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Development of highly efficient and highly selective HPLC columns that provide multiple polar separation mechanisms simultaneously

Research Project

Project/Area Number 17K05900
Research Category

Grant-in-Aid for Scientific Research (C)

Allocation TypeMulti-year Fund
Section一般
Research Field Analytical chemistry
Research InstitutionKyoto Institute of Technology

Principal Investigator

Ikegami Tohru  京都工芸繊維大学, 分子化学系, 准教授 (20301252)

Project Period (FY) 2017-04-01 – 2020-03-31
Project Status Completed (Fiscal Year 2019)
Budget Amount *help
¥4,940,000 (Direct Cost: ¥3,800,000、Indirect Cost: ¥1,140,000)
Fiscal Year 2019: ¥1,170,000 (Direct Cost: ¥900,000、Indirect Cost: ¥270,000)
Fiscal Year 2018: ¥1,170,000 (Direct Cost: ¥900,000、Indirect Cost: ¥270,000)
Fiscal Year 2017: ¥2,600,000 (Direct Cost: ¥2,000,000、Indirect Cost: ¥600,000)
Keywords液体クロマトグラフィー / 親水性相互作用クロマトグラフィー / 分離媒体 / 分離特性 / 重合修飾 / 糖の分離
Outline of Final Research Achievements

The relationship between the optimization of the polymerization reaction used for the surface modification of silica and the separation performance was studied. Poly(acrylamide) type silica was prepared by surface-initiated atom transfer radical polymerization (SI-ATRP) to obtain hydrophilic interaction chromatography (HILIC) columns providing highly retentive and good selectivity for polar biomolecules. The relationship between the degree of polymerization or surface coverage of the polymer and the separation characteristics was explored to achieve high hydrophilicity and great retention simultaneously with silica particles of 20 nm pores.
Using the column developed by us, fine separation of structural isomers of monosaccharides and oligosaccharides found in glycoproteins was carried out (with international joint work). Furthermore, anomeric separation of sugar was also performed, and the equilibrium constant of the process was measured.

Academic Significance and Societal Importance of the Research Achievements

本研究で合成した表面開始原子移動ラジカル重合型のポリアクリルアミドカラムは市販されているどのアミド型カラムとも違う特徴を示した。すなわち、シリカ表面に濃縮される水の層が厚く、弱い酸性の表面を提供できる。親水性の保持が大きく、かつ構造の差異に対する選択性が高い固定相であり、実用性が高いと判断される。また、糖タンパクに含まれる糖鎖の研究は、現在注目を集めている抗体医薬の製造や同一性の確認に不可欠であり、社会的意義が大きいと考える。

Report

(4 results)
  • 2019 Annual Research Report   Final Research Report ( PDF )
  • 2018 Research-status Report
  • 2017 Research-status Report
  • Research Products

    (24 results)

All 2020 2019 2018 2017 Other

All Int'l Joint Research (3 results) Journal Article (9 results) (of which Int'l Joint Research: 4 results,  Peer Reviewed: 9 results,  Open Access: 1 results,  Acknowledgement Compliant: 1 results) Presentation (12 results) (of which Int'l Joint Research: 8 results,  Invited: 1 results)

  • [Int'l Joint Research] テュービンゲン大学(ドイツ)

    • Related Report
      2019 Annual Research Report
  • [Int'l Joint Research] テュービンゲン大学(ドイツ)

    • Related Report
      2018 Research-status Report
  • [Int'l Joint Research] Eberhard-Karls-Universitaet Tuebingen(ドイツ)

    • Related Report
      2017 Research-status Report
  • [Journal Article] Retention characteristics of poly(N-(1H-tetrazole-5-yl)-methacrylamide)-bonded stationary phase in hydrophilic interaction chromatography2020

    • Author(s)
      Fu Xiaoqing、Cebo Malgorzata、Ikegami Tohru、L?mmerhofer Michael
    • Journal Title

      Journal of Chromatography A

      Volume: 1609 Pages: 460500-460500

    • DOI

      10.1016/j.chroma.2019.460500

    • Related Report
      2019 Annual Research Report
    • Peer Reviewed / Int'l Joint Research
  • [Journal Article] The relationship between polymer structures on silica particles and the separation characteristics of the corresponding columns for hydrophilic interaction chromatography2020

    • Author(s)
      Taniguchi Ashin、Tamura Saki、Ikegami Tohru
    • Journal Title

      Journal of Chromatography A

      Volume: 1618 Pages: 460837-460837

    • DOI

      10.1016/j.chroma.2019.460837

    • Related Report
      2019 Annual Research Report
    • Peer Reviewed
  • [Journal Article] Separation of carbohydrate isomers and anomers on poly-N-(1H-tetrazole-5-yl)-methacrylamide-bonded stationary phase by hydrophilic interaction chromatography as well as determination of anomer interconversion energy barriers2020

    • Author(s)
      Fu Xiaoqing、Cebo Malgorzata、Ikegami Tohru、Laemmerhofer Michael
    • Journal Title

      Journal of Chromatography A

      Volume: 1620 Pages: 460981-460981

    • DOI

      10.1016/j.chroma.2020.460981

    • Related Report
      2019 Annual Research Report
    • Peer Reviewed / Int'l Joint Research
  • [Journal Article] Fragment-based Design of Zwitterionic, Strong Cation- and Weak Anion-Exchange Type Mixed-mode Liquid Chromatography Ligands and their Chromatographic Exploration2020

    • Author(s)
      Ferri Martina、Baeurer Stefanie、Carotti Andrea、Wolter Marc、Alshaar Belal、Theiner Johannes、Ikegami Tohru、West Caroline、Laemmerhofer Michael
    • Journal Title

      Journal of Chromatography A

      Volume: 1621 Pages: 461075-461075

    • DOI

      10.1016/j.chroma.2020.461075

    • Related Report
      2019 Annual Research Report
    • Peer Reviewed / Int'l Joint Research
  • [Journal Article] Hydrophilic interaction chromatography for the analysis of biopharmaceutical drugs and therapeutic peptides: A review based on the separation characteristics of the hydrophilic interaction chromatography phases2019

    • Author(s)
      Ikegami Tohru
    • Journal Title

      Journal of Separation Science

      Volume: 42 Issue: 1 Pages: 130-213

    • DOI

      10.1002/jssc.201801074

    • Related Report
      2018 Research-status Report
    • Peer Reviewed / Int'l Joint Research
  • [Journal Article] Method optimization of hydrophilic interaction chromatography separation of nucleotides using design of experiment approaches I: Comparison of several zwitterionic columns2018

    • Author(s)
      Arase Shuntaro、Kimura Susumu、Ikegami Tohru
    • Journal Title

      Journal of Pharmaceutical and Biomedical Analysis

      Volume: 158 Pages: 307-316

    • DOI

      10.1016/j.jpba.2018.05.014

    • Related Report
      2018 Research-status Report
    • Peer Reviewed
  • [Journal Article] High-performance liquid chromatographic separation of 8-aminopyrene-1,3,6-trisulfonic acid labeled N -glycans using a functional tetrazole hydrophilic interaction liquid chromatography column2018

    • Author(s)
      Yamamoto Sachio、Kinoshita Mitsuhiro、Ikegami Toru、Suzuki Shigeo
    • Journal Title

      Journal of Chromatography A

      Volume: 1566 Pages: 44-50

    • DOI

      10.1016/j.chroma.2018.06.050

    • Related Report
      2018 Research-status Report
    • Peer Reviewed
  • [Journal Article] Molecular Structure of Poly(vinyl alcohol)-Derived Carbon-Centered Radicals Studied by Rapid-Flow and Spin-Trapping ESR Measurements: A Short-Lived Intermediate Radical in the Initial Stage of the Graft Polymerization Reaction2017

    • Author(s)
      Yuko Nishihara, Kazuma Matsui, Keiko Kuwabara, Naoya Murata, Tomoko Yamaguchi, Yusuke Miyake, Tohru Ikegami, Kenji Kanaori, and Kunihiko Tajima
    • Journal Title

      Bulletin of the Chemical Society of Japan

      Volume: 90 Issue: 2 Pages: 244-253

    • DOI

      10.1246/bcsj.20160332

    • NAID

      130005332366

    • ISSN
      0009-2673, 1348-0634
    • Related Report
      2017 Research-status Report
    • Peer Reviewed / Open Access / Acknowledgement Compliant
  • [Journal Article] Rapid-Flow and Spin-Trapping ESR Study on Carbonyl-Conjugated Radicals of Modified Poly(vinyl alcohol) Bearing 1,2-Propanediol Pendant Moiety as Intermediates of Graft Copolymerization2017

    • Author(s)
      Matsui, Kazuma; Nishihara, Yuko; Yamaguchi, Tomoko; Sakurai, Yasuhiro; Miyake, Yusuke; Ikegami, Tohru; Kanaori, Kenji; Tajima, Kunihiko
    • Journal Title

      Bulletin of the Chemical Society of Japan

      Volume: 90 Issue: 12 Pages: 1293-1308

    • DOI

      10.1246/bcsj.20170235

    • NAID

      130006250362

    • ISSN
      0009-2673, 1348-0634
    • Related Report
      2017 Research-status Report
    • Peer Reviewed
  • [Presentation] 親水性相互作用クロマトグラフィー用HPLC カラムにおけるシリカ粒子上のポリマー形態と分離特性の関係についての研究2019

    • Author(s)
      谷口亜紳, 池上 亨
    • Organizer
      第 26 回クロマトグラフィーシンポジウム
    • Related Report
      2019 Annual Research Report
  • [Presentation] MUSHROOM- OR BRUSH-TYPE POLYACRYLAMIDE ON SILICA: RELATIONSHIP BETWEEN POLYMER SHAPES AND SEPARATION CHARACTERISTICS OF HILIC STATIONARY PHASES2019

    • Author(s)
      Tohru Ikegami, Ashin Taniguchi
    • Organizer
      48TH International Symposium on High-Performance Liquid Phase Separations and Related Techniques
    • Related Report
      2019 Annual Research Report
    • Int'l Joint Research
  • [Presentation] STUDY ON RELATIONSHIP BETWEEN POLYMER STRUCTURES ON SILICA PARTICLES AND THE SEPARATION CHARACTERISTICS OF THE CORRESPONDING HPLC COLUMNS FOR HYDROPHILIC INTERACTION CHROMATOGRAPHY2019

    • Author(s)
      Ashin Taniguchi, Kazuki Ito, Saki Tamura, Tohru Ikegami
    • Organizer
      48TH International Symposium on High-Performance Liquid Phase Separations and Related Techniques
    • Related Report
      2019 Annual Research Report
    • Int'l Joint Research
  • [Presentation] Characterization of DCpak PTZ HILIC phase and its application to the separation of monosaccharides2019

    • Author(s)
      Xiaoqing Fu, Malgorzata Cebo, Tohru Ikegami, Michael Laemmerhofer
    • Organizer
      49th International Symposium on High Performance Liquid Phase Separations and Related Techniques
    • Related Report
      2019 Annual Research Report
    • Int'l Joint Research
  • [Presentation] PREPARATION OF QUININE- AND QUINIDINE BASED ZWITTERIONIC CHIRAL STATIONARY PHASES FOR HPLC USING A THIOL-CLICK REACTION, AND THEIR CHROMATOGRAPHIC CHARACTERIZATION2018

    • Author(s)
      Martina Ferri, Tohru Ikegami, Stefanie Baeurer, Michael Laemmerhofer
    • Organizer
      ISCC-42nd International Symposium on Capillary Chromatography 2018
    • Related Report
      2018 Research-status Report
    • Int'l Joint Research
  • [Presentation] Development and Characterization of a Novel HILIC Stationary Phase Modified with Poly(glycidyl methacrylate) Using Surface Initiated-Atom Transfer Radical Polymerization2018

    • Author(s)
      Ashin Taniguchi, Tohru Ikegami
    • Organizer
      ISC 2018 32nd International Symposium on Chromatography
    • Related Report
      2018 Research-status Report
    • Int'l Joint Research
  • [Presentation] Tohru Ikegami2018

    • Author(s)
      Significantly High Hydrophilicity of a New HILIC Column Modified with Brush-Type Polyacrylamide: Relationship Between the Polymer Structure and the Chromatographic Characteristics
    • Organizer
      ISC 2018 32nd International Symposium on Chromatography
    • Related Report
      2018 Research-status Report
    • Int'l Joint Research
  • [Presentation] 双性イオン型キラル分離媒体の部分構造と分離特性の相 関に関する研究2018

    • Author(s)
      Martina Ferri1 池上 亨 Stefanie Baeurer Michael Laemmerhofer
    • Organizer
      第29回 クロマトグラフィー科学会議
    • Related Report
      2018 Research-status Report
  • [Presentation] Mushroom- or brush-type polymers on silica? Development and characterization of HILIC stationary phases modified with polyacrylamide.2017

    • Author(s)
      Tohru Ikegami, Kazuki Itoh, Saki Tamura, Tomoyuki Okada
    • Organizer
      HPLC 2017 PRAGUE
    • Related Report
      2017 Research-status Report
    • Int'l Joint Research
  • [Presentation] Development and characterization of HILIC stationary phases modified with polymers possessing chiral group based on cysteine derivatives.2017

    • Author(s)
      Ashin Taniguchi, Tohru Ikegami
    • Organizer
      HPLC 2017 PRAGUE
    • Related Report
      2017 Research-status Report
    • Int'l Joint Research
  • [Presentation] HPLCカラムの分離特性解析2017

    • Author(s)
      池上 亨
    • Organizer
      第28回クロマトグラフィー科学会議
    • Related Report
      2017 Research-status Report
    • Invited
  • [Presentation] 実験計画法による双性イオン型カラムを用いたヌクレオチド分離メソッドの最適化2017

    • Author(s)
      新瀬俊太郎、木村 進、池上 亨
    • Organizer
      第28回クロマトグラフィー科学会議
    • Related Report
      2017 Research-status Report

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Published: 2017-04-28   Modified: 2021-02-19  

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