Quality evaluation of Shirebi Tablets based on combinative methods of HPLC fingerprint, quantitative analysis of multi-components and chemometrics analysis / 中草药

ABSTRACT

Objective: To establish a quality evaluation method of Shirebi Tablet based on HPLC fingerprints, quantitative analysis of multi-components and chemometrics analysis. Methods: The chromatographic column was Waters Symmetry C18 column (250 mm × 4.6 mm, 5 μm), and the column temperature was set at 30 ℃. The detection wavelength was set at 303 nm (for mulberroside A, mulberroside F and moracin M) and 270 nm (for forsythoside B, forsythoside A, forsythin, atractylodinol, atractylenolide II, and atractylodin). The mobile phase was composed of acetonitrile-0.2% phosphate acid solution in gradient elution manner at a flow rate of 1.0 mL/min. The HPLC fingerprint of Shirebi Tablet was established, the common peaks were determined by similarity evaluation system for chromatographic fingerprint of TCM (Version 2012.130723), and the similarity was calculated. The content determination methods for mulberroside A, mulberroside F, moracin M, forsythoside B, forsythoside A, forsythin, atractylodinol, atractylenolide II, and atractylodin were validated. The chemometrics methods such as cluster analysis and principal component analysis were used to evaluate the quality of Shirebi Tablet from different batches based on the results of fingerprint common peak area. Results: The fingerprint of Shirebi Tablet was established. Sixteen common peaks were identified. The similarity of fingerprints of 10 batches of Shirebi Tablet was more than 0.95. Nine components had good linear relationship in the range of mass concentration (r2 ≥ 0.999 1), and the average recoveries were 98.87%, 97.44%, 97.94%, 98.39%, 100.13%, 99.06%, 96.80%, 98.44% and 99.15% with the RSDs of 1.42%, 1.17%, 1.30%, 0.91%, 0.86%, 1.23%, 1.08%, 1.37% and 0.79%, respectively. The concentrations of mulberroside A, mulberroside F, moracin M, forsythoside B, forsythoside A, forsythin, atractylodinol, atractylenolide II, and atractylodin in 10 batches were 0.192—0.289, 0.057—0.095, 0.113—0.158, 0.309—0.375, 1.537—1.916, 0.478—0.596, 0.049—0.072, 0.279—0.354, and 0.629—0.759 mg/g, respectively. The results of cluster analysis showed that 10 batches of Shirebi Tablet were clustered into two groups, and the results of principal component analysis showed that the principal components 1—6 were the main factor affecting the quality evaluation of Shirebi Tablets. Conclusion: The method is simple, accurate and reproducible, which can be used for the quality control and evaluation of Shirebi Tablet.