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超薄膜アニソトロピーの実現による超高感度・高選択的HPLCの開発

Research Project

Project/Area Number 10F00343
Research Category

Grant-in-Aid for JSPS Fellows

Allocation TypeSingle-year Grants
Section外国
Research Field Analytical chemistry
Research InstitutionKumamoto University

Principal Investigator

澤田 剛  熊本大学, 大学院・自然科学研究科, 准教授

Co-Investigator(Kenkyū-buntansha) MALIK A.K.  熊本大学, 大学院・自然科学研究科, 外国人特別研究員
MALLIK A.K.  熊本大学, 大学院・自然科学研究科, 外国人特別研究員
Project Period (FY) 2010 – 2012
Project Status Completed (Fiscal Year 2012)
Budget Amount *help
¥2,300,000 (Direct Cost: ¥2,300,000)
Fiscal Year 2012: ¥900,000 (Direct Cost: ¥900,000)
Fiscal Year 2011: ¥900,000 (Direct Cost: ¥900,000)
Fiscal Year 2010: ¥500,000 (Direct Cost: ¥500,000)
Keywords分子認識 / 交互共重合 / ポリマーシリカハイブリッド / HPLC分離 / トコフェノール異性体 / βカロチン異性体 / 多環芳香族化合物 / ステロイド
Research Abstract

環境科学、食品科学、臨床医学などの分野で重要な物質の幾何異性体を、高速液体クロマトグラフィによって分離、分析することは、分析化学の分野で重要な課題である。本研究では、高選択的な逆相高速液体クロマトグラフィー(RP-HPLC)に利用可能な、新奇な交互共重合ポリマーシリカハイブリッド型充填剤を開発することを目的としている。
平成24年度は、分子ゲルを形成するL-グルタミド脂質を末端に導入し、アミド基を高密度で配向制御した超薄膜シリカ微粒子(si1-FIP)を合成し、RP-HPLC充填剤としての可能性を検討するとともに、これまでの研究成果をまとめて、図書の1章として発表した。
Si1-FIPは、L-グルタミド脂質を合成してアミド基を置換後、アミノイソプロピルトリメトキシシラン(APS)修飾シリカ表面に導入して合成した。Si1-FIPを充填剤としてRP-HPLCを行った結果、多環芳香族類、特に、o-,p-ターフェニルの分離において高い形状選択性を示した(α_p<-/o-Terpheny1>=24.9)。
また、これまでの研究成果を総括した結果、電荷移動相互作用を利用したN-マレイミド-オクタデシルアクリル酸エステルの交互共重合体や分子ゲル構造を利用した超薄膜を形成することで、アミド基やカルボニル基を高密度で配向制御した超薄膜が形成できることを見いだした。超薄膜シリカ微粒子をRP-HPLCの充填剤に利用することで、トコフェノール類やステロイド類、多環芳香族類をそれぞれ高い形状選択性を示した。特にトコフェノール異性体では、25min以内で完全分離が可能となった。これはL-グルタミド脂質部位とアミド基による水素結合、カルボニルπ相互作用等の弱い相互作用の多点集積化により、形状認識能が向上したためと考えられる。

Report

(3 results)
  • 2012 Annual Research Report
  • 2011 Annual Research Report
  • 2010 Annual Research Report
  • Research Products

    (18 results)

All 2012 2011 2010 Other

All Journal Article (7 results) (of which Peer Reviewed: 7 results) Presentation (7 results) Book (1 results) Remarks (3 results)

  • [Journal Article] Selectivity enhancement for the separation of tocopherols andsteroids by integration of highly ordered weak interaction sitesalong the polymer main chain2012

    • Author(s)
      A. K. Mallik, H. Qiu,M. Takafuji, H. Ihara
    • Journal Title

      Analytical and Bioanalytical Chemistry

      Volume: 404 Issue: 1 Pages: 229-238

    • DOI

      10.1007/s00216-012-6098-0

    • Related Report
      2012 Annual Research Report
    • Peer Reviewed
  • [Journal Article] Molecular-shape selective high-performance liquid chromatography : Stabilization effect of polymer main chain by alternating copolymerization2012

    • Author(s)
      A.K.Mallik; H.Qiu; T.Sawada; M.Takafuji; H.Ihara
    • Journal Title

      Journal of Chromatography A

      Volume: 1232 Pages: 183-189

    • DOI

      10.1016/j.chroma.2011.11.061

    • Related Report
      2011 Annual Research Report
    • Peer Reviewed
  • [Journal Article] Strategic achievement for the baseline separation of tocopherol isomers by integration of weak interaction sites on alternating copolymer2011

    • Author(s)
      A.K.Mallik; H.Qiu; M.Takafuji; H.Ihara
    • Journal Title

      Analytical Methods

      Volume: 3 Issue: 6 Pages: 1277-1279

    • DOI

      10.1039/c1ay05198a

    • Related Report
      2011 Annual Research Report
    • Peer Reviewed
  • [Journal Article] Ultra-High Molecular Shape Selectivity by Molecular Gel : Bioactive and Shape-Constrained Isomers through the Integration and Orientation of Weak Interaction Sites2011

    • Author(s)
      A.K.Mallik; H.Qiu; T.Sawada; M.Takafuji; H.Ihara
    • Journal Title

      Chemical Communications

      Volume: 47 Issue: 37 Pages: 10341-10343

    • DOI

      10.1039/c1cc13397g

    • Related Report
      2011 Annual Research Report
    • Peer Reviewed
  • [Journal Article] Novel Approach for the Separation of Shape-Constrained Isomers with Alternating Copolymer-Grafted Silica in Reversed-Phase Liquid Chromatography.2010

    • Author(s)
      Abul K.Mallik, T.Sawada, M.Takafuji, H.Ihara
    • Journal Title

      Analytical Chemistry

      Volume: 82 Pages: 3320-3328

    • Related Report
      2010 Annual Research Report
    • Peer Reviewed
  • [Journal Article] Complete chromatographic separation of steroids including 17a- and 17b-estradioles using carbazole-based polymeric organic phase in both revered and normal phase HPLC2010

    • Author(s)
      Abul K.Mallik, K.Shingo, U.G.Gautam, T.Sawada, M.Takafuji, H.Ihara
    • Journal Title

      Analytical and Bioanalytical Chemistry

      Volume: 397 Pages: 623-629

    • Related Report
      2010 Annual Research Report
    • Peer Reviewed
  • [Journal Article] Preparation of high selective HPLC packing materials based on alternating copolymer-grafted silica.2010

    • Author(s)
      Abul K.Mallik, T.Sawada, M.Takafuji, H.Ihara
    • Journal Title

      Journal of Separation Science

      Volume: 33 Pages: 2977-2989

    • Related Report
      2010 Annual Research Report
    • Peer Reviewed
  • [Presentation] Baseline separation of Tocopherol isomers and Carotenoidsthrough multiple-interactions with molecular gel formingcompound-drafted organic phase2012

    • Author(s)
      A. K. Mallik, H. Qiu,T. Sawada, M. Takafuji, H. Ihara
    • Organizer
      38th International Symposium on High Performance Liquid Phase Separations and Related Techniques (HPLC2012)
    • Place of Presentation
      Anaheim, CA, USA
    • Related Report
      2012 Annual Research Report
  • [Presentation] Molecular-Shape Selectivity for Constrained Solutes in Reversed-Phase Liquid Chromatography2011

    • Author(s)
      Abul K.Mallik
    • Organizer
      8th International Forum on New Waves in Supramolecular Chemistry and Superstructured Materials
    • Place of Presentation
      The 100 Anniversary Hall, Kumamoto University, Kumamoto, Japan
    • Year and Date
      2011-01-14
    • Related Report
      2010 Annual Research Report
  • [Presentation] Separation of Bioactive- and Shape-Constrained Isomers by Molecular Gel Forming Compounds-Grafted Silica in RP-HPLC2011

    • Author(s)
      A.K.Mallik, H.Qiu, T.Sawada, M.Takafuj, H.Ihara
    • Organizer
      37th International Symposium on High-Performance Liquid Phase Separations and Related Techniques
    • Place of Presentation
      Dalian, China
    • Related Report
      2011 Annual Research Report
  • [Presentation] New approach for high integration of weak interaction sites for selectivity enhancement in HPLC : Synthesis of new monomers and their alternating copolymerization on silica2011

    • Author(s)
      A.K.Mallik, H.Qiu, T.Sawada, M.Takafuj, H.Ihara
    • Organizer
      36th International Symposium on High-Performance Liquid Phase Separations and Related Techniques
    • Place of Presentation
      Budapest, Hungary
    • Related Report
      2011 Annual Research Report
  • [Presentation] New proposal of hydrophilic but nonionic polymer phase for high-selective normal phase liquid chromatography2011

    • Author(s)
      A.K.Mallik, K.Shingo, A.Ezaki, T.Sawada, M.Takafuji, H.Ihara
    • Organizer
      36th International Symposium on High-Performance Liquid Phase Separations and Related Techniques
    • Place of Presentation
      Budapest, Hungary
    • Related Report
      2011 Annual Research Report
  • [Presentation] Alternating Copolymer-Grafted Silica : A High-Selective Liquid Chromatographic Stationary Phase for the Separation of Shape-Constrained Isomers2011

    • Author(s)
      A.K.Mallik, T.Sawada, M.Takafuji, H.Ihara
    • Organizer
      Pusan-Gyeognam/Kyushu-Seibu Joint Symposium On High Polymaers (15th) and Fibers (13th)
    • Place of Presentation
      Pusan, Korea
    • Related Report
      2011 Annual Research Report
  • [Presentation] Separation of shape-constrained isomers by newly developed organic phase in RP-HPLC2011

    • Author(s)
      A.K.Mallik, H.Qiu, M.Takafuji, H.Ihara
    • Organizer
      IUPAC International Congress on Analytical Sciences 2011 (ICAS)
    • Place of Presentation
      Kyoto, Japan
    • Related Report
      2011 Annual Research Report
  • [Book] Chromatographic separation of tocopherol isomers.Tocopherol: Sources, Uses and Health Benefits,Edited by Angel Catala, Chapter 52012

    • Author(s)
      A. K. Mallik, H. Qiu, T. Sawada, M. Takafuji,H. Ihara
    • Total Pages
      7
    • Publisher
      Nova Science Publishers, Inc.
    • Related Report
      2012 Annual Research Report
  • [Remarks]

    • URL

      http://www.chem.kumamoto-u.ac.jp/~ihara/lab3/

    • Related Report
      2012 Annual Research Report
  • [Remarks]

    • URL

      http://www.chem.kumamoto-u.ac.jp/~ihara/lab3/

    • Related Report
      2011 Annual Research Report
  • [Remarks]

    • URL

      http://www.chem.kumamoto-u.ac.jp/~ihara/lab3/

    • Related Report
      2010 Annual Research Report

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Published: 2010-12-03   Modified: 2024-03-26  

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