Simultaneous Determination of Resibufogenin and Cinobufagin in Chinese Medicine Ch’an Su by GC–MS Following Microwave-Assisted Silylation

• DOI: 10.1365/s10337-009-0973-7
• Publication Date: 2009-02-03T19:16:51Z
• Authors: Xiaoyan Zhu; Zhiqiang Meng; Zhen Chen; Luming Liu
• Keywords: Trimethylsilyl; BSTFA

Resibufogenin and cinobufagin are the major bioactive constituents in the Chinese medicine Ch’an Su. In this paper, a novel, simple and rapid method was developed for the qualitative analysis of the two main compounds, which was based on microwave-assisted silylation followed by gas chromatography–mass spectrometry. The components of resibufogenin and cinobufagin were derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide under microwave irradiation, and the trimethylsilyl derivatives formed were analyzed by GC–MS. The derivatization conditions including microwave power and irradiation time were investigated, and the method validations (linear range, detection limit, precision and recovery) were also studied. The experimental results indicate that microwave-assisted silylation followed by GC–MS analysis is a new method for the determination of resibufogenin and cinobufagin in the Ch’an Su samples.