Chemical Research in Chinese Universities ›› 2019, Vol. 35 ›› Issue (6): 962-966.doi: 10.1007/s40242-019-9275-2

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Measurement of Free and Glucuronidated Cardamonin in Rat Plasma and Bile Using UPLC-MS/MS and Its Application to a Pharmacokinetic and Bile Excretion Study

WU Yi, JING Runan, JIA Guihua, WANG Yixiao, YU Tianmiao, ZHANG Weidong   

  1. School of Pharmaceutical Sciences, Jilin University, Changchun 130021, P. R. China
  • Received:2019-10-11 Revised:2019-10-28 Online:2019-12-01 Published:2019-11-29
  • Contact: ZHANG Weidong E-mail:weidongzhang@jlu.edu.cn
  • Supported by:
    Supported by the Science and Technology Development Plan of Jilin Province, China(No.20180101302JC), the Youth Technology Backbone Training Program of Health Department of Jilin Province, China(No.2017Q020), the Bethune Project of Jilin University, China(No.2018A08), the 13th Five-year Science and Technology Research Plan of the Education Department of Jilin Province, China(No.JJKH20190107KJ).

Abstract: A rapid and accurate ultra-high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry(UPLC-MS/MS) method was established and validated for the measurement of two forms of cardamonin, i.e., free and glucuronidated, in the plasma and bile of rats. Cardamonin and an internal standard (1,8-dihydroxyanthraquinone) were extracted from plasma and bile with ethyl ether via liquid-liquid extraction. The analytes in the extracts were separated by an Agilent Zorbax Stable Bond-C18 column(2.1 mm×50 mm, 1.8 μm) under isocratic elution conditions[acetonitrile(A) and 0.1% ammonium formate in water(B), 40:60(volume ratio)] with a flow rate of 0.4 mL/min, and mass spectrometry in negative ion MRM mode was implemented for analysis. Good linearity over the wide ranges of 0.01-5 μg/mL for plasma and 0.025-10 μg/mL for bile samples was acquired. Method validation was performed according to the FDA guidelines for bioanalytical methods.

Key words: Glucuronidated cardamonin, Pharmacokinetics, Bile excretion, Ultra-high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-MS/MS)