Separation and Detection of Bile Acid 24-Glucuronides in Human Urine by Liquid Chromatography Combined with Electrospray Ionization Mass Spectrometry.

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  • IKEGAWA Shigeo
    Graduate School of Pharmaceutical Sciences, Tohoku University
  • OKUYAMA Hiroko
    Graduate School of Pharmaceutical Sciences, Tohoku University
  • OOHASHI Junji
    Graduate School of Pharmaceutical Sciences, Tohoku University
  • MURAO Naoaki
    Graduate School of Pharmaceutical Sciences, Tohoku University
  • GOTO Junichi
    Graduate School of Pharmaceutical Sciences, Tohoku University

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A method for the separation and determination of bile acid 24-glucuronides using liquid chromatography (LC)/electro-spray ionization (ESI)-mass spectrometry (MS) has been developed. In the ESI mode, 24-glucuronides were characterized by an intense deprotonated molecule [M-H]- with a fragment ion [M-H-176]- formed by elimination of the glucuronic acid moiety. The ratio of these negative ions was significantly influenced by the orifice-1 and the ring lens voltages. Bile acid 24-glucuronides in human urine were extracted with an OASIS HLB cartridge and then subjected to the LC/ESI-MS analysis employing an 18O-labeled internal standard. The simultaneous separation was attained on a Develosil ODS-HG-5 column using 20 mM ammonium acetate (pH 6.0)-acetonitrile (3:1→3:2, v/v, 35 min) in a linear gradient elution mode, where the 24-glucuronides were monitored with a characteristic negative ion [M-H]-; the limit of detection was 10 fmol. This newly developed method was applied to the quantitation of bile acid 24-glucuronides in human urine with satisfactory selectivity and reliability.

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  • Analytical Sciences

    Analytical Sciences 15 (7), 625-631, 1999

    社団法人 日本分析化学会

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