil environments.

Differences in Structural Characteristics and Eu(III) Complexation for Molecular Size Fractionated Humic Acid (분자량별 분류에 따른 휴믹산의 구조적 특성 및 Eu(III)과의 착물 반응 특성 비교에 대한 연구)

  • Shin, Hyun-Sang;Rhee, Dong-Seok;Kang, Kihoon
    • Analytical Science and Technology
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    • v.14 no.2
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    • pp.159-166
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    • 2001
  • A humic acid(HA, Aldrich Co) sample was subjected to ultrafiltration for molecular size fractionation and three fractions of different nominal size($F_1$: 1,000-10,000 daltons; $F_2$: 10,000-50,000 daltons; $F_3$: 100,000-300,000 daltons) were obtained. The structural characteristics of the size-fractionated HA were analyzed using their IR and solid state C-13 NMR spectral data, and the carboxylate group contents of the humic acids were determined using their pH titration data. The $^7F_0-{^5}D_0$ excitation spectra of Eu(III) complexes of the size-fractionated mgHA in aqueous solution were acquired($[Eu(III)]=1.0{\times}10^{-4}mol\;L^{-1}$, $(HA)=470-970mg\;L^{-1}$) at pH 5.0 using a pulsed tunable laser system, in which metal binding properties of the size-fractionated HA were elucidated and compared on another. Characterization of the IR and C-13 NMR spectral data indicated that the fraction($F_3$) with molecules of larger size were primarily aliphatic, while the fractions($F_1$, $F_2$) with smaller molecules of less than 50,000 daltons were predominantly aromatic. Titration data were consistent with an increase in the number of carboxylate groups per unit mass as molecular size became smaller. The $^7F_0-{^5}D_0$ excitation spectral data of Eu(III)-humate complexes showed that the peak maxima on these spectra were shifted toward lower energies with increasing molecular size of HA, indicating the higher degree of bindings of the Eu in the molecules of larger size. We also discussed the relationship of the lower energy shifts of the maximum peaks with increasing the molecular size of HA with the structural differences of the size-fractionated HA.

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X-Ray and NMR Studies of Vanadium(V)-Nitrilotriacetate Complex (바나듐(V)-니크릴로트리아세테이트 착물의 X-선 및 핵자기공명 연구)

  • Lee, Man-Ho;Jeong, Woo-Won
    • Analytical Science and Technology
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    • v.10 no.3
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    • pp.196-202
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    • 1997
  • New vanadium(V) complex, $(NH_4)_2[VO_2NTA]$, has been synthesized and its structure has been determined by solution and solid-state NMR spectroscopies as well as X-ray crystallography. The unit cell of the monoclinic crystals contains four complexes with $a=6.923(1){\AA}$, $b=8.824(2){\AA}$, $c=19.218(11){\AA}$ and ${\beta}=91.60(3)^{\circ}$ in the space group of $P2_1/n$. The $[VO_2NTA]^{2-}$ anion has distorted octahedral geometry with cis-$VO_2$ moiety. It is confirmed that the octahedral geometry is retained in both of solution and solid-state complexes.

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The Solubilization Site of Some Phenyl Alkanols in Aqueous Sodium Dodecylsulfate Micelle (몇가지 페닐 알카놀의 Sodium Dodeylsulfate 수용액 미셀내에서의 가용화 위치)

  • Jeong, Jong Jae;Gang, Jeong Bu;Lee, Gyeong Hui
    • Journal of the Korean Chemical Society
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    • v.38 no.3
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    • pp.194-199
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    • 1994
  • The solubilization sites of some phenyl alkanols such as phenol, benzyl alcohol, phenethyl alcohol, 3-phenyl-1-propanol solubilized in 0.2 M aqueous sodium dodecylsulfate micelle solution was studied by two dimensional heteronuclear correlation spectroscopy (2D C-H COSY). The results show more quantitative and clear solubilization sites in the SDS micelle than previous results using $^1H$-NMR spectrum integration. We found that most of the phenyl alkanols penetrate into the core of SDS micelle, and the insertion depth was 6.5∼7.0 methylene units from ${\alpha}$-methylene.

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The Effect of Gingko Biloba Extract on Energy Metabolic Status in C3H Mouse Fibrosarcoma : Evaluated by in vivo $^{31}P$ Magnetic Resonance Spectroscopy (Gingko biloba extract가 C3H 마우스 섬유육종의 에너지 대사 상태에 미치는 영향 : 생체내 $^{31}P$ 자기공명 분광법을 이용한 분석)

  • Ha Sung Whan;Kim Won Dong;Ahn Yong Chan;Park Chan Il;Lim Tae Hwan;Lee Tae Kuen
    • Radiation Oncology Journal
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    • v.20 no.2
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    • pp.147-154
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    • 2002
  • Purpose : Gingko biloba extract (GBE), a natural product extracted from Gingko leaves, is known to increase the radiosensitivity of tumors. This radiosensitization probably arises from the increase in the peripheral blood flow by decreasing the blood viscosity and relaxing the vasospasm. The influence of a GBE on the metabolic status in fibrosarcoma II (FSall) of a C3H mouse was investigated using $^{31}P$ magnetic resonance spectroscopy (MRS). Materials and Methods : Eighteen C3H mice with fibrosarcoma II $(from\;100\;mm^3\;to\;130\;mm^3)$ were prepared for this experiment. The mice were divided into 2 groups; one (9 mice) without a priming dose, and the other (9 mice) with a priming dose of GBE. The GBE priming dose (100 mg/kg) was administered by an intraperitoneal (i.p.) injection 24 hours prior to the measurement. First $^{31}P$ MRS spectra were measured in the mice from each group as a baseline and test dose of GBE (100 mg/kg) was then administered to each group. One hour later, the $^{31}P$ MRS spectra were measured again to evaluate the change in the energy metabolic status. Results : In the group without the priming dose, the mean pH, PCr/Pi, PME/ATP, Pi/ATP, PCr/(Pi+PME) values 1 hour after the test dose were not changed significantly compared to the values at the baseline. However, in the group with the priming dose, the mean PCr/Pi, Pi/ATP, PCr/(Pi+PME) values 1 hour after the test dose changed from the baseline values of 0.49, 0.77, 0.17 to 0.74, 0.57, 0.28 respectively. According to the paired t-test, the differences were statistically significant. Conclusion : The above findings suggest that the metabolic status is significantly improved after administering GBE if the priming dose is given 24 hours earlier. This shows that the radiosensitizing effect of GBE is based on the increase of tumor blood flow and the improvement in the metabolic status.

DNA Binding Studies and Cytotoxicity of the Novel 1,10-phenanthroline Palladium(II) Complexes of Dithiocarbamate Derivatives (디티오카르바메이트 유도체의 새로운 1,10-페난트롤린 팔라디움(II) 착물의 DNA 결합 성질 및 세포독성에 관한 연구)

  • Mansouri-Torshizi, Hassan;Saeidifar, Maryam;Ghasemi, Zahra Yekke;Khastan, Mahmood;Divsalar, Adeleh;Saboury, Ali Akbar
    • Journal of the Korean Chemical Society
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    • v.55 no.1
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    • pp.70-80
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    • 2011
  • Two new palladium (II) complexes, [Pd (phen)(pip-dtc)]$NO_3$ and [Pd(phen)(mor-dtc)]$NO_3$, (where phen is 1,10-Phenantroline, pip-dtc is piperidinedithiocarbamate anion and mor-dtc is morpholinedithiocarbamate anion) have been synthesized and characterized by elemental analysis, spectroscopic studies (FT-IR, $^1H$ NMR, UV-Vis) and conductance measurement. In these complexes, the dithiocarbamate ligands coordinate with Pd (II) center as bidentate with two sulfur atoms. These two complexes have been tested against chronic myelogenous leukemia cell line, K562. They show $IC_{50}$ values less than cisplatin and thus the mode of binding of the complexes to calf thymus DNA (CT-DNA) were investigated by ultraviolet difference and fluorescence spectroscopy. They can denature DNA, exhibit cooperative binding and intercalate into DNA. Several binding and thermodynamic parameters are also described.

Measurement and Assessment of Absolute Quantification from in Vitro Canine Brain Metabolites Using 500 MHz Proton Nuclear Magnetic Resonance Spectroscopy: Preliminary Results (개의 뇌 조직로부터 추출한 대사물질의 절대농도 측정 및 평가: 500 MHz 고자장 핵자기공명분광법을 이용한 예비연구결과)

  • Woo, Dong-Cheol;Bang, Eun-Jung;Choi, Chi-Bong;Lee, Sung-Ho;Kim, Sang-Soo;Rhim, Hyang-Shuk;Kim, Hwi-Yool;Choe, Bo-Young
    • Investigative Magnetic Resonance Imaging
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    • v.12 no.2
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    • pp.100-106
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    • 2008
  • The purpose of this study was to confirm the exactitude of in vitro nuclear magnetic resonance spectroscopy(NMRS) and to complement the defect of in vivo NMRS. It has been difficult to understand the metabolism of a cerebellum using in vivo NMRS owing to the generated inhomogeneity of magnetic fields (B0 and B1 field) by the complexity of the cerebellum structure. Thus, this study tried to more exactly analyze the metabolism of a canine cerebellum using the cell extraction and high resolution NMRS. In order to conduct the absolute metabolic quantification in a canine cerebellum, the spectrum of our phantom included in various brain metabolites (i.e., NAA, Cr, Cho, Ins, Lac, GABA, Glu, Gln, Tau and Ala) was obtained. The canine cerebellum tissue was extracted using the methanol-chloroform water extraction (M/C extraction) and one group was filtered and the other group was not under extract processing. Finally, NMRS of a phantom solution and two extract solution (90% D2O) was progressed using a 500MHz (11.4 T) NMR machine. Filtering a solution of the tissue extract increased the signal to noise ratio (SNR). The metabolic concentrations of a canine cerebellum were more close to rat’s metabolic concentration than human’s metabolic concentration. The present study demonstrates the absolute quantification technique in vitro high resolution NMRS with tissue extraction as the method to accurately measure metabolite concentration.

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Comparison of in Vivo, in Vitro 3T MR Spectroscopy and Proton NMR Spectroscopy for the Fluid from Cystic Tumor: Preliminary Study (낭성 종양의 체액에 대한 생체내, 생체외 3T 양성자 자기공명분 광법과 양성자 핵자기공명기법의 비교: Preliminary Study)

  • Lee, Hui-Joong;Kim, Jong-Yeol;Chang, Yong-Min
    • Investigative Magnetic Resonance Imaging
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    • v.12 no.2
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    • pp.107-114
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    • 2008
  • Purpose : The aim of this study is to determine possibility of application of in vivo proton ($^1H$) magnetic resonance spectroscopy (MRS) in distinguishing cystic mass arising around pancreas by comparison of in vivo MRS, in vitro MRS using 3T MR machine, based on nuclear magnetic resonance (NMR). Materials and Methods : We obtained spectra of in vivo MRS, in vitro MRS and NMR from abdominal mass arising around pancreas (mucinous cystic neoplasm=5, intraductal papillary mucin producing tumor=5, pseudocyst=1, and lymphangioma=1). We estimated existence of peak of in vivo MRS, and in vitro MRS concordant to that of NMR. We also evaluated differential peak for predicting specific disease. Results : Correlation of presence of peak with NMR showed showed sensitivity of 29.6%, specificity of 82.6% and accuracy of 67.7% on in vivo MRS (p = 0.096, McNemar test), sensitivity of 57.1% and specificity of 92.6% and accuracy of 82.3% on in vitro MRS (p = 0.362, McNemar test). The spectra of NMR for IPMT showed more frequent peaks at 3.5-4.0 ppm (p=0.026). Conclusion : Although chemical analysis, using NMR could be regarded as possible tool to differentiate cystic masses, in vivo and in vitro MRS need further technical evolution for clinical application.

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Synthesis and Characterization of Polymers with Azobenzene and Hexamethylene Groups in Main Chain (주사슬에 아조벤젠기와 헥사메틸렌기를 갖는 고분자의 합성 및 특성)

  • Gu, Su-Jin;Lee, Eung-Jae;Bang, Moon-Soo
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.4
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    • pp.86-92
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    • 2019
  • Polymers with various compositions of azobenzene and hexamethylene groups in the main chain were synthesized by a Schotten-Baumann reaction and their properties were investigated. The chemical structures and physical properties of the synthesized polymers were investigated by Fourier transform infrared spectroscopy, proton nuclear magnetic resonance spectroscopy, differential scanning calorimetry, thermogravimetric analysis, polarized optical microscopy, and x-ray diffraction. The polymers showed an inherent viscosity of 1.28-1.36 dl/g and were relatively insoluble in most organic solvents. The melt transition temperature increased rapidly with increasing number of azobenzene groups in the polymer. When the azobenzene monomer content was more than 50 mol%, no melting transition occurred below the decomposition temperature. Among the polymers with a melt transition temperature, the MP-A3C7 and MP-A5C5 polymers were liquid crystalline materials and exhibited a nematic phase with weak liquid crystallinity over a wide liquid crystal temperature range. This difference in the properties of the synthesized polymers is likely due to the changes in intermolecular forces resulting from the linearity and polarity of the trans-form of azobenzene.