Separatory determination of bile acid 3-sulfates by liquid chromatography/electrospray ionization mass spectrometry

Shigeo Ikegawa, Takamitsu Yanagihara, Naoaki Murao, Hiroo Watanabe, Jimichi Goto, Toshifumi Niwa

Research output: Contribution to journalArticle

45 Citations (Scopus)

Abstract

A method for the separatory determination of bile acid 3-sulfates by liquid chromatography (LC)/electrospray ionization (ESI) mass spectrometry (MS) was developed. The sulfates were characterized by an abundant pseudomolecular ion [M - H]- with a doubly charged ion [M - 2H]2-, and the ratio of these negative ions was markedly influenced by an acidic component of salt added to the mobile phase according to the pK(a) value of the conjugated form at C-24. The resolution into unconjugated and glycine- and taurine-conjugated cholic acid, chenodeoxycholic acid, deoxycholic acid, ursodeoxycholic acid and lithocholic acid 3-sulfates was achieved on a Capcell Pak C18 column with 20 mM ammonium acetate-methanol (10:12, v/v) by selected ion monitoring, monitored with their corresponding pseudo-molecular ions. The combined use of stable isotope-labeled compounds as internal standards in LC/MS was applied to the determination of bile acid 3-sulfates in human urine.

Original languageEnglish
Pages (from-to)401-407
Number of pages7
JournalJournal of Mass Spectrometry
Volume32
Issue number4
DOIs
Publication statusPublished - 1997 Jan 1

Keywords

  • Bile acid 3-sulfates
  • Electrospray ionization
  • Liquid chromatography/mass spectrometry
  • O-Labeling
  • Selected ion monitoring

ASJC Scopus subject areas

  • Spectroscopy

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