• Title/Summary/Keyword: Solution NMR

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Solution structure and functional analysis of HelaTx1: the first toxin member of the κ-KTx5 subfamily

  • Park, Bong Gyu;Peigneur, Steve;Esaki, Nao;Yamaguchi, Yoko;Ryu, Jae Ha;Tytgat, Jan;Kim, Jae Il;Sato, Kazuki
    • BMB Reports
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    • v.53 no.5
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    • pp.260-265
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    • 2020
  • Scorpion venom comprises a cocktail of toxins that have proven to be useful molecular tools for studying the pharmacological properties of membrane ion channels. HelaTx1, a short peptide neurotoxin isolated recently from the venom of the scorpion Heterometrus laoticus, is a 25 amino acid peptide with two disulfide bonds that shares low sequence homology with other scorpion toxins. HelaTx1 effectively decreases the amplitude of the K+ currents of voltage-gated Kv1.1 and Kv1.6 channels expressed in Xenopus oocytes, and was identified as the first toxin member of the κ-KTx5 subfamily, based on a sequence comparison and phylogenetic analysis. In the present study, we report the NMR solution structure of HelaTx1, and the major interaction points for its binding to voltage-gated Kv1.1 channels. The NMR results indicate that HelaTx1 adopts a helix-loop-helix fold linked by two disulfide bonds without any β-sheets, resembling the molecular folding of other cysteine-stabilized helix-loop-helix (Cs α/α) scorpion toxins such as κ-hefutoxin, HeTx, and OmTx, as well as conotoxin pl14a. A series of alanine-scanning analogs revealed a broad surface on the toxin molecule largely comprising positively-charged residues that is crucial for interaction with voltage-gated Kv1.1 channels. Interestingly, the functional dyad, a key molecular determinant for activity against voltage-gated potassium channels in other toxins, is not present in HelaTx1.

Analysis of the solution structure of the human antibiotic peptide dermcidin and its interaction with phospholipid vesicles

  • Jung, Hyun-Ho;Yang, Sung-Tae;Sim, Ji-Yeong;Lee, Seung-Kyu;Lee, Ju-Yeon;Kim, Ha-Hyung;Shin, Song-Yub;Kim, Jae-Il
    • BMB Reports
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    • v.43 no.5
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    • pp.362-368
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    • 2010
  • Dermcidin is a human antibiotic peptide that is secreted by the sweat glands and has no homology to other known antimicrobial peptides. As an initial step toward understanding dermcidin's mode of action at bacterial membranes, we used homonuclear and heteronuclear NMR to determine the conformation of the peptide in 50% trifluoroethanol solution. We found that dermcidin adopts a flexible amphipathic $\alpha$-helical structure with a helix-hinge-helix motif, which is a common molecular fold among antimicrobial peptides. Spin-down assays of dermcidin and several related peptides revealed that the affinity with which dermcidin binds to bacterial-mimetic membranes is primarily dependent on its amphipathic $\alpha$-helical structure and its length (>30 residues); its negative net charge and acidic pI have little effect on binding. These findings suggest that the mode of action of dermcidin is similar to that of other membrane-targeting antimicrobial peptides, though the details of its antimicrobial action remain to be determined.

Preparation of Poly(vinyl chloride)-graft-poly(styrene sulfonic acid) Composite Nanofiltration Membranes (폴리비닐클로라이드-그래프트-폴리스티렌 술폰산 복합 나노막 제조)

  • Kim, Jong-Hak;Park, Jung-Tae;Koh, Joo-Hwan;Roh, Dong-Kyu;Seo, Jin-Ah
    • Membrane Journal
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    • v.18 no.2
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    • pp.132-137
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    • 2008
  • Nanofiltration membranes were prepared based on coating a sulfonated comb-like copolymer layer on top of a poly(vinylidene fluoride) (PVDF) support. The comb-like copolymer comprising poly(vinyl chloride) backbone and poly(styrene sulfonic acid) side chains, i.e. PVC-g-PSSA was synthesized by atom transfer radical polymerization (ATRP) using direct initiation of the secondary chlorines of PVC. The successful synthesis of graft copolymers were confirmed by nuclear magnetic resonance ($^1H$-NMR), FT-IR spectroscopy and wide angle X-ray scattering (WAXS). Composite nanofiltration membranes consisting PVC-g-PSSA as a top layer exhibited the increase of both rejections and solution flux with increasing PSSA concentration. This performance enhancement is presumably due to the increase of SO3H groups and membrane hydrophilicity. The rejections of composite membranes containing 71 wt% of PSSA were 88% for $Na_2SO_4$ and 33% for NaCl, and the solution flux were 26 and $34L/m^2h$, respectively, at 0.3 MPa pressure.

Photocycloaddition Reaction of 4',5'-Dihydropsoralen to Tetramethylethylene (4',5'-디히드로소랄렌과 테트라메틸에틸렌의 광고리화 첨가반응에 관한 연구)

  • Sang Chul Shim;Jong Sung Koh
    • Journal of the Korean Chemical Society
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    • v.26 no.3
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    • pp.172-178
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    • 1982
  • A psoralen-DNA monoadduct analogue, 4',5'-dihydropsoralen (DHP) is synthesized and its photophysical properties such as fluorescence quantum yield (0.08), phosphorescence quantum yield (0.013), fluorescence lifetime (0.95ns), and phosphorescence lifetime(0.039s) were measured in ether solution and in frozen matrix state at 77K. The photocycloaddition reaction of DHP with tetramethylethylene(TME) was carried out in solution and in the frozen state. The major photoadduct was isolated and characterized by elemental analysis and physical methods such as UV, IR, NMR, and mass spectrometry. The major DHP-TME photoadduct was proved to be an 1 : 1 $C_4$-cycloadduct formed through 2 + 2 cycloaddition of the pyrone double bond of DHP to TME.

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Syntheses and Characterization of PBO Precursors Containing Dimethylphenoxy and/or MPEG Pendant Groups (Dimethylphenoxy와 MPEG 팬던트 그룹을 갖는 폴리벤즈옥사졸 전구체의 합성 및 특성)

  • Yoon Doo-Soo;Choi Jae-Kon;Jo Byung-Wook
    • Polymer(Korea)
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    • v.29 no.5
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    • pp.493-500
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    • 2005
  • Polyhydroxyamides(PHAs) having poly(ethylene glycol)methyl ether (MPEG) and/or dimethylphenoxy pendant groups were synthesized by solution polycondensation at low temperature. The inherent viscosities of the PHAs measured at $35^{\circ}C$ in DMAC or DMAc/LiCl solution were in the range of $0.51\~2.31dL/g$. This precursor polymers were studied by FT-IR, $1H-NMR$, DSC, and TGA. Solubility of the precursors with higher MPEG unit was increased, especially the polymer having MPEG $(M_n=1100)$ was soluble or partially soluble in ethanol, methanol, and water as well as aprotic solvents, but the PBOs were nearly insoluble in a variety of solvents. PHAs were converted to polybenzoxazoles (PBOs) by thermal cyclization reaction with heat of endotherm. In case of the precursors having MPEG nit, the precursor polymers with a higher $M_n$ were fully cyclized at a lower temperature than one with a lower $M_n$.

Photopolymerization and Properties of PCL-Based Biodegradable Molecularly Imprinted Polymers (PCL 기반 생분해성 분자 날인 고분자의 광중합 및 물성)

  • Kim, Sun-Hui;Lee, Kyung-Soo;Kim, Yong-Hoon;Choi, Woo-Jin;Kim, Beom-Soo;Kim, Eung-Kook;Kim, Dae-Su
    • Polymer(Korea)
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    • v.31 no.2
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    • pp.153-159
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    • 2007
  • Biodegradable molecularly imprinted polymers (MIPs) can be applied in the biomedical area of biosensors, drug delivery, etc. Therefore, in this study, biodegradable theophylline MIPs were synthesized via photopolymerization using a poly $(\varepsilon-caprolactone)$ (PCL) macromer as a cross-linker and their physical properties were investigated. The yield for the synthesis of the PCL macromer with terminal acrylate groups was ca. 78 mol%. The products were characterized by the combination of FT-IR and $^1H-NMR$ spectroscopic analyses. UV/Visible spectroscopic analysis for removing and rebinding theophylline was performed by monitoring the theophylline concentration in the solution. In vitro biodegradation tests of the theophylline MIPs performed in phosphate buffered saline (PBS) solution at $37^{\circ}C$ showed good biodegradability of the MIPs.

Preparation and Optical Properties of Polarizing Film Based on Poly(vinyl Alcohol) Dyed by Reactive Dichroic Dyes Using Organic Solvents (유기 용매를 사용한 반응성 이색성 염료의 염착에 의한 폴리비닐알코올계 편광필름의 제조 및 광학특성)

  • Choi, E-Joon;Choi, Seung Sock;Kim, Eun-Chol;Kim, Si Min;Back, Sang-Hyun
    • Journal of Adhesion and Interface
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    • v.13 no.3
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    • pp.131-136
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    • 2012
  • In this study, commercial poly(vinyl alcohol) (PVA) film was dyed with reactive dichroic dyes under mild conditions using organic solvents in stead of strong basic aqueous solution. After drawing of 500% of this PVA film, the polarizing efficiency and the single piece transmittance were measured. The degree of saponification of the commercialized PVA film was determined by using NMR and FT-IR spectromety. The commercial PVA film, with ca. 100% of the degree of saponification determined by NMR spectrometry, was dyed with the reactive dichroic dyes, which have 3,5-dichloro-2,4,6-triazine moiety. As a result, we found that the PVA film dyed with the reactive congo red showed relatively good polarization efficiency, and the PVA film dyed with the reactive direct black 22 exhibited relatively good single piece transmittance.

Coordination Modes and Properties of Ag(I) Complex with N,N,N',N',N''-Pentamethyldiethylenetriamine

  • Chun, In-Sung;Kwon, Jung-Ah;Bae, Myung-Nam;Lee, Sim-Seong;Jung, Ok-Sang
    • Bulletin of the Korean Chemical Society
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    • v.27 no.7
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    • pp.1005-1008
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    • 2006
  • The reaction of $AgClO_{4}$ with acyclic potential tridentate N,N,N',N',N''-pentamethyldiethylenetriamine (pmdeta) has given colorless crystals suitable for X-ray crystallography. The crystal structure ($P2_{1}$/n, a = 14.413(1) $\AA$, b = 25.270(2) $\AA$, c = 16.130(1) $\AA$, b = $103.012(1){^{\circ}}$, V = 5723.7(8) A$\AA^{3}$, Z = 4, R = 0.0349) has been solved and refined. Three silver(I) ions connect four pmdeta ligands to produce discrete complex of $[Ag_3(pmdeta)_4](ClO_4)_3$. A pmdeta ligand is bridged to three silver(I) ions, and three other pmdeta ligands are chelated to each silver(I) center in a tridentate mode. Thus, the product is a rare tri-nuclear silver(I) complex with two different chemical environments. $^{13}C$ NMR and $MAS\;^{13}$C NMR indicate that the tri-nuclear silver(I) complex is not rigid in solution. The contact angles and thermal analyses of the complex are measured and discussed.

Synthesis and Spectroscopic Studies of Metal Complexes Formed in the Reaction of Metal Ions with Urea at High Temperature (높은 온도에서 Urea와 금속이온과의 반응으로 얻어진 금속 Complexes의 합성과 분광학적 연구)

  • Gaballa, Akmal S.;Teleb, Said M.;Nour, El-Metwally
    • Journal of the Korean Chemical Society
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    • v.51 no.4
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    • pp.339-345
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    • 2007
  • Urea reacts with PtCl2, H2[PtCl6]·6H2O, H2[IrCl6] and Ni(CH3CO2)2 in aqueous solution at high temperature (60-80 °C) yielding [PtCl2(Urea)]·2H2O (1), (NH4)2[PtCl6] (2), (NH4)2[IrCl6]·H2O (3) and [Ni2(OH)2(NCO)2(H2O)2] (4) complexes, respectively. In complex 1, urea coordinates to Pt(II) as a neutral bidentate ligand via amido nitrogen atoms. In complexes 2, 3 and 4 it seems that the coordinated urea molecules decompose during the reaction at high temperature and a variety of reaction products are obtained. All complexes were isolated in moderate yields as dark green (1), yellow (2), pale brown (3) and faint green (4) precipitates, respectively. The reaction products were characterized by their microanalysis, IR, 1H and 13C NMR spectra as well as thermal analysis. General mechanisms describing the formation of these complexes were suggested.

Construction of Antibacterial Electrospun Nanofiber from Poly(styrene-co-sulfadiazine) via Electrospinning (폴리(스티렌-설파디아진) 공중합체를 이용한 항균 나노섬유 제조)

  • Hwang, Seok-Ho;Ahn, Kyung-Hwan;Cha, Heechul;Kim, Jeong-Yeol;Hwang, Hong-Gu;Huh, Wansoo;Lee, Sangwon
    • Applied Chemistry for Engineering
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    • v.20 no.4
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    • pp.386-390
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    • 2009
  • In this study, sulfadiazine acrylamide monomer was synthesized by the reaction of sulfadiazine, known as an antibiotic substance, with acryloyl chloride. The monomer was characterized by $^1H-NMR$, and $^{13}C-NMR$. Using the synthesized sulfadiazine acrylamide monomer and styrene monomer, a copolymer, poly(styrene-co-sulfadiazine), was obtained by the free radical copolymerization and characterized by $^1H-NMR$, GPC, DSC and TGA. The copolymer nanofibers web has been successfully prepared by electrospinning technique under DMF solution. The diameter of the nanofibers was in the range between 500 and 800 nm. Antibacterial activity of the nanofiber web was evaluated utilizing the colony counting method against Staphylococcus aureus and Escherichia coli.