• Title/Summary/Keyword: $^1$H-NMR spectra

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Re-evaluation of physicochemical and NMR data of triol ginsenosides Re, Rf, Rg2, and 20-gluco-Rf from Panax ginseng roots

  • Cho, Jin-Gyeong;In, Seo-Ji;Jung, Ye-Jin;Cha, Byeong-Ju;Lee, Dae-Young;Kim, Yong-Bum;Yeom, Myeonghun;Baek, Nam-In
    • Journal of Ginseng Research
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    • v.38 no.2
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    • pp.116-122
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    • 2014
  • Ginseng roots were extracted with aqueous methanol, and extracts were suspended in water and extracted successively with ethyl acetate and n-butanol. Column chromatography using the n-butanol fraction yielded four purified triol ginseng saponins: the ginsenosides Re, Rf, Rg2, and 20-gluco-Rf. The physicochemical, spectroscopic, and chromatographic characteristics of the ginsenosides were measured and compared with reports from the literature. For spectroscopic analysis, two-dimensional nuclear magnetic resonance (NMR) methods such as $^1H$-$^1H$ correlation spectroscopy, nuclear Overhauser effect spectroscopy, heteronuclear single quantum correlation, and heteronuclear multiple bond connectivity were employed to identify exact peak assignments. Some peak assignments for previously published $^1H$-and $^{13}C$-NMR spectra were found to be inaccurate. This study reports the complete NMR assignment of 20-gluco-Rf for the first time.

$^{51}V$ NMR and Cyclic Voltammetry Studies on the Interaction of Vanadate and N-Benzyliminodiacetate in Aqueous Solution (Vanadate와 N-Benzyliminodiacetate 리간드의 상호작용에 대한 $^{51}V$ 핵자기공명분광법과 순환전압 - 전류법 연구)

  • Park, Chul-Jin;Park, Sam-Su;Lee, Man-Ho
    • Analytical Science and Technology
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    • v.12 no.3
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    • pp.184-189
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    • 1999
  • $^{51}V$ NMR and cyclic voltammetry studies on the interaction of vanadate and N-benzyliminodiacetate (Bz-IDA) in aqueous solution have been studied. From the NMR spectra two $^{51}V$ NMR peaks resulting at -515.5 and -500.1 ppm, due to the complexations between vanadate(V) and Bz-IDA at pH 5. has been observed. From the cyclic voltammograms the reduction-oxidation of the vanadate(V) complex has been found to be one-electron reaction.

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Syntheses and Spectroscopic Studies of Metal-Metal Bonded Complexes (Zr-Fe)

  • Ko, Jae-Jung
    • Bulletin of the Korean Chemical Society
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    • v.7 no.5
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    • pp.334-337
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    • 1986
  • The preparation of the metal-metal bonded complex $Cp_2ZrClFeCp(CO)_2$ has been achieved by the reaction of $Cp_2ZrCl_2$ and strong nucleophile $NaFeCp(CO)_2$. The more soluble metal-metal bonded complexes $Cp_2ZrRFeCp(CO)_2(R=CH_3,\;n-C_8H_{17}$) have also been prepared through the reaction of Cp$_{2}$ZrRCl and NaCpFe(CO)$_{2}$. The complexes were characterized by IR, Raman, $^{1}$H NMR and Mass spectra. The complete absorption (100-3800 cm$^{-1}$) spectra for the three metal-metal bonded molecules are reported and the bands of each vibration were assigned.

Antioxidative and Neuroprotective Effects of Extract and Fractions from Adenophora triphylla (잔대 추출물과 이들 분획물들의 항산화 및 뇌신경세포 보호 효과)

  • Chung, Mi Ja;Lee, Sanghyun;Park, Yong Il;Kwon, Ki Han
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.11
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    • pp.1580-1588
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    • 2016
  • The 70% ethanol extract from Adenophora triphylla showed a strong antioxidant effect and reduced cytotoxicity of $H_2O_2$ in SK-N-SH cells. The chloroform fraction from A. triphylla extract (AT-CH) among the six fractions showed strong DPPH radical and intracellular reactive oxygen species (ROS) scavenger effects and the highest protective effect against $H_2O_2$-induced SK-N-SH cell death. Bioactivity compounds were purified from AT-CH, and the chemical structures of the compounds were determined as ${\beta}$-sitosterol and daucosterol on the basis of $^1H-NMR$, $^{13}C-NMR$, and EI mass spectra. ${\beta}$-Sitosterol and daucosterol also had protective effects against oxidative stress in SK-N-SH cells. Phospho-p38 MAPK levels were elevated by $H_2O_2$ but were inhibited by treatment with AT-CH and phytosterols (${\beta}$-sitosterol and daucosterol) isolated from AT-CH. These results suggest that AT-CH has brain neuroprotective effects against oxidative stress ($H_2O_2$) by inhibiting activation of p38 pathways and scavenging intracellular ROS.

NMR Characterization of Oxidized Form of Human 8-kDa Dynein Light Chain

  • Shin, Jae-Sun;Jeong, Woo-Jin;Chi, Seung-Wook
    • Journal of the Korean Magnetic Resonance Society
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    • v.14 no.2
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    • pp.127-133
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    • 2010
  • Redox-dependent conformational change of human 8-kDa Dynein light chain (LC8) plays important role in regulating NF-${\kappa}B$ signaling pathway. In this study we characterized the structural states of the oxidized and reduced forms of LC8 by using NMR spectroscopy. The $^1H-^{15}N$ 2D HSQC spectra of oxidized LC8 indicated that no significant change in tertiary structure of LC8 occurred upon oxidation. The chemical shift perturbations of LC8 upon oxidation suggest a redox-dependent quaternary structural change.

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.

Deuterium Naturally Present in Solvent and Site-Specific Isotope Population of Deuterium-Enriched Solute

  • Hwang, Ryeo Yun;Han, Oc Hee;Lee, Juhee;Kim, Eun Hee
    • Bulletin of the Korean Chemical Society
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    • v.34 no.10
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    • pp.2959-2962
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    • 2013
  • As the concentration of aqueous $CD_3OH$ solutions was decreased, the OD peaks in $^2H$ NMR spectra grew relative to the $CD_3$ peaks. Isotope impurity for OH groups of $CD_3OH$ and deuterium naturally present in water contributed to the OD peaks. Using these peak area data, the site-specific isotope populations of isotope enriched chemicals were measured. In addition, the method using both $^1H$ and $^2H$ NMR spectroscopy was demonstrated with neat $CD_3OH$ to measure the site-specific isotope populations. The results indicate that although it represents only ~0.015% of hydrogen isotopes, the deuterium naturally present in solvents cannot be ignored, especially when the concentration of deuterium-enriched solutes is varied. Proton/deuteron exchange between methyl and methyl/hydroxyl groups was confirmed to be negligible, while that among hydroxyl groups was detectable.

Structural Study of the Cytosolic C-terminus of Vanilloid Receptor 1

  • Seo, Min-Duk;Won, Hyung-Sik;Oh, Uh-Taek;Lee, Bong-Jin
    • Journal of the Korean Magnetic Resonance Society
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    • v.11 no.2
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    • pp.85-94
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    • 2007
  • Vanilloid receptor I [transient receptor potential vanilloid subfamily member 1 (TRPV1), also known as VR1] is a non-selective cationic channel activated by noxious heat, vanilloids, and acid, thereby causing pain. VR1 possesses six transmembrane domain and N-and C-terminus cytosolic domains, and appears to be a homotetramer. We studied the structural properties of Cterminus of VR1 (VR1C) using CD and NMR spectroscopy. DPC micelles, with a zwitterionic surface, and SDS micelles, with a negatively charged surface, were used as a membrane mimetic model system. Both SDS and DPC micelles could increase the stability of helical structures and/or reduce the aggregation form of the VR1C. However, the structural changing mode of the VR1C induced by the SDS and DPC micelles was different. The changes according to the various pHs were also different in two micelles conditions. Because the net charges of the SDS and DPC micelles are negative and neutral, respectively, we anticipate that this difference might affect the structure of the VR1C by electrostatic interaction between the surface of the VR1C and phospholipids of the detergent micelles. Based on these similarity and dissimilarity of changing aspects of the VR1C, it is supposed that the VR1C probably has the real pI value near the pH 7. Generally, mild extracellular acidic pH ($6.5{\sim}6.8$) potentiates VRI channel activation by noxious heat and vanilloids, whereas acidic conditions directly activate the channel. The channel activation of the VRI might be related to the structural change of VR1C caused by pH (electrostatic interactions), especially near the pH 7. By measuring the $^1-^{15}N$ TROSY spectra of the VR1C, we could get more resolved and dispersed spectra at the low pH and/or detergent micelles conditions. We will try to do further NMR experiments in low pH with micelles conditions in order to get more information about the structure of VR1C.

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Isolation and Characterization of α-Glucosidase Inhibitor Produced by Bacillus sp. SKU31-1 Strain (Bacillus sp. SKU31-1가 생산하는 α-Glucosidase 저해제 분리 및 특성 조사)

  • Kim, Shin-Duk
    • Korean Journal of Microbiology
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    • v.50 no.4
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    • pp.381-383
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    • 2014
  • In the course of screening for ${\alpha}$-glucosidase inhibitor produced by microorganism, the active compound was isolated from the culture filtrate of Bacillus sp. SKU31-1 using a series of chromatography procedures. The structure of the active compound was elucidated as 5-amino-1-hydroxymethyl-1, 2, 3, 4-cyclohexanetetrol on the basis of spectroscopic evidence obtained and comparison with data from the literature. The active compound showed potent inhibitory activity against ${\alpha}$-glucosidase with an $IC_{50}$ value of $1.9{\mu}M$ for maltose and 4.9 mM for sucrose. A Lineweaver-Burk plot indicated that its inhibition of ${\alpha}$-glucosidase was competitive, with a $K_i$ value of 0.15 mM.

Development plan for a persistent 1.3 GHz NMR magnet in a new MIRAI project on joint technology for HTS wires/cables in Japan

  • Yanagisawa, Y.;Suetomi, Y.;Piao, R.;Yamagishi, K.;Takao, T.;Hamada, M.;Saito, K.;Ohki, K.;Yamaguchi, T.;Nagaishi, T.;Kitaguchi, H.;Ueda, H.;Shimoyama, J.;Ishii, Y.;Tomita, M.;Maeda, H.
    • Superconductivity and Cryogenics
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    • v.20 no.2
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    • pp.15-22
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    • 2018
  • The present article briefly overviews the plan for a new project on joint technology for HTS wires/cables and describes the development plan for the world's highest field NMR magnet, which is a major development item in the project. For full-fledged social implementation of superconducting devices, high temperature superconducting (HTS) wire is a key technology since they can be cooled by liquid nitrogen and they can generate a super-high magnetic field of >>24 T at liquid helium temperatures. However, one of the major drawbacks of the HTS wires is their availability only in short lengths of a single piece of wire. This necessitates a number of joints being installed in superconducting devices, resulting in a difficult manufacturing process and a large joint resistance. In Japan, a large-scale project has commenced, including two technical demonstration items: (i) Development of superconducting joints between HTS wires, which are used in the world's highest field 1.3 GHz (30.5 T) NMR magnet in persistent current mode; the joints performance is evaluated based on NMR spectra for proteins. (ii) Development of ultra-low resistive joints between DC superconducting feeder cables for railway systems. The project starts a new initiative of next generation super-high field NMR development as well as that of realization of better superconducting power cables.

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