固肠止泻丸及中间体的多波长HPLC-DAD指纹图谱质量评价

目的: 建立固肠止泻丸平行5波长HPLC指纹谱,鉴定固肠止泻丸及中间体质量,以主成分分析比较固肠止泻丸及中间体主要的药效物质变化。 方法: 以平行5波长HPLC梯度洗脱方法结合系统指纹定量法对12批固肠止泻丸及中间体的质量进行鉴定。运用主成分分析(PCA)对两者的药效物质特征峰进行区分。 结果: 以盐酸小檗碱为参照物峰,确定了21个共有峰。系统指纹定量法评价结果显示,除230 nm外,其他4个波长下测到的各批样品质量合格。PCA结果显示,固肠止泻丸制剂和中间体之间仍存在显著差异。与固肠止泻丸中间体特征指纹图谱相比,固肠止泻丸有9个成分峰在成药后含量显著降低。在13.05 min附近有2个峰消失。 结论: 建立了固肠止泻丸及中间体的HPLC指纹图谱。并比较了两者的差异。以系统指纹定量法评价中药制剂的质量,方法快捷、有效和可靠,为固肠止泻丸的整体质控提供了参考依据。

SQFM Methods Based on HPLC-DAD with Five Wavelengths for Fingerprint Determination of Guchang Zhixie Pill and Powders

Objective: Due to the difficulties of dealing with traditional Chinese medicine quality controlling, systematic quantified fingerprint method (SQFM) and the principal component analysis (PCA) were performed to evaluate the quality of Guchang Zhixie (GCZX) pill and powders. Method: The pill and powders were determined by high performance liquid chromatography with diode array detector (HPLC-DAD). Five absorption wavelengths (254, 345, 230, 240,280 nm) were applied to reflect the characterization of six main components from GCZX pill and powders. The 12 batches analytes were processed by SQFM and PCA approaches and berberine hydrochloride was used as reference peak. Result: Refer to berberine hydrochloride peak, 21 common peaks were obtained. According to the results of the SQFM and PCA analysis, qualities of all batches analytes were qualified, except the results under 230 nm. Compared to GCZX powders` fingerprint, a distinct distance from the pills could be investigated on PCA scores plot, meanwhile, 9 component peaks reduced after prepared and 2 peaks disappeared around 13.05 min. Also, validation of the method has been performed. Conclusion: SQFM and PCA methods were successfully tested in GCZX pill and powders fingerprint studies. Results from assay validations showed that these two methods are selective, sensitive and robust. The developed methods were applied to Chinese traditional medicine evaluation.