Abstract
Background: In the modern clinical practice of TCM science, the formula Xihuang pill has been widely used as a remedy for the treatment of various tumors in clinical application. Due to the diversity of the manufacturers and relatively lower quality standards, the quality problem of Xihuang pill frequently resulted in unstable effect in clinical application. It is imperative to develop more effective and comprehensive quality control method capable of ensuring the safety and efficacy. The objective of our study is to introduce GC-FID/GC-MS for multiple components quantification and fingerprint description of the volatile oil in Xihuang pill.
Methods: A GC-FID method was developed for a chemical fingerprint analysis of Xihuang pill, and gas chromatography coupled with mass spectrometry was applied for the identification of major components in the fingerprints. In order to systematically validate the method, specificity, precision, repeatability and stability were measured. Fingerprints data analysis was mainly performed by three pieces of original software, namely ‘Similarity evaluation system for chromatographic fingerprint of TCM’, SPSS and SIMCA-P+. The similarities of ten batches of Xihuang pill were characterized using cluster analysis, PCA and similarity analysis. Results: The Euclidean distance, cosine, and correlation coefficient of the 10 batches of Xihuang pill were greater than 0.89, which showed that samples from different batches were basically the same and consistent, despite some slightly differences of chemical indexes were found. The results of cluster analysis, PCA and similarity analysis were consistent with each other, and the principal component factors that had significant correlation with the similarity were analyzed. Combined with GC-MS, total of 22 volatiles among 32 separated ones were identified by searching spectra database and literatures, and their relative content was calculated by using peak area normalization method. Conclusion: The GC-FID fingerprint combined with a variety of statistical and stoichiometry approach could be readily utilized for comprehensive quality assessment and control of Xihuang pill.Keywords: Xihuang Pill, GC/GC-MS, fingerprint, qualitative analysis, quality control, TCM science.
Graphical Abstract
37
2