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Simultaneous Determination of Resibufogenin and Its Major Metabolite 3-epi-Resibufogenin in Rat Plasma by HPLC Coupled with Tandem Mass Spectrometry
Chen, Huirong1,2; Deng, Sa1; Chang, Peter R.3; Wang, Changyuan1; Ma, Xiaochi1; Liu, Kexin1; Tian, Yan1; Yao, Jihong1; Guo, Xiaoyu2
关键词Resibufogenin 3-epi-Resibufogenin LC-ESI-MS/MS Pharmacokinetics Metabolite
刊名CHROMATOGRAPHIA
2012-02-01
DOI10.1007/s10337-011-2165-5
75期:3-4页:103-109
收录类别SCI
文章类型Article
WOS标题词Science & Technology
类目[WOS]Biochemical Research Methods ; Chemistry, Analytical
研究领域[WOS]Biochemistry & Molecular Biology ; Chemistry
关键词[WOS]BUFADIENOLIDES ; CHROMATOGRAPHY ; CINOBUFAGIN ; BUFALIN ; EXTRACT ; KETONES ; CHANSU ; CELLS
英文摘要

A rapid, sensitive and specific method for the simultaneous quantification of resibufogenin (RBG) and 3-epi-resibufogenin (3-ERBG) in rat plasma was developed by using a liquid-liquid extraction procedure and liquid chromatography-electrospray ionization/tandem mass spectrometric (LC-ESI-MS/MS) analysis. The separation was performed by HPLC on a reversed phase C(18) HPLC column (150 x 2.1 mm, 3.5 mu m) using a mobile phase of acetonitrilel-0.1% formic acid aqueous solution (45:55, v/v). The determination was performed by a triple-quadrupole mass spectrometer in the multiple reaction monitoring using positive mode of electrospray ionization (ESI). The calibration curves were both linear (R > 0.995) over the concentration range of 3.0-5,000 ng mL(-1), and the lower limits of quantification were 3.0 ng mL(-1) for both RBG and 3-ERBG. The intra-day and inter-day precisions (% RSD) were all less than 15%, and the accuracies (%RE) were within the range of +/- 15%. The mean recoveries of RBG, 3-ERBG and IS were over 82.7, 84.8 and 90.0% (n = 6), respectively. The method was proved to be rapid, sensitive and specific, and has been successfully applied to determine RBG and its major metabolite 3-ERBG in rat plasma after oral administration of RBG for pharmacokinetic study. Comparison of pharmacokinetic data with anti-tumor activities of RBG and ERBG suggested that 3-ERBG, as a major metabolite of RBG in rats, was perhaps also a bioactive form of RBG in vivo.

语种英语
WOS记录号WOS:000299486100003
项目编号LS2010059 ; 30701088 ; 81073013 ; 81160559
资助机构Education Department of Liaoning Province ; Program for Liaoning Excellent Talents in University (LNET) ; National Natural Science Foundation of China
引用统计
被引频次:5[WOS]   [WOS记录]     [WOS相关记录]
文献类型期刊论文
条目标识符http://ir.bjmu.edu.cn/handle/400002259/63028
专题北京大学药学院_天然药物学系
作者单位1.Dalian Med Univ, Sch Pharm, Dalian 116044, Peoples R China
2.Peking Univ, Sch Pharmaceut Sci, Dept Nat Med, Beijing 100191, Peoples R China
3.Agr & Agri Food Canada, Bioprod & Bioproc Natl Sci Program, Saskatoon, SK S7N 0X2, Canada
推荐引用方式
GB/T 7714
Chen, Huirong,Deng, Sa,Chang, Peter R.,et al. Simultaneous Determination of Resibufogenin and Its Major Metabolite 3-epi-Resibufogenin in Rat Plasma by HPLC Coupled with Tandem Mass Spectrometry[J]. CHROMATOGRAPHIA,2012,75(3-4):103-109.
APA Chen, Huirong.,Deng, Sa.,Chang, Peter R..,Wang, Changyuan.,Ma, Xiaochi.,...&Guo, Xiaoyu.(2012).Simultaneous Determination of Resibufogenin and Its Major Metabolite 3-epi-Resibufogenin in Rat Plasma by HPLC Coupled with Tandem Mass Spectrometry.CHROMATOGRAPHIA,75(3-4),103-109.
MLA Chen, Huirong,et al."Simultaneous Determination of Resibufogenin and Its Major Metabolite 3-epi-Resibufogenin in Rat Plasma by HPLC Coupled with Tandem Mass Spectrometry".CHROMATOGRAPHIA 75.3-4(2012):103-109.
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