Improvement of Quality Standard of Shenwei Gubi Tablets and Changes of Transfer Rates of Its Quality Control Indicators in Production Based on Chemical Pattern Recognition Technology / 中国实验方剂学杂志

ABSTRACT

Objective:To improve the quality standard of Shenwei Gubi tablets， and to explore the reasons for the great difference in the contents of quality control index components between batches of this product. Method:The fingerprint of this product was established by HPLC， the determination was performed on Diamonsil C18 column （4.6 mm×250 mm， 5 μm） with acetonitrile （A）-0.1% phosphoric acid solution （B） for gradient elution （0-5 min， 10%A； 5-15 min， 10%-12%A； 15-30 min， 12%-26%A； 30-43 min， 26%-31%A， 43-50 min， 31%-40%A， 50-70 min， 40%-55%A； 70-84 min， 55%-72.5%A） as the mobile phase at detection wavelength of 230 nm. The orthogonal partial least squares-discriminant analysis-variable importance in the projection （OPLS-DA-VIP） map was drawn with the common peak as the independent variable. The contribution of 26 common peaks to the fingerprint differences among different batches of this product was quantified. By searching for the chromatographic peaks with great differences， combined with relevant literature， the components related to the clinical indications of the product were screened out and their contents were determined by specificity experiment， and the quantitative indicators were finally selected. HPLC-doide array detector （DAD） was employed to determine the contents of the above preferred indexes with detection wavelengths of 236， 276， 230， 322 nm， other conditions were the same as HPLC fingerprint detection method. Result:A total of 26 common peaks were calibrated on the HPLC fingerprint of Shenwei Gubi tablets. The similarity between the fingerprint of each batch samples and the reference fingerprint was≥0.950. Loganic acid， gentiopicroside， paeoniflorin and osthole were optimized as the quantitative indicators of this product， their average contents were 161.02， 401.80， 255.54， 80.68 μg·g-1. Conclusion:The established fingerprint and multi-index quantitative analysis method are stable and reliable， and can be used for quality control of Shenwei Gubi tablets. Difference in contents of quality control components between batches of raw materials and the imperfect quality control method of intermediates in the production process are the main reasons for the great difference in the contents of quality control indicators between batches of this product.