Abstract

European Journal of Mass Spectrometry
Volume 15 Issue 4, Pages 531–539 (2009)
doi: 10.1255/ejms.1006

Identification of the metabolites of ecabet bismuth in rat bile by liquid chromatography-electrospray ionization-tandem mass spectrometry

Yue Wu,^a Jing Yang,^a, Li Ding,^a,* Guili Xu,^b,* Wenjuan Qian,^a Changhong Yun,^a and Jianchang He^b
a Department of Pharmaceutical Analysis, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China. E-mail: dinglidl@hotmail.com
^bKunming General Hospital affiliated to Chengdu Region of PLA, Kunming 650032, China

In the present study, a liquid chromatography-electrospray ionization-tandem mass spectrometry (LC- ESI-MS/MS) method was developed for the screening and the structural elucidation of the metabolites of ecabet bismuth in rat bile. Solid-phase extraction cartridges were used for sample pre-treatment and a gradient liquid chromatographic system composed of 10 mM ammonium acetate buffer and methanol was used for chromatographic separation on a Phenomenex Kromasil C18 column. The triple quadrupole mass spectrometer was employed to thoroughly detect and acquire the detailed MS/MS spectra of ecabet and its metabolites. By comparing the chromatographic retention behaviors, as well as the changes in molecular weight and full-scan MS/MS spectra of the potential metabolites with those of the parent compound, two main metabolites were identified as glucuronide conjugate of carbonylated ecabet (7-oxo-ecabet) and glucuronide conjugate of ecabet. Both two metabolites have not been reported in the literatures. The metabolic pathways of ecabet in rat were also proposed in this paper.

Keywords: ecabet bismuth, ecabet, tricyclic diterpene carboxylic acid, metabolite, structural identification, RDA fragmentation, LC-ESI-MS/MS, CID, metabolism

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