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

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Abstract

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.

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Acknowledgements

This work was supported by a research program from National Department of Science and Technology of China (Grant No. 2005DFA30130) and Postdoctoral Program of China (Grant No. 20060390619).

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Authors and Affiliations

  1. Department of Integrative Oncology, Cancer Hospital, Fudan University, No. 270, Dong An Road, 200032, Shanghai, People’s Republic of China

    Xiaoyan Zhu, Zhiqiang Meng, Zhen Chen & Luming Liu

  2. Department of Oncology, Shanghai Medical College, Fudan University, No. 130, Dong An Road, 200032, Shanghai, People’s Republic of China

    Xiaoyan Zhu, Zhiqiang Meng, Zhen Chen & Luming Liu

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  1. Xiaoyan Zhu
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  2. Zhiqiang Meng
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  3. Zhen Chen
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  4. Luming Liu
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Correspondence to Luming Liu.

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Zhu, X., Meng, Z., Chen, Z. et al. Simultaneous Determination of Resibufogenin and Cinobufagin in Chinese Medicine Ch’an Su by GC–MS Following Microwave-Assisted Silylation. Chroma 69, 749–754 (2009). https://doi.org/10.1365/s10337-009-0973-7

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