TY - JOUR
T1 - Separatory determination of bile acid 3-sulfates by liquid chromatography/electrospray ionization mass spectrometry
AU - Ikegawa, Shigeo
AU - Yanagihara, Takamitsu
AU - Murao, Naoaki
AU - Watanabe, Hiroo
AU - Goto, Jimichi
AU - Niwa, Toshifumi
PY - 1997
Y1 - 1997
N2 - 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.
AB - 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.
KW - Bile acid 3-sulfates
KW - Electrospray ionization
KW - Liquid chromatography/mass spectrometry
KW - O-Labeling
KW - Selected ion monitoring
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U2 - 10.1002/(SICI)1096-9888(199704)32:4<401::AID-JMS488>3.0.CO;2-E
DO - 10.1002/(SICI)1096-9888(199704)32:4<401::AID-JMS488>3.0.CO;2-E
M3 - Article
AN - SCOPUS:0030933887
SN - 1076-5174
VL - 32
SP - 401
EP - 407
JO - Journal of Mass Spectrometry
JF - Journal of Mass Spectrometry
IS - 4
ER -