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1998 Fiscal Year Final Research Report Summary

NONCRYSTALLINE STRUCTURES AND DYNAMICS OF FIBERS AND POLYMERS STUDIED WITH 15N,13C AND 2H SOLID STATE NMR

Research Project

Project/Area Number 09450357
Research Category

Grant-in-Aid for Scientific Research (B)

Allocation TypeSingle-year Grants
Section一般
Research Field 高分子構造・物性(含繊維)
Research InstitutionTOKYO UNIVERSITY OF AGRICULTURE AND TECHNOLOGY

Principal Investigator

ASAKURA Tetsuo  TOKYO UNIVERSITY OF AGRICULTURE AND TECHNOLOGYT・BIOTECHNOLOGY・PROFESSER, 工学部, 教授 (30139208)

Co-Investigator(Kenkyū-buntansha) DEMURA Makoto  HOKKAIDO UNIVERSITY・GRADUATE SCHOOL OF SCIENCE・FACULTY OF SCIENCE・ASSOCIATE PROF, 大学院・理学研究科・理学部, 助教授 (70188704)
Project Period (FY) 1997 – 1998
KeywordsSOLID STATE NMR / NONCRYSTALLINE STRUCTURE OF FIBER AND POLYMER / DYNAMICS OF FIBER AND POLYMER / NMR CHEMICAL SHIFT / BOMBYX MORI AND SAMIA CYNCIA RICINI SILK FIBROIN / ISOTOPE LABELED SILK / POLYLACTIC ACID / KERATIN
Research Abstract

THE STRUCTURE AND DYNAMICS OF FIBERS AND POLYMERS WERE STUDIED WITH SOLID STATE 1 5N,1 30 AND 2H NMR.ESPECIALLY.THE DEVELOPMENT OF NMR ANALYSIS OF THE NONCRYSTALLINE STRUCTURE AND STABLE ISOTOPE LABELING OF THE SAMPLES WERE EMPHASIZED.THE SAMPLES USED HERE ARE 15N.13C AND 2K LABELED BOMBYX MORI AND SAMIA CYNCIA RICINI SILK FIBROINS, POLYLACTIC ACID AND KERATIN.THE NMR ANALITICAL METHODS WERE THE ANGLE DEPENDENT-NMR ANALYSIS FOR ORIENTED FIBER AND POLYMER, DYNAMICS STUDY WITH 2K SOLID STATE NMR, ISOTROPIC NMR CHEMICAL SHIFT AND CHEMICAL SHIFT CALCULATION, SOLID STATE SPIN DIFFUSION NMR AND REDOR.
THE BACKBONE AND SIDE CHAIN STRUCTURES , THAT IS, TORSION ANGLES OF GLYCINE, ALANINE,SERINE,TYROSINE AND VALINE RESIDUES OF SILK FIBROINS WERE DETERMINED WITH ANGLE-DEPENDENT NMR AND 130 CHEMICAL SHIFT CONTOUR PLOTS OF ALANE RESIDUE.THE DYNAMICS OF BACKBONE AND SIDE CHAIN OF SILK FIBROINS WERE STUDIED WITH 2H SOLID STATE NMR AND RELATIONSHIP AMONG DYNAMICS, STRUCTURE AND PROPERTIES OF SILK FIBROINS WERE DISCUSSED.

  • Research Products

    (66 results)

All Other

All Publications (66 results)

  • [Publications] T.Asakura, M.Demura, T.Date, N.Miyashita, K.Ogawa, M.P.Williamson: "NMR Study of Silk I Structure of Bombyx mori Silk Fibroin with ^<15>N- and ^<13>C-NMR Chemical Shift Contour Plots" Biopolymers. 41. 193-203 (1997)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] T.Asakura, M.Iwadate, T.Date, M.Demura and K.Nokihara: "Refinement of the Solution Structure of Neurokinin A (4-10) on the Basis of ^1H NMR Chemical Shift Calculations" Peptide Chemistry 1996. 345-348 (1997)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] M.Iwadate, T.Asakura and M.P.Williamson: "The structure of the melittin tetramer at differennt temperatures : An NOE-based calculation with chemical shift refinement" European J.of Biochemistry. 257. 479-487 (1998)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] M.Iwadate, T.Asakura and M.P.Williamson: "Cα and Cβ Carbon13 Chemical Shifts in Proteins from an Empirical Database" J.Biomol.NMR. (in press).

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] J.Kikuchi, T.Asakura, P.A.Loach, P.S.Parkes-Loach, K.Shimada, C.N.Hunter, M.J.Conroy and M.P.Williamson: "A light-harvesting antenna protein retains its folded conformation in the absence of protein-lipid and protein-pigment interactions" Biopolymers. (in press).

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] J.Kikuchi and T.Asakura: "Use of ^<13>C conformation-dependent chemical shifts to elucidate the local structure of a large protein with homologous domains in solution and solid state" J.Biochem.Biophys.Method. (in press).

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] T.Asakura, M.Iwadate, M.Demura and M.P.Williamson: "Structural Analysis of Silk using ^<13>C NMR Chemical Shift Contour Plots." Int.J.Biolog.Macromol. (in press).

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] J.Kikuchi, T.Asakura, K.Hasuda, T.Ito, K.Ohwaku and M.P.Williamson: "An Advantage for Use of Isotope Labeling and NMR Chemical Shifts to Analyze The Structure of Four Homologous IgG-binding Domains of Staphylococcal Protein A" J.Biochem.Biophys.Method. (submitted.).

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] Y.Hori, M.Demura, M.Iwadate, T.Niidome, H.Aoyagi and T.Asakura: Biophysical J.(submitted.).

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] T.Asakura, M.Minami, R.Shimada, M.Demura, M.Osanai, T.Fujito, M.Imanari, A.S.Ulrich: "^2H-Labelling of Silk Fibroin Fibers and Their Structural Characterization by Solid State ^2H NMR" Macromolecules. 30. 2429-2435 (1997)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] M.Demura, M.Minami, T.Asakura, and T.A.Cross: "Structure of Bombyx mori Silk Fibroin Based on Solid State NMR Orientational Constraints and Fiber Diffraction Unit Cell Parameters" J.Am.Chem.Soc.120. 1300-1308 (1998)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] M.Demura, Y.Yamazaki, T.Asakura and K.Ogawa: "Structure of Uniaxially Aligned ^<13>C Labeled Silk Fibroin Fibers with Solid State ^<13>C-NMR" J.Molecular Structure. 441. 155-163 (1998)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] T.Asakura, Y.Yamazaki, Koo Wey Seng and M.Demura: "Determination of the Mutual Orientation of the ^<15>N and ^<13>C NMR Chemical Shift Tensors of ^<13>C-^<15>N Double Labeled Model Peptides for Silk Fibroin from the Dipolar-Coupled Powder Patterns" J.Molecular Structure. 446. 179-190 (1998)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] T.Ito, Y.Maruhashi, M.Demura and T.Asakura: "Carbon-13 Solid State n.m.r.Study on Uniaxially Oriented Poly(L-lactic acid)Films" Polymers. (submitted).

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] T.Asakura and M.Demura: "Structure and Dynamics of Silk Fibroin Studied with ^<13>C, ^<15>N and ^2H Solid State NMR" Macromol.Chem.Macromolecular Symp.(in press.).

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] N.Nishikawa, Y.Tanizawa, S.Tanaka, Y.Horiguchi and T.Asakura: "Structure change of keratin protein in human hair by permanent waving treatment" Polymer. 39, 16. 3835-3840 (1998)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] N.Nishikawa, Y.Tanizawa, S.Tanaka, Y.Horiguchi, H.Matsuno and T.Asakura: "Carbon-13n.m.r.studies of keratin intermediate filament hair" Polymer. 39, 4. 1001-1004 (1998)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] N.Nishikawa, Y.Tanizawa, S.Tanaka, Y.Horiguchi, H.Matsuno and T.Asakura: "pH Dependence of the Coiled-Coil Structure of Keratin Intermediate Filament in Human Hair by ^<13>C NMR Spectrosroscopy and the Mechanism of Its Disruption" Polymer J.30, 2. 125-132 (1998)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] J.Kikuchi, Y.Mitsui, T.Asakura, K.Hasuda, H.Araki and K.Owaku: "Spectroscopic inverstigation of tertiary fold of staphylococcal protein A to explore its engineering application" Biomaterials. (in press.).

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] N.Nishikawa, Y.Horiguchi, Tetsuo Asakura and Iso Ando: "Carbon-13 solid-state n.m.r.study of 13C-enriched human hair keratin" Polymer. 40. 2139-2144 (1999)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] Y.Hori, M.Demura, T.Asakura, T.Niidome and H.Aoyagi: "Determination of Molecular Orientation in Peptide-Phospholipid Bilayer System using Angular Dependent Solid State ^<31>P, ^2H and ^<15>N NMR" Reports on Progress in Polymer Physics in Japan. 40. 609-612 (1997)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] M.Demura, Y.Ohkawa and T.Asakura: "Side Chain Dynamics of〔3, 3-^2H_2〕Serine Labeled Silk Fibroin using Solid State ^2H NMR" Reports on Progress in Polymer Physics in Japan. 40. 613-616 (1997)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] A.Aoki and T.Asakura: "Packing Effect on ^<13>C CP/MAS NMR Spectra of Isotactic Polypropylene" Reports on Progress in Polymer Physics in Japan. 40. 475-478 (1997)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] J.Kikuchi, T.Yamazaki and T.Asakura: "Characterization of Aggregated State of Light-harvesting Antenna Protein in Detergent Micelles" Reports on Progress in Polymer Physics in Japan. (in press.).

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] J.Kikuchi, K.Shimada and T.Asakura: "Solid-state NMR Spectroscopic Study of Membrane-bound Proteins in Rhodobacter Sphaeroides" Reports on Progress in Polymer Physics in Japan. (in press.).

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] M.Demura, O.Saita, T.Asakura, J.D.van Beek and Beat.H.Meier: "Determination of Torsion Angles of Silk Fibroin by Two-Dimensional Spin Diffusion NMR" Reports on Progress in Polymer Physics in Japan. (in press.).

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] M.P.Williamson and T.Asakura: "Protein Chemical Shifts, Methods in Molecular Biology" Protein NMR Techniques Edited by D.G.Reid Humana Press Inc., Totowa, NJ.60. (1997)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] T.Asakura, M.Demura and N.Naoki: "Structural Analysis of Oriented Polymers by Solid-State NMR" (Annual Reports on NMR Spectroscopy)(Ed.G.A.Webb)(ACADEMIC PRESS, London). 34. 301-346 (1997)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] 朝倉哲郎: "繊維構造に関するNMR研究" 繊維学会誌. 53. 300-304 (1997)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] 朝倉哲郎、出村誠: "シルク研究の新展開" 高分子. 47. 390-393 (1998)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] I.Ando and T.Asakura Eds.: "Proteins in “Solid State NMR of Polymers"" Elsevier, 1000 (1998)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] T.Asakura, M.Demura, T.Date, N.Miyashita, K.Ogawa, M.P.Williamson: "NMR Study of Silk I Structure of Bombyx mori Silk Fibroin with ^<15>N-and ^<13>C-NMR Chemical Shift Contour Plots" Biopolymers. 41. 193-203 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] T.Asakura, M.Iwadate, T.Date, M.Demura and K.Nokihara: "Refinement of the Solution Structure of Neurokinin A (4-10) on the Basis of ^1H NMR Chemical Shift Calculations" Peptide Chemistry. 1996. 345-348 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] M.Iwadate, T.Asakura and M.P.Williamson: "The structure of the melittin tetramer at differennt temperatures : An NOE-based calculation with chemical shift refinement" European J.of Biochemistry. 257. 479-487 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] M.Iwadate, T.Asakura and M.P.Williamson: "C_ and C_ Carbon 13 Chemical Shifts in Proteins from an Empirical Database" J.Biomol.NMR.(in press).

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] J.Kikuchi, T.Asakura, P.A.Loach, P.S.Parkes-Loach, K.Shimada, C.N.Hunter, M.J.Conroy and M.P.Williamson: "A light-harvesting antenna protein retains its folded conformation in the absence of protein-lipid and protein-pigment interactions" Biopolymers. (in press).

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] J.Kikuchi and T.Asakura: "Use of ^<13>C conformation-dependent chemical shifts to elucidate the local structure of a large protein with homologous domains in solution and solid state" J.Biochem.Biophys.Method.(in press).

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] T.Asakura, M.Iwadate, M.Demura and M.P.Williamson: "Structural Analysis of Silk with ^<13>C NMR Chemical Shift Contour Plots" Int.J.Biolog.Macromol.(in press).

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] J.Kikuchi, T.Asakura, K.Hasuda, T.Ito, K.Ohwaku and M.P.Williamson: "An Advantage for Use of Isotope Labeling and NMR Chemical Shifts to Analyze The Structure of Four Homologous IgG-binding Domains of Staphylococcal Protein A" J.Biochem.Biophys.Method.(submitted).

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] Y.Hori, M.Demura, M.Iwadate, T.Niidome, H.Aoyagi and T.Asakura: Biophysical J.(submitted).

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] T.Asakura, M.Minami, R.Shimada, M.Demura, M.Osanai, T.Fujito, M.Imanari, A.S.Ulrich: "^2H-Labelling of Silk Fibroin Fibers and Their Structural Characterization by Solid State ^2H NMR" Macromolecules. 30. 2429-2435 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] M.Demura, M.Minami, T.Asakura, and T.A.Cross: "Structure of Bombyx mori Silk Fibroin Based on Solid State NMR Orientational Constraints and Fiber Diffraction Unit Cell Parameters" J.Am.Chem.Soc.120. 1300-1308 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] M.Demura, Y.Yamazaki, T.Asakura and K.Ogawa: "Structure of Uniaxially Aligned ^<13>C Labeled Silk Fibroin Fibers with Solid State ^<13>C-NMR" J.Molecular Structure. 441. 155-163 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] T.Asakura, Y.Yamazaki, Koo Wey Seng and M.Demura: "Determination of the Mutual Orientation of the ^<15>N and ^<13>C NMR Chemical Shift Tensors of ^<13>C-^<15>N Double Labeled Model Peptides for Silk Fibroin from the Dipolar-Coupled Powder Patterns" J.Molecular Structure. 446. 179-190 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] T.Ito, Y.Maruhashi, M.Demura and T.Asakura: "Carbon-13 Solid State n.m.r.Study on Uniaxially Oriented Poly (L-lactic acid) Films" Polymers. (submitted).

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] T.Asakura and M.Demura: "Structure and Dynamics of Silk Fibroin Studied with ^<13>C,^<15>N and ^2H Solid State NMR" Macromol.Chem.Macromolecular Symp.(in press).

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] N.Nishikawa, Y.Tanizawa, S.Tanaka, Y.Horiguchi and T.Asakura: "Structure change of keratin protein in human hair by permanent waving treatment" Ploymer. 39,16. 3835-3840 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] N.Nishikawa, Y.Tanizawa, S.Tanaka, Y.Horiguchi, H.Matsuno and T.Asakura: "Carbon-13 n.m.r.studies of keratin intermediate filament hair" Polymer. 39,4. 1001-1004 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] N.Nishikawa, Y.Tanizawa, S.Tanaka, Y.Horiguchi, H.Matsuno and T.Asakura: "pH Dependence of the Coiled-Coil Structure of Keratin Intermediate Filament in Human Hair by ^<13>C NMR Spectrosroscopy and the Mechanism of Its Disruption" Polymer J.30,2. 125-132 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] J.Kikuchi, Y.Mitsui, T.Asakura, K.Hasuda, H.Araki and K.Owaku: "Spectroscopic inverstigation of tertiary fold of staphylococcal protein A to explore its engineering application" Biomaterials. (in press).

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] N.Nishikawa, Y.Horiguchi, T.Asakura and I.Ando: "Carbon-13 solid-state n.m.r. study of 13C-enriched human hair keratin" Polymer. 40. 2139-2144 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] Y.Hori, M.Demura, T.Asakura, T.Niidome and H.Aoyagi: "Determination of Molecular Orientation in Peptide-Phospholipid Bilayer System using Angular Dependent Solid State ^<31>P,^2H and ^<15> N NMR" Rep.Prog.Polym.Phys.Jpn.40. 609-612 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] M.Demura, Y.Ohkawa and T.Asakura: "Side Chain Dynamics of [3,3-^2H_2] Serine Labeled Silk Fibroin using Solid State ^2H NMR" Rep.Prog.Polym.Phys.Jpn.40. 613-616 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] A.Aoki and T.Asakura: "Packing Effect on ^<13>C CP/MAS NMR Spectra of Isotactic Polypropylene" Rep.Prog.Polym.Phys.Jpn.40. 475-478 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] J.Kikuchi, T.Yamazaki and T.Asakura: "Characterization of Aggregated State of Light-harvesting Antenna Protein in Detergent Micelles" Rep.Prog.Polym.Phys.Jpn.(in press.).

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] J.Kikuchi, K.Shimada and T.Asakura: "Solid-state NMR Spectroscopic Study of Membrane-bound Proteins in Rhodobacter Sphaeroides" Rep.Prog.Polym.Phys.Jpn.(in press).

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] M.Demura, O.Saita, T.Asakura, J.D.van Beek and Beat.H.Meier: "Determination of Torsion Angles of Silk Fibroin by Two-Dimensional Spin Diffusion NMR" Rep.Prog.Polym.Phys.Jpn.(in press.).

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] M.P.Williamson and T.Asakura: "Protein Chemical Shifts, Methods in Molecular Biology, Vol.60 : Protein NMR Techiques" Edited by D.G.Reid Humana Press Inc., Totowa, NJ. (1997)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] T.Asakura, M.Demura and N.Naoki: "Structural Analysis of Oriented Polymers by Solid-State NMR" Annual Reports on NMR Spectroscopy. (Ed.G.A.Webb) (ACADEMIC PRESS,London). 34,301-346 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] T.Asakura: "NMR Study on Fiber Structure" SEN-I GAKKAISHI. 53. 300-304 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] T.Asakura, M.Demura: "Progress in Silk Research" KOBUNSHI. 47. 390-393 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] T.Asakura, M.Demura, N.Nishikawa and H.Yoshimizu: "Proteins in "Solid State NMR of Polymers"" I.Ando and T.Asakura Eds.Elsevier. 853-890 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] T.Asakura and T.Ito: "Poly (ethylene terephthalate) in "Solid State NMR of Polymers"" I.Ando and T.Asakura Eds.Elsevier. 91-508 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] I.Ando and T.Asakura: "Polyamides in "Solid State NMR of Polymers"" I.Ando and T.Asakura Eds.Elsevier. 445-468 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] T.Asakura and M.Demura: "Oriented Fibers and Polymers in "Solid State NMR of Polymers"" I.Ando and T.Asakura Eds.Elsevier. 307-326 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] A.Aoki and T.Asakura: "Polyolefins in "Solid State NMR of Polymers"" I.Ando and T.Asakura Eds.Elsevier. 415-444 (1998)

    • Description
      「研究成果報告書概要(欧文)」より

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Published: 1999-12-08  

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