• 제목/요약/키워드: NMR measurements

검색결과 157건 처리시간 0.024초

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
    • 한국자기공명학회논문지
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    • 제14권2호
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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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    • 한국초전도학회 2000년도 High Temperature Superconductivity Vol.X
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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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    • 제11권2호
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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
    • 한국자기공명학회논문지
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    • 제23권1호
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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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    • 제17권5호
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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
    • 한국자기공명학회논문지
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    • 제13권1호
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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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    • 제5권3호
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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
    • 대한화학회지
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    • 제47권3호
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    • pp.199-205
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    • 2003
  • 우라닐 이온, $UO^+_2$와 Schiff-base 와의 착화합물이 글리실글라이신과 살리실알데히드, 2-히드록시-1-나프트알데히드, 2,3-디히드록시 벤즈알데히드 그리고 2,4-디히드록시 벤즈알데히드와의 축합에 의해 합성되었으며 이들 착화합물의 특성을 원소분석, 전도도 측정, 자기화율 측정, UV, IR, NMR 스펙트라와 DTA, TG, DSC 결과를 이용하여 조사하였다. 구조와 열분해 메카니즘이 제안되었다.

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

  • 한정관;오동근;이창훈;이철의;김정남;김성철
    • 한국자기학회지
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    • 제6권5호
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    • pp.294-297
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    • 1996
  • Electrooptic 물질 $KTiOPO_{4}(KTP)$에 대하여 $^{31}P$ 핵자기공명을 수행하였다. 17.9 MHz의 공명 주파수에서 77-390 K 온도 범위내에서의 스핀-격자 완화 시간($T_{1}$) 측정으로부터 전도 기구의 변화에 따른 두 개의 상전이를 관측하였으며, 이에 따른 각 상에서의 활성화 에너지를 구할 수 있었다.

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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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    • 제30권8호
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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.