ガスクロマトグラフィー : 質量分析法による胆汁酸生合成中間体の定量法の開発  [in Japanese] Development of an analytical method for intermediates in bile acid biosynthesis by GC/MS  [in Japanese]

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Author(s)

Abstract

モノヒドロキシ胆汁酸 (3α-hydroxy-5β-cholan-24-oic acid及び3β-hydroxy-5-cholen-24-oic acid) は胆汁うっ滞を誘起する原因物質の一つであり, これらの新規生成経路の存在が推測されている. また, 胆汁酸生合成機構の一つとして, 25位水酸化による側鎖切断反応が知られている. 上記胆汁酸の生成機構と本経路の関連を検討することを目的として, 生合成中間体と推測される各種胆汁アルコール, ヒドロキシコレステロール及び上記胆汁酸のGC/MSによる一斉分析法の開発を行った. 各種中間体標品をトリメチルシリルエーテル誘導体とした後, 高分解能選択イオンモニタリング (SIM) 法により分析を行った. 得られた検量線はいずれも10~250pmolの範囲で良好な直線性を示した. 検出限界は50~100fmolであった. 逆相系固相抽出法を用いる前処理のみで生体由来の妨害ピークは認められなかった. 本分析法は各種生体試料中の上記中間体及び胆汁酸の分析法として適用可能であることが明らかとなった.

A method for the analysis of bile alcohols and hydroxycholesterols as intermediates in mono-hydroxyl bile acid biosynthesis has been developed by gas chromatography/mass spectrometry (GC/MS) with selected ion monitoring in a high-resolution mode. The linearity of the calibration curves for the bile alcohols, hydroxycholesterol and bile acids ranged from 10∼250 pmol (<i>r</i>>0.999), and the detection limits were 50∼100 fmol (<i>S/N</i> = 2∼6). The recoveries of the bile alcohols, hydroxycholesterol and bile acids from the rat liver mitochondrial fraction ranged over 97.9∼111%, respectively, of the added amounts of their standard samples. The present method was made available for the determination of bile alcohols, hydroxycholesterol and related monohydroxy bile acids in incubation mixtures after only a simple extraction procedure using a solid-phase extraction cartridge.

Journal

  • Bunseki kagaku

    Bunseki kagaku 51(6), 443-448, 2002-06-05

    The Japan Society for Analytical Chemistry

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Codes

  • NII Article ID (NAID)
    110002905087
  • NII NACSIS-CAT ID (NCID)
    AN00222633
  • Text Lang
    JPN
  • Article Type
    ART
  • ISSN
    05251931
  • NDL Article ID
    6185566
  • NDL Source Classification
    ZP4(科学技術--化学・化学工業--分析化学)
  • NDL Call No.
    Z17-9
  • Data Source
    CJP  NDL  NII-ELS  J-STAGE  NDL-Digital 
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