• Title/Summary/Keyword: NMR measurements

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Triple isotope-[13C, 15N, 2H] labeling and NMR measurements of the inactive, reduced monomer form of Escherichia coli Hsp33

  • Lee, Yoo-Sup;Ko, Hyun-Suk;Ryu, Kyoung-Seok;Jeon, Young-Ho;Won, Hyung-Sik
    • Journal of the Korean Magnetic Resonance Society
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    • v.14 no.2
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    • pp.117-126
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    • 2010
  • Hsp33 is a molecular chaperone achieving a holdase activity upon response to a dual stress by heat and oxidation. Despite several crystal structures available, the activation process is not clearly understood, because the structure inactive Hsp33 as its reduced, zinc-bound, monomeric form has not been solved yet. Thus, we initiated structural investigation of the reduced Hsp33 monomer by NMR. In this study, to overcome the high molecular weight (33 kDa), the protein was triply isotope-[$^{13}C$, $^{15}N$, $^2H$]-labeled and its inactive, monomeric state was ensured. 2D-[$^1H$, $^{15}N$]-TROSY and a series of triple resonance spectra could be successfully obtained on a high-field (900 MHz) NMR machine with a cryoprobe. However, under all of the different conditions tested, the number of resonances observed was significantly less than that expected from the amino acid sequence. Thus, a possible contribution of dynamic conformational exchange leading to a line broadening is suggested that might be important for activation process of Hsp33.

($^{11}$B NMR study of vortex dynamics in LuNi$_2$B$_2$C

  • Lee, K.H.;Seo, S.W.;Kim, D.H.;Khang, K.H.;Seo, H.S.;Hwang, C.S.;Cho, B.K.;Lee, Moo-Hee
    • 한국초전도학회:학술대회논문집
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    • v.10
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    • pp.107-110
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    • 2000
  • ($^{11}$B NMR measurements have been performed on single crystals of LuNi$_2$B$_2$C superconductor to investigate vortex lattice structures and dynamical behavior. The spectrum in the superconducting state is significantly broadened by local field inhomogeneity due to the vortex lattice and the peak point of the spectrum shifts toward low magnetic field due to the imperfect field penetration. The linewidth of the spectrum reflecting local field variation is much smaller than expected for conventional vortex lattices and shows peculiar increase at low temperature. Furthermore, the transverse relaxation rate, 1/T$_2$, probing the slow motion of vortices, exhibits a single peak as temperature decreases. These prominent results highlight significant fluctuation of vortices even for this low T$_c$, and nearly isotropic 3D superconductor.

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Development of Reagent for Cancer Diagnosis by Urine Color Reaction (I)-Comparative analysis of cancer and non-cancer urine by NMR, HPLC and Gift reagent

  • Park, Man-Ki;Yang, Jeong-Seon;Lee, Mi-Yung;Kim, Yong-Ki;Weon, Nam-Bee;Kim, Young-Do
    • Archives of Pharmacal Research
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    • v.11 no.2
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    • pp.134-138
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    • 1988
  • Urine measurements by MNR were made for 25 persons including cancer and non-cancer patients. The aromatic proton signals of NMR wer observed much more often in cancer patients' urine than non-cancer patients' one. To compare the amount of the phenolic compounds excreted in urine between cancer and non-cancer patient, urine analysis by HPLC with UV detector was performed. Total peak area and major peak areas of cancer patients' urine wer emuch greater than those of non-cancer patients' one. To check the phenolic compound excreted in urine, a new jellied reagent named Gift reagent which was based on Millon's reagent, was developed for urine color reaction. When the reagent was tested, the sensitivity and specificity for urine samples of 69 persons including cancer and non-cancer patients were measured by 85.3% and 91.4%, respectively, indicating that the Gift reagent afford a possibility of cancer diagnosis.

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Measuring T1 contrast in ex-vivo prostate tissue at the Earth's magnetic field

  • Oh, Sangwon;Han, Jae Ho;Kwon, Ji Eun;Shim, Jeong Hyun;Lee, Seong-Joo;Hwang, Seong-Min;Hilschenz, Ingo;Kim, Kiwoong
    • Journal of the Korean Magnetic Resonance Society
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    • v.23 no.1
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    • pp.12-19
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    • 2019
  • A former study has shown that the spin-lattice relaxation time ($T_1$) in cancerous prostate tissue had enhanced contrast at an ultra-low magnetic field, $132{\mu}T$. To study the field dependence and the origin of the contrast we measured $T_1$ in pairs of ex-vivo prostate tissues at the Earth's magnetic field. A portable and coil-based nuclear magnetic resonance (NMR) system was adopted for $T_1$ measurements at $40{\mu}T$. The $T_1$ contrast, ${\delta}=1-T_1$ (more cancer)/$T_1$(less cancer), was calculated from each pair. Additionally, we performed pathological examinations such as Gleason's score, cell proliferation index, and micro-vessel density (MVD), to quantify correlations between the pathological parameters and $T_1$ of the cancerous prostate tissues.

Verification of Core/Shell Structure of Poly(glycidyl methacrylate-co-divinyl benzene) Microspheres

  • Jin, Jeong-Min;Choi, Jin-Young;Lee, Kang-Seok;Choe, Soon-Ja
    • Macromolecular Research
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    • v.17 no.5
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    • pp.339-345
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    • 2009
  • The core/shell type structure of the highly crosslinked poly(glycidylmetharylate-co-divinylbenzene) microspheres prepared in the precipitation polymerization in acetonitrile was thoroughly verified by means of swelling, $^1H$ NMR, XPS, TEM and TGA measurements. In the XPS measurement, the higher the GMA content, the higher the oxygen content was observed, implying that the higher content of GMA is observed in the particle surface. The further verification of the core/shell structure of the poly(GMA-co-DVB) particles was carried out using $^1H$ NMR and TEM techniques, resulting in the poly(GMA-co-DVB) particles with the GMA rich-phase and DVB rich-phase. In overall, the poly(GMA-co-DVB) microspheres consist of a highly crosslinked DVB rich-phase in the core and slightly or non-crosslinked GMA rich-phase in the shell part due to the different reaction ratios between two monomers and self-crosslinking density of DVB.

Syndecan-4 cytoplasmic domain could disturb the multilamellar vesicle

  • Kim, Suhk-Mann
    • Journal of the Korean Magnetic Resonance Society
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    • v.13 no.1
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    • pp.1-6
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    • 2009
  • Syndecan-4 cytoplasmic domain was tested to confirm the interactions with the bilayer membrane using $^{31}P$ solid-state NMR measurements. Syndecan-4 was known as a coreceptor with integrins in the cell adhesion. The syndecan-4 V region is not understood of its functional roles and tested its ability of the interaction with multilamellar vesicles. The $^{31}P$ powder pattern was dramatically changed and showed isotropic peak which imply the bilayer membrane changed its topology to the micelle-like structure. Especially, phosphatidylcholine membrane was affected this effect more than phosphatidylethanolamine membrane.

Crosslinking Reaction of Phenolic Side Chains in Silk Fibroin by Tyrosinase

  • Kang, Gyung-Don;Lee, Ki-Hoon;Ki, Chang-Seok;Park, Young-Hwan
    • Fibers and Polymers
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    • v.5 no.3
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    • pp.234-238
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    • 2004
  • Tyrosinase oxidizes the tyrosyl residues in silk fibroin (SF) with oxygen, resulting in the production of ο-quinone residues. Subsequently, the inter-or intramolecular crosslinks are formed by reaction with amino groups in through nonenzymatic process. The measurement of oxygen consumption proved that the tyrosyl residues in SF were mostly oxidized to quinone residues by tyrosinase. The reaction mechanisms were proposed in this study and the crosslinking reaction of ο-quinone residues and the enzymatic oxidation of tyrosyl residues could be confirmed by the measurements of UV, $^1$H-NMR and GFC.

Spectral and Thermal Properties of Some Uranyl Complexes of Some Schiff-Bases Derived from Glycylglycine

  • Sh. A. Sallam;M. I. Ayad
    • Journal of the Korean Chemical Society
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    • v.47 no.3
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    • pp.199-205
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    • 2003
  • Complexes of uranyl ion $UO^{+2}_2$with Schiff-bases obtained by condensing glycylglycine with salicylaldehyde; 2-hydroxy-1-naphthaldehyde, 2,3-dihydroxybenzaldehyde, and 2,4-dihydroxybenzaldehyde have been synthesized and characterized through elemental analysis, conductivity measurements, magnetic susceptibility determinations, u.v., i.r. and $^1H$ nmr spectra as well as d.t.a., t.g. and d.s.c. techniques. Structures and mechanisms of thermal decomposition are proposed.

NMR Study of the Electrooptic Material $KTiOPO_4(KTP)$ (Electrooptic 물질 $KTiOPO_4(KTP)$의 핵자기공명 연구)

  • 한정관;오동근;이창훈;이철의;김정남;김성철
    • Journal of the Korean Magnetics Society
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    • v.6 no.5
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    • pp.294-297
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    • 1996
  • We have carried out a $^{31}P$ nuclear magnetic resonance (NMR) study on the electrooptic material $KTiOPO_{4}(KTP)$. From the spin -lattice relaxation time ($T_{1}$) measurements at 17.9 MHz in the temperature range 77-390 K, two phase transitions associated with the change of the dominant charge carriers were observed and the activation energies were obtained in each phase.

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Synthesis and Spectroscopic Characterization of the New Sitting-atop Complexes from Reaction of Zirconyl Nitrate and Free Base meso-Tetraarylporphyrins in Mild Conditions

  • Dehghani, Hossein;Mansournia, Mohammad Reza
    • Bulletin of the Korean Chemical Society
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    • v.30 no.8
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    • pp.1715-1718
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    • 2009
  • A series of sitting-atop (SAT) complexes, [(ZrO)$H_2t(X)pp(NO_3)_2$], have been prepared via the reactions of free base meso-tetraarylporphyrins, $H_2$t(X)pp, with zirconyl nitrate hydrate, ZrO(N$O_3)_2{\cdot}xH_2$O. The products have been characterized by a variety of methods including $^1H\;NMR,\;^{13}C$ NMR, IR and UV-Vis spectroscopies, elemental analysis and conductance measurements. The data indicate that the meso-tetraarylporphyrins coordinate with two pyrrolenine nitrogen atoms to the zirconyl cation located above the distorted porphyrin plane and two protons remain on the pyrrole nitrogens. Such half sandwich-type sitting-atop complexes may be considered as models for the initial steps of the metallation of the macrocycles.