Separatory Determination of Bile Acid 3-Sulfates by Liquid Chromatography/Electrospray Ionization Mass Spectrometry

✍ Scribed by Ikegawa, Shigeo; Yanagihara, Takamitsu; Murao, Naoaki; Watanabe, Hiroo; Goto, Junichi; Niwa, Toshifumi

• Publisher: John Wiley and Sons
• Year: 1997
• Tongue: English
• Weight: 370 KB
• Volume: 32
• Category: Article
• ISSN: 1076-5174
• DOI: 10.1002/(sici)1096-9888(199704)32:4<401::aid-jms488>3.0.co;2-e

✦ Synopsis

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 Ô H ]with a doubly charged ion [ M Ô 2H ] 2-, and the ratio of these negative ions was markedly inÑuenced by an acidic component of salt added to the mobile phase according to the value of the pK a 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 column with 20 mM ammonium acetate-methanol (10 : 12, v/v) by selected ion monitoring, monitored C 18 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.

1997 by John