Identification of a novel conjugate in human urine: bile acid acyl galactosides
Identification of a novel conjugate in human urine: bile acid acyl galactosides
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DOI：
10.1016/j.steroids.2004.12.006
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发表时间：
2005-03-01
期刊：
影响因子：
2.7
通讯作者：
Goto, J
中科院分区：
文献类型：
--
作者：
Goto, T;Shibata, A;Goto, J
我们报告了一种新型结合物——胆汁酸酰基半乳糖苷，它存在于健康志愿者的尿液中。为了鉴定健康受试者尿液样本中获得的两个未知峰，对样本进行固相萃取，然后进行液相色谱分离。收集对应于色谱图中未知峰的洗脱液。经过碱性水解和液相色谱 (LC)/电喷雾电离 (ESI)-质谱 (MS) 分析，胆酸 (CA) 和脱氧胆酸 (DCA) 被鉴定为释放的胆汁酸。当部分碱性水解产物与1-苯基-3-甲基5-吡唑啉酮进行衍生反应时，通过LC/ESI-MS检测到半乳糖衍生物。最后，将尿液标本中这些未知化合物的液相色谱和质谱性质与真实标本进行比较，确定其结构为CA 24-半乳糖苷和DCA 24-半乳糖苷。这些结果强烈表明，胆汁酸 24-半乳糖苷（一种新型缀合物）是在人体内合成的。 (c) 2005 Elsevier Inc. 保留所有权利。
We report a novel conjugate, bile acid acyl galactosides, which exist in the urine of healthy volunteers. To identify the two unknown peaks obtained in urine specimens from healthy subjects, the specimens were subjected to solid phase extraction and then to liquid chromatographic separation. The eluate corresponding to the unknown peaks on the chromatogram was collected. Following alkaline hydrolysis and liquid chromatography (LC)/electrospray ionization (ESI)-mass spectrometric (MS) analysis, cholic acid (CA) and deoxycholic acid (DCA) were identified as liberated bile acids. When a portion of the alkaline hydrolyzate was subjected to a derivatization reaction with 1-phenyl-3-methyl5-pyrazolone, a derivative of galactose was detected by LC/ESI-MS. Finally, the liquid chromatographic and mass spectrometric properties of these unknown compounds in urine specimens were compared to those of authentic specimens and the structures were confirmed as CA 24-galactoside and DCA 24-galactoside. These results strongly imply that bile acid 24-galactosides, a novel conjugate, were synthesized in the human body. (c) 2005 Elsevier Inc. All rights reserved.