LC/ESI-tandem mass spectrometric determination of bile acid 3-sulfates in human urine 3beta-Sulfooxy-12alpha-hydroxy-5beta-cholanoic acid is an abundant nonamidated sulfate.
We developed a highly sensitive and quantitative method to detect bile acid 3-sulfates in human urine employing liquid chromatography/electrospray ionization-tandem mass spectrometry. This method allows simultaneous analysis of bile acid 3-sulfates, including nonamidated, glycine-, and taurine-conjugated bile acids, cholic acid (CA), chenodeoxycholic acid (CDCA), deoxycholic acid (DCA), ursodeoxycholic acid (UDCA), and lithocholic acid (LCA), using selected reaction monitoring (SRM) analysis. The method was applied to analyze bile acid 3-sulfates in human urine from healthy volunteers. The results indicated an unknown compound with the nonamidated common bile acid 3-sulfates on the chromatogram obtained by the selected reaction monitoring analysis. By comparison of the retention behavior and MS/MS spectrum of the unknown peak with the authentic specimen, the unknown compound was identified as 3beta,12alpha-dihydroxy-5beta-cholanoic acid 3-sulfate.
Goto
Takaaki
T
Graduate School of Pharmaceutical Sciences, Tohoku University, Aobayama, Aoba-ku, Sendai 980-8578, Japan.
Myint
Khin Than
KT
Sato
Koichi
K
Wada
Osamu
O
Kakiyama
Genta
G
Iida
Takashi
T
Hishinuma
Takanori
T
Mano
Nariyasu
N
Goto
Junichi
J
D000328:Adult; D001647:Bile Acids and Salts / Q000652:urine*; D002793:Cholic Acids / Q000652:urine*; D002853:Chromatography, Liquid / Q000379:methods*; D006801:Humans; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
C518438:3beta-sulfooxy-12alpha-hydroxy-5beta-cholanoic acid; D001647:Bile Acids and Salts; D002793:Cholic Acids; C020980:bile acid sulfates