High-performance liquid chromatography/electron capture atmospheric pressure chemical ionization-mass spectrometric determination of biologically active steroids

  • HIGASHI Tatsuya
    Division of Pharmaceutical Sciences, Graduate School of Natural Science and Technology, Kanazawa University
  • SHIMADA Kazutake
    Division of Pharmaceutical Sciences, Graduate School of Natural Science and Technology, Kanazawa University

Bibliographic Information

Other Title
  • 電子捕獲大気圧化学イオン化を利用する生理活性ステロイドの高速液体クロマトグラフィー/質量分析
  • デンシ ホカク タイキアツ カガク イオンカ オ リヨウ スル セイリ カッセイ ステロイド ノ コウソク エキタイ クロマトグラフィー シツリョウ ブンセキ

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Abstract

Steroids are essential bio-molecules for the maintenance of life. Kinetic and functional analyses of steroids are necessary to elucidate the nature of the many endocrine disease processes, and thus be useful for diagnosis and treatment. High-performance liquid chromatography/mass spectrometry (LC/MS) has recently been used for steroid analysis due to its specificity and versatility. However, conventional LC/MS sometimes does not demonstrate the required sensitivity for the trace analysis of steroids in biological samples, because the ionization efficiencies of most steroids are relatively low for electrospray ionization and usual atmospheric pressure chemical ionization (APCI). On the other hand, electron-affinitive compounds are efficiently ionized by the electron capture reaction in APCI in the negative-ion mode (electron capture APCI). Therefore, in this mode, a high sensitivity can be obtained by tagging steroids with electron-affinitive (electron capturing) moieties. On this basis, we have developed detection-oriented derivatization methods for the LC/electron capture APCI-MS analysis of steroids and applied these methods to the determination of vitamin D3 metabolites in human plasma and to the analysis of changes in rat brain neurosteroid levels by acute stress.<br>

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 53 (7), 645-655, 2004

    The Japan Society for Analytical Chemistry

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