• Title/Summary/Keyword: Solution NMR

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Study of thermal stability on PVC using mixed metal soap and stabilizer (복합금속비누와 안정화조제를 이용한 PVC의 열안정화에 대한 연구)

  • Jeon, In-Ki;Ahn, Sung-Hwan;Chung, Kwang-Bo
    • Journal of the Korean Applied Science and Technology
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    • v.27 no.4
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    • pp.552-558
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    • 2010
  • Zinc soap and Zn/Ba mixed metal soap were synthesized and PVC plastisol with mixed metal soap and various costabilizers were also synthesized with good structures and characterized by IR and $^1H$-NMR. The IR spectrums and $^1H$-NMR spectrums of the synthesized soaps were in very good accordance with the structures proposed by earlier workers. In using phosphite as a costabilizer, TIDP phosphite was shown to be the excellent thermal stabilization effect at the low temperature and TNPP phosphite was shown to be the excellent thermal stabilization effect at the high temperature. In case of antioxidant, it was revealed that antioxidant was not effective in the low temperature thermal stabilization effect while highly effective in the high temperature thermal stability. $NaClO_4$ solution with sorbitol solvent had the best thermal stabilization effect among $NaClO_4$ solution series at low and high temperature.

Solution Structure of the D/E Helix Linker of Skeletal Troponin-C: As Studied by Circular Dichroism and Two-Dimensional NMR Spectroscopy

  • 이원태;G. M. Anatharamaiah;Herbert C. Cheung;N. Rama Krishna
    • Bulletin of the Korean Chemical Society
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    • v.19 no.1
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    • pp.57-62
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    • 1998
  • We have synthesized a 17-residue peptide with the amino acid sequence RQMKEDAKGKSEEELAD corresponding to residues 84-100 of chicken skeletal troponin C. This stretch of the protein sequence is in the middle one-third of the 32-residue 9-turn α-helix that connects the two globular domains of the dumbell-shaped molecule and includes the D/E linker helix. We describe here the solution conformation of the helix linker as studied by circular dichroism (CD) and two-dimensional nuclear magnetic resonance (2-D NMR) spectroscopy. The NOE connectivities together with the vicinal $^3J_{N{\alpha}}$ coupling constants suggest that the peptide exists in a fast conformational equilibrium among several secondary structure: a nascent helix near the N-terminus, a helix, and a substational population of extended and random coil forms. In addition, two interresidue α-α NOEs are observed suggesting a bent structure with a bend that includes the single glycine in position 92. These results are consistent with the ideas that in neutral solution the D/E linker region of the central helix in troponin C can adopt a helical conformation and the central helix may have a segmental flexibility around Gly 92.

Synthesis of n-nitrilotris(methylene) Phosphonic Acid Potassium Salt as a Draw Solute in Forward Osmosis Process (정삼투 분리막 공정 적용을 위한 n-nitrilotris(methylene) Phosphonic Acid Potassium Salt 유도용질의 합성)

  • Lee, Hye-Jin;Choi, Jin-Il;Kwon, Sei;Kim, In-Chul
    • Membrane Journal
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    • v.28 no.5
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    • pp.368-377
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    • 2018
  • The n-nitrilotris(methylene) phosphonic acid (NTPA) potassium salt was synthesized as a draw solute for forward osmosis. NTPA-4K, NTPA-5K and NTPA-6K were synthesized by varying the content of KOH added to NTPA and confirmed by $^1H$-NMR and $^{13}C$-NMR. The osmotic pressure, viscosity, water flux and reverse salt flux were measured to characterize the draw solute. In the forward osmosis process when distilled water was used as a feed solution and 0.5 M of NTPA-4K, NTPA-5K and NTPA-6K were used as a draw solution, the water flux was 35.8, 38.8 and 42.2 LMH, the reverse salt flux was 5.4, 6.9 and 7.4 gMH, respectively. It was confirmed that the water flux was lower than the conventional NaCl draw solution, but the reverse salt flux was much lower. In order to recover the diluted draw solution, nanofiltration was conducted. The results showed that the draw solute could be retained by above 90%.

Isolation and Identification of Degradation products of Herbicide Propanil in Solution (제초제(除草劑) Propanil의 용액중(溶液中) 분해산물(分解産物)의 분리(分離) 및 동정(同定))

  • Kim, Jang Eok;Shin, Yun Gyo;Hong, Jong Uck
    • Current Research on Agriculture and Life Sciences
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    • v.5
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    • pp.27-32
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    • 1987
  • To isolate and identify degradation products of propanil in solution which propanil concentration was 2000ppm with a certain temperature, degradation products and pathway were investigated every 2 weeks for 12 weeks. Extracted mixture was developed with benzene on TLC plate, and Rf values of isolated DCA and TCAB were 0.65 and 0.94 respectively. At the GC analysis, propanil and its degradation products could seperate at the column temperature $200^{\circ}C$, but in order to more good resolution, the column temperature of DCA and TCAB was $140^{\circ}C$ and $250^{\circ}C$ respectively. Functional group of OCA was determined by IR spectrum $3400cm^{-1}$ and $800cm^{-1}$. Proton peaks of OCA were NMR spectrum $6.7{\delta}$ and $3.7{\delta}$. As the results, the major degradation products of propanil in solution were seperated on TLC plate, and thus identified by the analysis of GC, IR and NMR. Proposed degradation pathway of propanil in solution was from DCA to TCAB.

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Exploitation of the biologically active components in Youngia sonchifolia Max (고들빼기 생리활성물질의 검색)

  • Shin, Soo-Cheol
    • Applied Biological Chemistry
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    • v.36 no.2
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    • pp.134-137
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    • 1993
  • Yongia sonchifolia Max. has been used as raw materials of traditional Kimchi and medicinal herb in Korea. This study was performed to investigate biologically active components in the plant. First, the writer carried out the experiment of antitumor screening test against Sarcoma-180A and the cytotoxic activity against Chinese hamster V-79 cells with methanol extract of the plant. And the aqueous solution of the extract from roots of Youngia sonchifolia Max. was partitioned into n-hexane. The concentrated extract of n-hexane layer was chromatographed on silica gel column and developed with n-hexane and ethylacetate. Two yellow elutes, on concentration, were recrystallized from ethylacetate, and the $R_f$ value of TLC of the crystal was 0.43. After analysis by $^{1}H-NMR$, $^{13}C-NMR$ and MS to confirm the structure, the author could identify the compound as bauerenyl acetate, a naturally occurring pentacyclic triterpene. The crystal was colorless plate and m.p. was $280{\sim}282^{\circ}C$.

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Mainchain NMR Assignments and secondary structure prediction of the C-terminal domain of BldD, a developmental transcriptional regulator from Streptomyces coelicolor A3(2)

  • Kim, Jeong-Mok;Won, Hyung-Sik;Kang, Sa-Ouk
    • Journal of the Korean Magnetic Resonance Society
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    • v.17 no.1
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    • pp.59-66
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    • 2013
  • BldD, a developmental transcription factor from Streptomyces coelicolor, is a homodimeric, DNA-binding protein with 167 amino acids in each subunit. Each monomer consists of two structurally distinct domains, the N-terminal domain (BldD-NTD) responsible for DNA-binding and dimerization and the C-terminal domain (BldD-CTD). In contrast to the BldD-NTD, of which crystal structure has been solved, the BldD-CTD has been characterized neither in structure nor in function. Thus, in terms of structural genomics, structural study of the BldD-CTD has been conducted in solution, and in the present work, mainchain NMR assignments of the recombinant BldD-CTD (residues 80-167 of BldD) could be achieved by a series of heteronuclear multidimensional NMR experiments on a [$^{13}C/^{15}N$]-enriched protein sample. Finally, the secondary structure prediction by CSI and TALOS+ analysis using the assigned chemical shifts data identified a ${\beta}-{\alpha}-{\alpha}-{\beta}-{\alpha}-{\alpha}-{\alpha}$ topology of the domain. The results will provide the most fundamental data for more detailed approach to the atomic structure of the BldD-CTD, which would be essential for entire understanding of the molecular function of BldD.

An NMR Study on Complexation of Cesium Ion by p-tert-Butylcalix[6]arene Ethyl Ester

  • Chung, Kee-Choo;Namgoong, Hyun;Lee, Jo-Woong
    • Bulletin of the Korean Chemical Society
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    • v.25 no.5
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    • pp.609-616
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    • 2004
  • Complexation of cesium ion by p-tert-butylcalix[6]arene ethyl ester was studied by NMR spectroscopy in nonpolar $CDCl_3$ and polar acetone-$d_6$ and the results were compared with each other. Analysis of temperature dependent $^1H$ spectra and titration curves reveals that both solvents result in a 1 : 1 cone-form complex with nonpolar $CDCl_3$yielding a more tightly bound one than acetone-$d_6$. Unexpectedly, at very low temperature, we have found that two phenyl ring proton peaks of equal intensity appear both in $CDCl_3$and in acetone-$d_6$ solution which gradually collapse and eventually coalesce into a single line as temperature is raised. This observation could be interpreted in terms of the chemical exchange through direct and/or indirect interconversion between two equivalent conformations possible the complex in both solvents over the temperature range observed. And broadening of $^{133}Cs$ (I = 7/2) nmr line with increasing temperature has also been observed, indicating the exchange of $^{133}Cs$ ion between the complex and the solvent. From numerical fitting of lineshape changes for one-dimensional $^1H$ and $^{133}Cs$ spectra, the exchange rate constants and other relevant parameters for this conformational interconversion and the complex-solvent exchange were deduced.

Solution State Structure of pB1, the Mimotopic Peptide of Apolipoprotein B-100, by NMR

  • Lee, Sung-Ran;Kim, Dae-Sung;Kim, Hyo-Joon;Lee, Yong-Woo;Won, Ho-Shik
    • Bulletin of the Korean Chemical Society
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    • v.25 no.12
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    • pp.1845-1849
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    • 2004
  • Apolipoprotein B-100 (Apo-B100) is a major protein component for low density lipoproteins (LDL). A number of mimetic peptides of Apo-B100 were screened from the phase-displayed random peptide library by utilizing monoclonal antibody (B9). Mimetic peptide for B9 epitope against apo B-100 was CRNVPPIFNDVYWIAF (pB1). From the BLAST search, the mimetic peptide pB1 had 40% homology with apo B-100. As a result of the structural determination of this mimotope using homo/hetero nuclear 2D-NMR techniques and NMR-based distance geometry (DG)/molecular dynamic (MD) computations, DG structure had low penalty value of 0.3-0.6 ${\AA}^2$ and the total RMSD was 0.5-1.5 ${\AA}. Moreover, pB1 structure included a weak $3_{10}$-helix from $Ile^7$,/TEX> to $Trp^{13}$.

Biochemical and NMR Characterization of MTH1880 Mutant Proteins for Folding-Unfolding Studies

  • Kim, Hee-Youn;Ryu, Soo-Young;Yun, Ji-Hye;Kim, Suhk-Mann;Chang, Ik-Soo;Lee, Weon-Tae
    • Bulletin of the Korean Chemical Society
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    • v.31 no.12
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    • pp.3521-3524
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    • 2010
  • MTH1880 is a hypothetical protein derived from Methanobacterium thermoautotrophicum, thermophilic methanogen. The solution structure determined by NMR spectroscopy showed that it has a novel $\alpha+\beta$-fold with a highly acidic ligand binding pocket. Since MTH1880 maintains its ultra-stable structural characteristics at both high temperature and pressure, it has been considered as an excellent model for studying protein folding. To initiate the structural and folding study of MTH1880 in proving its unusual stability, we performed the site directed mutagenesis and biochemical analysis of MTH1880 mutants. Data from circular dichroism and NMR spectroscopy suggest that the point mutations perturbed the structural stability of protein even though the secondary structure is retained. This study will provide the useful information in understanding the role of participating residues during folding-unfolding process and our result will be used in designing further folding experiments for hyper-thermopile proteins like MTH1880.

The Characterization of Borohydride-Stabilized Nanosilvers in Laponite Sol Using 1H NMR: Its Ligand Exchange Reactions with MUA and TOP

  • Seo, Jae-Seok;Son, Dong-Min;Lee, Han-Na;Kim, Jee-Kwang;Kim, You-Hyuk
    • Bulletin of the Korean Chemical Society
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    • v.30 no.11
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    • pp.2651-2654
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    • 2009
  • In borohydride-protected nanosilvers in laponite sol, the silver particles aggregate to form short chains and a dumbbell shape. The $^{1}H$ NMR measurements in this study represent, to our knowledge, the first observation of proton resonances of borohydride-protected nanosilvers in aqueous solution. Borohydride on nanosilver can be exchanged with 11-mercaptoundecanoic acid (MUA) or trioctylphosphine (TOP). Transmission electron microscopy and UV-Vis spectroscopy data show that the number of aggregated silver nanoparticles decreases upon addition of aforementioned ligands due to the formation of silver MPCs (monolayer-protected clusters). Adsorption of MUA or TOP on nanosilver is confirmed through the observation of broad proton resonances of MPCs in $^{1}H$ NMR spectra.