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

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Abstract

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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Authors and Affiliations

  1. Graduate School of Pharmaceutical Sciences, Tohoku University, Aobayama, Sendai, 980-8578, Japan

    Shigeo Ikegawa, Hiroko Okuyama, Junji Oohashi, Naoaki Murao & Junichi Goto

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  1. Shigeo Ikegawa
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  2. Hiroko Okuyama
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  3. Junji Oohashi
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  4. Naoaki Murao
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  5. Junichi Goto
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Ikegawa, S., Okuyama, H., Oohashi, J. et al. Separation and Detection of Bile Acid 24-Glucuronides in Human Urine by Liquid Chromatography Combined with Electrospray Ionization Mass Spectrometry. ANAL. SCI. 15, 625–631 (1999). https://doi.org/10.2116/analsci.15.625

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  • DOI: https://doi.org/10.2116/analsci.15.625

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