• Title/Summary/Keyword: Solution NMR

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Structure-Function of the TNF Receptor-like Cysteine-rich Domain of Osteoprotegerin

  • Shin, Joon;Kim, Young-Mee;Li, Song-Zhe;Lim, Sung-Kil;Lee, Weontae
    • Molecules and Cells
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    • v.25 no.3
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    • pp.352-357
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    • 2008
  • Osteoprotegerin (OPG) is a soluble decoy receptor that inhibits osteoclastogenesis and is closely associated with bone resorption processes. We have designed and determined the solution structures of potent OPG analogue peptides, derived from sequences of the cysteine-rich domain of OPG. The inhibitory effects of the peptides on osteoclastogenesis are dose-dependent ($10^{-6}M-10^{-4}M$), and the activity of the linear peptide at $10^{-4}M$ is ten-fold higher than that of the cyclic OPG peptide. Both linear and cyclic peptides have a ${\beta}$-turn-like conformation and the cyclic peptide has a rigid conformation, suggesting that structural flexibility is an important factor for receptor binding. Based on structural and biochemical information about RANKL and the OPG peptides, we suggest that complex formation between the peptide and RANKL is mediated by both hydrophobic and hydrogen bonding interactions. These results provide structural insights that should aid in the design of peptidyl-mimetic inhibitors for treating metabolic bone diseases caused by abnormal osteoclast recruitment.

Chelation of Calcium Ions by Poly(${\gamma}$-Glutamic Acid) from Bacillus subtilis (Chungkookjang)

  • Tsujimoto, Takashi;Kimura, Junya;Takeuchi, Yasushi;Uyama, Hiroshi;Park, Chung;Sung, Moon-Hee
    • Journal of Microbiology and Biotechnology
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    • v.20 no.10
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    • pp.1436-1439
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    • 2010
  • Many studies have clarified that poly(${\gamma}$-glutamic acid) (PGA) increases the solubility of $Ca^{2+}$, suggesting that PGA enhances calcium absorption in the small intestine. However, there has been no report on the specific interaction between PGA and $Ca^{2+}$ in water. We studied the aqueous solution properties of PGA calcium salt (PGA-Ca complex). The chelating ability and binding strength of PGA for $Ca^{2+}$ were evaluated. The PGA-Ca complex was soluble in water, in contrast to the insolubility of poly(acrylic acid) (PAA) calcium salt, and the chelating ability of PGA for $Ca^{2+}$ was almost the same as that of PAA. The globular conformation of the PGA-Ca complex in water was estimated by SEC and viscosity measurements. The chelation ability of PGA for $Ca^{2+}$ was examined by $^1H$ NMR. The present study showing the characteristics of the PGA-Ca complex will provide useful information about the calcium absorption by PGA in vivo.

Application of FT - PGSE for Micelle Formation of Surfactant Solution (계면활성제 용액의 미셀형성에 있어 FT - PGSE의 응용)

  • Nam, K.D.;Choi, S.O.
    • Journal of the Korean Applied Science and Technology
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    • v.16 no.1
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    • pp.1-14
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    • 1999
  • 계면활성제는 수용액에서 미셀을 형성함에 있어서 자기확산이 분자 운동과 상변화에 대하여 자세한 정보를 제공하고 공업적으로 응용할 수 있는 기술이 점차 증가하고 있다. 계면활성제가 미셀을 형성함에 있어 자기확산 정도는 화학구조의 변화성과 상호 결합 및 회합현상에 매우 민감한 것은 사실이다. 특히 계면활성제 용액의 넓은 범위의 분자 시스템과 콜로이드 상태의 변화성은 다향한 물리, 화학적 성질에 기여됨이 많다. 더욱이 미셀 형성에서 자기확산 계수는 분자 치환에 직간접적으로 상호관계가 있어 NMR 분광학에서 스핀 이완속도의 해석과 분자의 재배열, 스핀 이완에 대한 모델선정 등에 많은 관심을 갖는다. 그중 미셀형성에 있어서 자기확산에 대한 측정 방법중 가장 많이 이용되고 있는 Fourier Transform Pulsed Gradient Spin Echo(FT-PGSE) 측정법은 계면활성제의 미셀형성에 대한 상변화성 및 물리, 화학적 성질을 다루는데 새로운 도구로 제공되고 있다. 이는 이 계통의 기술적 측정방법에 있어서 적절한 개선과 새로운 응용분야를 확장하는데 있어서 많은 가능성을 갖고있다. 그리하여 이들에 대한 역사적 배경과 기초적인 이론을 가지고 미셀 형성에 있어 자기확산에 대한 개념을 말하고 그에 대한 응용성을 계통적으로 설명하고자 한다.

Synthesis and Properties of Fatty Ester Type Cationic Gemini Surfactants (고급지방산 에스테르형 양이온 제미니 계면활성제의 합성 및 특성)

  • Park, Jong-Kwon;Jeong, Noh-Hee
    • Journal of the Korean Applied Science and Technology
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    • v.28 no.2
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    • pp.140-145
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    • 2011
  • Cationic gemini-surfactant, namely 1,4-butane-bis(N-alkanoyloxyethyl-N,Ndimethyl)-diammonium bromide was synthesized and their inhibition effect on corrosion of mild steel in 1 M HCl solution was tested by weight loss method. The synthesized product was confirmed by FT-IR and $^1H-NMR$ spectroscopy. Surface tensions were measured by surface tensiometer Sigma 70. Their c.m.c. values evaluated by surface tension method was $4.1{\times}10^{-5}{\sim}5.4{\times}10^{-5}$ mol/L. The Krafft point of the these surfactants were <0~$10.7^{\circ}C$. The emulsifying properties of synthesized cationic gemini surfactants and sodium dodecyl sulfate (SDS), tetradecyl trimethyl ammonium bromide (TTAB) was investigated. Of these, 1,4-butane-bis(N-lauroyloxyethyl-N,N-dimethyl)- diammonium bromide, CGL 14-4-14 has been confirmed as a good emulsifier. The inhibition efficiency increases by increasing cationic gemini surfactant concentration. As a result, these surfactants are expected to be applied as corrosion inhibitors.

Anti-Foaming Properties of Polypropylene Glycol Oleates (올레산 폴리프로필렌글리콜 에스테르류의 소포특성)

  • Li, Hai-Yan;Choi, Hyoung-Chul;Jeong, Noh-Hee
    • Journal of the Korean Applied Science and Technology
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    • v.28 no.2
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    • pp.146-151
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    • 2011
  • In this study, by using oleic acid and polypropylene glycol, good natured antifoaming agent for suitable electronics process under the alkaline conditions were synthesized. For the synthesized mono and diesters, acid value, hydroxyl value was measured, and identified by FT-IR and $^1H-NMR$ spectroscopy. Surface properties such as surface tension, critical micelle concentration(cmc) for diluted aqueous solution was measured, and tested the antifoaming properties according to the difference of alkyl chain length, various concentration, temperature and pH. The surface tension of synthesized antifoaming agent, PPMO(Polypropylene glycol monooleate) was 24.3 dyne/cm, PPDO(Polypropylene glycol dioleate) was 23.7 dyne/cm. By increasing of the alkyl chain length, surface tension was decreased slightly, and showed good antifoaming properties at 0.06 wt% concentration and $50^{\circ}C$, pH 11. These synthesized compounds are expected to apply as a suitable antifoaming agents in the semiconductor and the PCB(Printed Circuit Board) manufacturing process.

Synthesis of Gemini Type Cationic Surfactants and Properties of Spacer Length (제미니형 양이온 계면활성제 합성 및 Spacer 길이에 따른 물성)

  • Park, Jong-Kwon;Jeong, Noh-Hee
    • Journal of the Korean Applied Science and Technology
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    • v.31 no.1
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    • pp.1-6
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    • 2014
  • Gemini type of cationic surfactant, namely ${\alpha},{\omega}$-alkane-bis(N-lauroyloxyethyl-N,N-dimethyl)-diammonium bromide was synthesized and confirmed by FT-IR and $^1H$-NMR spectroscopy. Their inhibition effect on corrosion of mild steel in 1 M HCl solution was tested by weight loss method. Surface tensions were measured by surface tensiometer Sigma 70. Their c.m.c. values evaluated by surface tension method was $4.01{\times}10^{-5}{\sim}4.99{\times}10^{-5}mol/L$. The Krafft point of the these surfactants were < $0^{\circ}C$. The emulsifying properties of synthesized cationic gemini surfactants and sodium dodecyl sulfate (SDS), tetradecyl trimethyl ammonium bromide (TTAB) was investigated. Of these, ${\alpha},{\omega}$-alkane-bis(N-lauroyloxyethyl-N,N-dimethyl)-diammonium bromide has been confirmed as a good emulsifier. The inhibition efficiency increases by increasing cationic gemini surfactant concentration. As a result, these surfactants are expected to be applied as corrosion inhibitors.

Structure Determination of Anti-plaque Agents for Prevention of Dental Caries from Cccao Bean Husk (Cacao Bean Husk로부터 분리한 충치 예방물질의 구조 결정)

  • 권익부;안봉전유주현이신영
    • KSBB Journal
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    • v.8 no.1
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    • pp.69-74
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    • 1993
  • For an anti-plaque agent, two flavan-3-ols isolated from Theobroma cacao bean husk showed positive reactions with $H_2SO_4$-anisaldehyde solution, $FeCl_3$, and were identified as monomeric, dimeric flavan-3-ots in TLC. They were (-)-epicatechin and procyanidin B-2(epicatechin-(4$\beta$$\rightarrow$8)-epicatechin). The structures were established by spectroscopic and chemical methods. (-)-Epicatechin had moderate inhibitory activity on GTase at concentration of 1.0mM while procyanidin B-2 showed complete inhibition activity at the same concentration. The hydroxyl group of flavan-3-ol was supposed to be the essential element for inhibition on GTase.

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Synthesis and Properties of Oligomers Containing 3-Triethylsilyl-1-silacyclopent-3-ene and Borane Derivatives via Polyaddition Reaction

  • Lee, Jung-Hwan;Park, Young-Tae
    • Bulletin of the Korean Chemical Society
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    • v.25 no.6
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    • pp.889-894
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    • 2004
  • Polyaddition reactions of 1,1-diethynyl-3-triethylsilyl-1-silacyclopent-3-ene with several organoborane derivatives have afforded the oligomeric materials containing organosilacyclic group and organoboron moiety along the oligomer main chains. All of these materials are soluble in THF as well as chloroform, and their molecular weights are in the range of 1,990/1,190-21,950/7,050 ($M_w/M_n$) with the polydispersity indexes of 1.67-3.43. The prepared oligomers are characterized by several spectroscopic methods such as $^1H,\;^{13}C, \;^{29}Si,\;^{11}B$ NMR and FTIR spectra along with elemental analysis. FTIR spectra of all the oligomers show that the new strong C=C stretching frequencies appear at 1599-1712 $cm^{-1}$, in particular. The UV-vis absorption spectra of the materials in THF solution exhibit the strong absorption bands at the ${\lambda}_{max}$ of 268-275 nm. The oligomeric materials show that the strong excitation peaks appear at the ${\lambda}_{max}$ of 255-279 nm and the strong fluorescence emission bands at the ${\lambda}_{max}$ of 306-370 nm. All the spectroscopic data suggest that the obtained materials contain both the organoboron ${\pi}$-conjugation moiety of C=C-B-C=C and the organosilacyclic group of 3-triethylsilyl-1-silacyclopent-3-ene along the oligomer main chains. The oligomers are thermally stable up to 162-200 $^{\circ}C$ under nitrogen.

Anion Sensing Properties of New Colorimetric Chemosensors Based on Thiourea and Urea Moieties

  • Kim, Dong-Wan;Kim, Jung-Hwan;Hwang, Jae-Young;Park, Jong-Keun;Kim, Jae-Sang
    • Bulletin of the Korean Chemical Society
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    • v.33 no.4
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    • pp.1159-1164
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    • 2012
  • A new colorimetric sensors containing thiourea (1-(4-nitrophenyl)-3-quinolin-6-ylthiourea; 1) and urea(1-(4-nitrophenyl)-3-quinolin-6-ylurea; 2) moieties for fluoride were designed and synthesized. These simple receptors were characterized their stoichiometry, and investigates the mechanism of their selectivity as anion receptors. The addition of tetrabutylammonium fluoride salts to the solution of receptors caused a dramatically and clearly observable color changes from colorless to yellow. To examine their application as anion receptors by UV-vis and $^1H$ NMR spectroscopy results revealed their higher selectivity for fluoride ion than other anions. The receptors and fluoride ion formed a 1:1 stoichiometry complex through strong hydrogen bonding interactions in the first step, followed by a process of deprotonation in presence of an excess of $F^-$ in DMSO solvent.

Endo- and Exo-Coordinated Mercury(II) Complexes of O3S2 Macrocycles: Effect of Dibenzo-Substituents on Coordination Mode

  • Lee, Ji-Eun;Kim, Hyun-Jee;Lee, So-Young;Lee, Jai-Young;Jin, Yong-Nu;Lee, Shim-Sung
    • Bulletin of the Korean Chemical Society
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    • v.28 no.11
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    • pp.2041-2044
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    • 2007
  • The reactions of mercury(II) chloride with O3S2-donor macrocyclic ligands with (L1) and without (L2) dibenzosubunit afforded respective exo- (1) and endo-coordinated (2) complexes depending on the ring rigidity of the ligands. From the X-ray crystal structures and comparative NMR studies for the complexes 1 and 2, it is confirmed that the resulting species with different coordination modes exist not only in solid state but also in solution state.