• Title/Summary/Keyword: Solution NMR

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Preparation of Surface-anionized Poly(vinyl alcohol-co-methacrylic acid) Hydrogel Beads (표면에 음이온이 도입된 폴리(비닐 알코올-co-메타아크릴산) 하이드로젤 입자의 제조)

  • 윤주표;박연흠;이세근;박기홍;이철주
    • Polymer(Korea)
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    • v.27 no.2
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    • pp.159-166
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    • 2003
  • For the purpose of obtaining surface-anionized poly(vinyl alcohol) (PVA) hydrogel beads, vinyl acetate(VAc) and methacrylic acid(MMA) were copolymerized by the suspension polymerization technique and followed by the saponification. It was confirmed by $^1$H-NMR that the copolymerized microspheres contained carboxylic acid groups in their surface. poly(VAc-co-MAA) microspheres were completely saponified in the heterogeneous system. The saponification reaction was laster than that of PVAc microspheres. We observed the swelling property of saponified PVA microspheres treated in the acidic solution and in the alkaline solution successively. Saponified microspheres shrank in acidic solution and swelled in alkaline solution respectively, which was reversible. from the result, saponified microspheres were highly water-absorbing hydrogel beads and were certified -COOH group at their surface by $^1$H-NMR and FT-IR.

Comparative analysis of glycerin in cosmetics by LC/MS and 1H NMR (LC/MS와 1H NMR을 이용한 화장품속의 글리세린 비교분석)

  • Park, Gyo-Beom;Park, Chan Jo;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.20 no.5
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    • pp.400-405
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    • 2007
  • The comparative analysis of glycerin in cosmetic samples was carried out by LC/MS and $^1H$ NMR spectrometry. For the LC/MS analysis, aqueous solution was controlled in strong basic condition with sodium hydroxide, and benzoyl chloride was added to the solution for the derivatization of glycerin. The derivative was extracted using pentane and analyzed by the LC/MS. For the $^1H$ NMR analysis, sample was directly dissolved in $D_2O$ solvent without pretreatment. The quantitative analysis of glycerin was done by $^1H$ NMR ERETIC method. The analysis results of LC/MS and $^1H$ NMR showed that the calibration curves were a good linearity with $r^2=0.9991$ in the range of 0.1 to $10{\mu}g/mL$ and $r^2=1$ in the range of 25 to $500{\mu}g/mL$, respectively.

Solution and Solid-state Vanadium-51 NMR Studies of Vanadium (V) Complexes

  • Lee, Man-Ho
    • Journal of the Korean Magnetic Resonance Society
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    • v.1 no.1
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    • pp.1-6
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    • 1997
  • Several dioxovanadate (V) complexes are synthesized and studied by solution and solid-state 51V NMR spectroscopy. In the results, large 51V chemical shift anisotropy ({{{{ DELTA delta }}a = -800 ∼720 ppm) and quadrupole coupling (e2q /h = 7.50 ∼ 9.16 MHz) were observed in the solid-state complexes. The isotropic chemical shifts of the solid samples are very close to the values obtained from solution measurements.

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Structure of CT16 in the C-terminal of Amyloid Precursor Protein Studied by NMR Spectroscopy

  • Lee, Kyoung-Ik;Baek, Dong-Ha;Shin, Song-Yub;Kim, Yang-Mee
    • Journal of the Korean Magnetic Resonance Society
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    • v.8 no.1
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    • pp.19-27
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    • 2004
  • C-terminal fragments of APP (APP-CTs), that contain complete Abeta sequence, are found in neuritic plaques, neurofibrillary tangles and the cytosol of lymphoblastoid cells obtained from AD patients. CT16, Lys649-Asp664 (KKQYTSIHHGVVEVD) has been known as the most toxic part in the C-terminal fragment of amyloid precursor protein (APP). The solution structure of CT16 was investigated using NMR spectroscopy in various membrane-mimicking environments. According to Circular Dichroim (CD) spectra, CT16 has a random structure in aqueous solution, while conformational change was induced by addition of TFE and SDS micelle. Tertiary structure as determined by NMR spectroscopy shows that CT16 has a ${\beta}$-turn conformation in trifluoroethanol-containing aqueous solution.

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Solution Structure of pA2, the Mimotopic Peptide of Apolipoprotein A-I, by NMR Spectroscopy

  • Won, Ho-Shik
    • Bulletin of the Korean Chemical Society
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    • v.32 no.11
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    • pp.4016-4020
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    • 2011
  • A number of mimetic peptides of apolipoprotein A-I, a major component for high density lipoproteins (HDL), were screened from the phase-displayed random peptide library by utilizing monoclonal antibodies (A12). A mimetic peptide for A12 epitope against apolipoprotein A-I was selected as FVLVRDTFPSSVCCP(pA2) exhibiting 45% homology with Apo A-I in the BLAST search. Solution structure determination of this mimotope was made by using 2D-NMR data and NMR-based distance geometry (DG)/molecular dynamic calculations. The resulting DG structures had low penalty value of 0.4-0.6 ${\AA}^2$ and the total RMSD of 0.7-1.7 ${\AA}$. The mimotope pA2 exhibited a characteristic ${\beta}$-turn conformation from Val[2] to Phe[8] near Pro[9] residue.

NMR Study of Poly(γ-Glutamic Acid)Hydrogels Prepared by γ-Irradiation : Characterization of Bond Formation and Scission

  • 한옥희;최혁준
    • Bulletin of the Korean Chemical Society
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    • v.20 no.8
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    • pp.921-924
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    • 1999
  • Hydrogels were prepared from poly( Υ-glutamic acid) (PGA) solution by g-irradiation of 90 kGy and 170 kGy. The hydrogels were more cross-linked with a higher dosage g-irradiation and completely hydrolyzed at 85℃ within 4 hours resulting in homogeneous solution. NMR techniques were employed to clarify chemical bond formation and scission involved during γ-irradiation and hydrolysis. Characterization of these samples was carried out by taking both liquid state and solid state NMR spectra of PGA and hydrolyzed hydrogels and comparison of these spectra with the solid state NMR spectra of hydrogels. Our results indicate that complicated chemical bond formation and scission have occurred during hydrolysis and γ-irradiation. The samples prepared with higher dosage of γ-irradiation showed more diverse chemical bond formation and scission.

In-cell nuclear magnetic resonance spectroscopy for studying intermolecular interactions

  • Sugiki, Toshihiko;Lin, Yuxi;Lee, Young-Ho
    • Journal of the Korean Magnetic Resonance Society
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    • v.23 no.1
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    • pp.33-39
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    • 2019
  • Studies on the interactions of proteins with partner molecules at the atomic resolution are essential for understanding the biological function of proteins in cells and for developing drug molecules. Solution NMR spectroscopy has shown remarkably useful capability for investigating properties on the weak to strong intermolecular interactions in both diluted and crowded solution such as cell lysates. Of note, the state-of-the-art in-cell NMR method has made it possible to obtain atomistic information on natures of intermolecular interactions between target proteins with partner molecules in living cells. In this mini-review, we comprehensively describe the several technological advances and developments in the in-cell NMR spectroscopy.

$^{51}V$ 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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NMR Studies of Ni-binding Luteinizing Hormone Releasing Hormone

  • Kim, Jin;Won, Ho-Shik
    • Journal of the Korean Magnetic Resonance Society
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    • v.13 no.2
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    • pp.143-153
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    • 2009
  • Luteinizing Hormone Releasing Hormone (LHRH) is composed of 10 amino acids, and is best known as a neurotransmitter. Because of the 80% homology in animals, much more concerns have focused on the substances that have similar functions or can control LHRH. Ni, Cu-LHRH complexes were synthesized. The degree of complexation was monitored by $^1H,\;^{13}C$-NMR chemical shifts, and final products were identified by ESI-Mass spectrum. Solution-state structure determination of Ni-LHRH complex was accomplished by using NMR results and NMR-based distance geometry (DG). Interproton distances from nuclear Overhauser effect spectroscopy (NOESY) were utilized for the molecular structure determination. Results were compared with previous structures obtained from energy minimization and other spectroscopic methods. Structure obtained in this study has a cyclic conformation which is similar to that of energy minimized, and exhibits a specific a-helical turn with residue numbers (2~7) out of 10 amino acids. Comparison of chemical shifts and EPR studies of Ni, Cu-LHRH complexes exhibit that Ni-LHRH complex has same binding sites with the 4-coordination mode as in Zn-LHRH complex.