LC/ESI-tandem mass spectrometric determination of bile acid 3-sulfates in human urine 3β-sulfooxy-12α-hydroxy-5β-cholanoic acid is an abundant nonamidated sulfate

被引:47
作者
Goto, Takaaki
Myint, Khin Than
Sato, Koichi
Wada, Osamu
Kakiyama, Genta
Iida, Takashi
Hishinuma, Takanori
Mano, Nariyasu
Goto, Junichi [1 ]
机构
[1] Tohoku Univ, Grad Sch Pharmaceut Sci, Aoba Ku, Sendai, Miyagi 9808578, Japan
[2] Nihon Univ, Coll Humanities & Sci, Dept Chem, Setagaya Ku, Tokyo 1568550, Japan
[3] Tohoku Univ Hosp, Dept Pharmaceut Sci, Aoba Ku, Sendai, Miyagi 9808574, Japan
来源
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES | 2007年 / 846卷 / 1-2期
关键词
bile acid; sulfate; liquid chromatography/tandem mass spectrometry; electrospray ionization; human; urine;
D O I
10.1016/j.jchromb.2006.08.013
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
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 3(3,12o-dihydroxy-5(3-cholanoic acid 3-sulfate. (c) 2006 Elsevier B.V. All rights reserved.
引用
收藏
页码:69 / 77
页数:9
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