• 제목/요약/키워드: H-NMR

검색결과 2,740건 처리시간 0.033초

Constructing Overhauser Dynamic Nuclear Polarization-Nuclear Magnetic Resonance System Using Benchtop Electron Paramagnetic Resonance Spectrometer

  • Saun, Seung-Bo;Kim, JiWon;Han, Oc Hee
    • 한국자기공명학회논문지
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    • 제22권2호
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    • pp.34-39
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    • 2018
  • The Nuclear Magnetic Resonance (NMR) technique using Dynamic Nuclear Polarization (DNP) procedures is one of the promising techniques that enable overcoming low sensitivity problems in NMR spectroscopy. We constructed an ODNP-NMR system using a commercial benchtop EPR spectrometer. The $^1H$ NMR peak area of water in aqueous solutions of 4-hydroxy-TEMPO was enhanced more than 95 times in the ODNP-NMR experiments. Our signal enhancement results were about 55% of the previously reported result. This could be due to non-uniform microwave power over a sample and unwanted sample heating by microwave. However, this portable ODNP-NMR spectrometer will be eventually useful for site-specific detection with nano-scale spatial resolutions and molecular dynamics studies with significantly improved signal sensitivity.

Liquid Chromatography-Solid Phase Extraction-NMR (LC-SPE-NMR) Analysis of Liquid Crystalline Mixtures

  • Park, Gregory Hyung-Jin;Park, Ae-Na;Rho, Kyung-Rae;Shin, Jong-Ho;Kim, Yeong-Jeon;Jo, Sung-Chan;Oh, Weon-Sik
    • 한국자기공명학회논문지
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    • 제15권1호
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    • pp.14-24
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    • 2011
  • We have performed Liquid Chromatography-Solid Phase Extraction-NMR (LC-SPE-NMR) analysis for liquid crystalline mixture and elucidated the structures of selected components by NMR spectra. Combining the results of one-dimensional 1H experiments as well as homonuclear and heteronuclear two-dimensional experiments, we could analyze the molecular structure of the liquid crystal singles whose structure had not been interpretable by mass spectrometry alone.

Molecular Dynamics in Paraelectric Phase of KH2PO4 Crystals Studied by Single Crystal NMR and MAS NMR

  • Paik, Younkee;Chang, Celesta L.
    • 한국자기공명학회논문지
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    • 제17권1호
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    • pp.19-23
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    • 2013
  • The temperature dependences of the NMR spectrum and the spin-lattice relaxation times in $KH_2PO_4$ were investigated via single-crystal NMR and MAS NMR. The stretched-exponential relaxation that occurred because of the distribution of correlation times was indicative of the degree of the distribution of the double-well potential on the hydrogen bond. The behaviors responsible for the strong temperature dependences of the $^1H$ and $^{31}P$ spin-lattice relaxation times in the rotating frame $T_{1{\rho}}$ in $KH_2PO_4$ are likely related to the reorientational motion of the hydrogen-bond geometry and the $PO_4$ tetrahedral distortion.

High-pressure NMR application for α-synuclein

  • Kim, Jin Hae
    • 한국자기공명학회논문지
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    • 제26권2호
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    • pp.21-23
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    • 2022
  • High-pressure (HP) NMR is a powerful method to elucidate various structural features of amyloidogenic proteins. Following the previous mini-review recapitulating the HP-NMR application for amyloid-β peptides of the last issue [J. H. Kim, J. Kor. Mag. Reson. Soc. 26, 17 (2022)], the recent advancements in the HP NMR application for α-synuclein (α-Syn) are briefly summarized and discussed here. Although α-Syn is a well-known intrinsically disordered protein (IDP), several studies have shown that it can also exhibit heterogeneous yet partially folded conformations, which may correlate with its amyloid-forming propensity. HP NMR has been a valuable tool for investigating the dynamic and transient structural features of α-Syn and has provided unique insights to appreciate its aggregation-prone characters.

1H NMR-based metabolite profiling of diet-induced obesity in a mouse mode

  • Jung, Jee-Youn;Kim, Il-Yong;Kim, Yo-Na;Kim, Jin-Sup;Shin, Jae-Hoon;Jang, Zi-Hey;Lee, Ho-Sub;Hwang, Geum-Sook;Seong, Je-Kyung
    • BMB Reports
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    • 제45권7호
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    • pp.419-424
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    • 2012
  • High-fat diets (HFD) and high-carbohydrate diets (HCD)-induced obesity through different pathways, but the metabolic differences between these diets are not fully understood. Therefore, we applied proton nuclear magnetic resonance ($^1H$ NMR)-based metabolomics to compare the metabolic patterns between C57BL/6 mice fed HCD and those fed HFD. Principal component analysis derived from $^1H$ NMR spectra of urine showed a clear separation between the HCD and HFD groups. Based on the changes in urinary metabolites, the slow rate of weight gain in mice fed the HCD related to activation of the tricarboxylic acid cycle (resulting in increased levels of citrate and succinate in HCD mice), while the HFD affected nicotinamide metabolism (increased levels of 1-methylnicotineamide, nicotinamide-N-oxide in HFD mice), which leads to systemic oxidative stress. In addition, perturbation of gut microflora metabolism was also related to different metabolic patterns of those two diets. These findings demonstrate that $^1H$ NMR-based metabolomics can identify diet-dependent perturbations in biological pathways.

Structural stability of CD1 domain of human mitotic checkpoint serine/threonine-protein kinase, Bub1

  • Kim, Hyun-Hwi;Song, Hyun-Kyu;Lee, Bong-Jin;Park, Sung Jean
    • 한국자기공명학회논문지
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    • 제19권2호
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    • pp.88-94
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    • 2015
  • Bub1 is one of the spindle checkpoint proteins and plays a role in recruitment of the related proteins to kinetochore. Here, we studied the structural characteristic of the evolutionarily conserved 160 amino acid region in the N-terminus (hBub1 CD1), using Circular Dichroism (CD) and NMR. Our CD results showed that hBub1 CD1 is a highly helical protein and its structure was affected by pH: as pH was elevated to basic pH, the helical propensity increased. This could be related to the surface charge of the hBub1 CD1. However, the structural change did not largely depend on the salt concentration, though the thermal stability a little increased. The previous NMR analysis revealed that the hBub1 CD1 adopts eight helices, which is consistent with the CD result. Our result would be helpful for evaluating the molecular mechanism of the hBub1 CD1 and protein-protein interactions.

황정(黃精) 추출물의 화학구조 결정에 관한 연구(I) (Studies on Chemical Structure Determination of Polygonatum sibiricum Extracts(I))

  • 신동수;윤중호;박주희;권기락;안철진;주우홍;강진호;문병호
    • 생명과학회지
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    • 제9권2호
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    • pp.207-211
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    • 1999
  • 당뇨에 대한 황정의 약효가 알려지면서 황정의 생리활성 연구가 많이 진행되고 있다. 따라서 본 연구에서는 황정 추출물의 hexane층에서 생리활성 물질로 기대되는 새로운 화합물 I를 분리하고, 분리한 화합물의 화학적인 구조를 분광학적인 방법에 의하여 확인하였다. 1H-nmr, 13C-nmr, DEPT135, COSY, HMQC, HMBC 스펙트럼 및 MS 스펙트럼으로 확인하여 화합물 I의 구조가 9,12-(9E, 12E)-octadecadienoic acid 임을 알 수 있었다.

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가스크로마토그라피 분석을 통한 $\alpha$-브로모-$\omega$ -플루오로알칸의 효율적 합성 (Effective Synthesis of $\alpha$--Bromo-$\omega$ -fluoroalkane with Analysis of Gas-chromatography)

  • 유국현
    • 대한화학회지
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    • 제39권5호
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    • pp.414-420
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    • 1995
  • 디브로모알칸, AgF 및 tetrabutylammoniumbromide(TBABr)를 acetonitrile 용매하에서 $82^{\circ}C$에서 20분간 반응시켜 19~55%의 수율로 $\alpha$-브로모-$\omega$-플르오르알칸을 합성하였다. 반응 조건은 가스 크로마토그라피를 이용하여 조절하였으며, 반응 생성물인 $\alpha$-브로모-$\omega$-플르오르알칸, 디플르오로알칸, 플르오로알켄 및 브로모알켄을 1^H$ NMR 및 $19^F$ NMR로 확인하였다.

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Complete assignments of $^{1}H$ and $^{13}C NMR$ spectra of Chivosazole F

  • Park, Jung-Rae;Jongheonn Shin;Kim, Jin-Cheol;Ahn, Jong-Woong
    • 한국자기공명학회논문지
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    • 제5권2호
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    • pp.91-98
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    • 2001
  • The $^1$H and $^{13}$ C NMR spectra of chivosazole F from Sorangium cellulosum were completely assigned by a combination of ID and 2D NMR techniques. The configurations of double bonds were confirmed from the ROESY spectra. The stereochemistry at asymmetric carboncenters was partially assigned on the basis of the results of NOE analysis.

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Influence of Hot Pressing on the Pore Structure of Nafion Electrolyte Membrane Investigated by 1H NMR

  • Jeonga, Soon-Yong;Han, Oc-Hee
    • Bulletin of the Korean Chemical Society
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    • 제30권7호
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    • pp.1559-1562
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    • 2009
  • The influence of hot pressing on the pore structures of Nafion membranes was investigated by observing the Nafion before and after hot pressing with $^1H$ nuclear magnetic resonance (NMR) spectroscopy. The freezing point depression and chemical shift data of water in the Nafion indicated the presence of two different pore size ranges in Nafion. Hot pressing mainly reduced the sizes and number of the big pores. The reduction of water uptake and proton conductivity after hot pressing was explained by this variation of pore size and number. We demonstrated the potential application of chemical shift data and NMR cryoporometry experiments to measure the relative pore sizes, on a nano scale, and numbers.