目的 建立腰痹通胶囊(Yaobitong Capsules,YC)的HPLC指纹图谱及多成分定量测定方法,并结合相关化学计量学评价多批次制剂的质量。方法 建立YC的指纹图谱,采用层次聚类分析(hierarchical cluster analysis,HCA)、主成分分析(principal component analysis,PCA)评价多批次制剂质量,同时采用Hotelling's T²和DModX方法对不同批次制剂的质量设定控制范围;HPLC法测定多批次YC中绿原酸、芍药内酯苷、芍药苷、阿魏酸4种有效成分的含量,并结合聚类热图分析进行质量评价。结果 YC指纹图谱方法学考察结果符合测定要求,标记17个共有峰,并对共有峰进行归属,通过对照品比对指认出8个色谱峰,14批样品相似度大于0.90;HCA和PCA中未见异常批次,表明批间一致性较好,Hotelling's T²和DModX控制上限为15.077和1.653;14批YC样品中芍药内酯苷、芍药苷、绿原酸、阿魏酸的质量分数分别为1.733~2.853、4.674~8.127、1.128~2.417、0.586~1.232 mg/g,线性关系良好(r ≥ 0.999 3);聚类热图分析结果表明,14批样品可聚为3类。结论 建立的HPLC指纹图谱方法和多成分含量测定方法准确可靠,可用于YC的质量评价。多批次制剂数据结合化学计量学评价方法,表明YC多批次制剂之间一致性较好。

Objective To establish an HPLC fingerprint method and a method for the determination of multi-component content of Yaobitong Capsules (腰痹通胶囊, YC), and to evaluate the quality of multiple batches of the product by combining related chemometrics methods. Methods Based on the fingerprinting of lumbar paralysis capsules, hierarchical cluster analysis (HCA) and principal component analysis (PCA) were used to evaluate the quality of multiple batches of samples, while Hotelling's T² and DModX methods were used to establish control ranges for the quality of different batches of products; The content of four active ingredients, namely chlorogenic acid, albiflorin, paeoniflorin and ferulic acid, in multiple batches of YC was determined by HPLC and the quality was evaluated by cluster heat map analysis. Results The results of fingerprint methodology of YC were in accordance with the requirements of the determination, 17 common peaks were labeled, and eight chromatographic peaks were identified by standard comparison, and the similarity of samples from 14 batches was more than 0.90. No abnormal batches were found in HCA and PCA, indicating good inter-batch consistency. The upper limits of Hotelling's T² and DModX control were 15.077 and 1.653, respectively. The contents of albiflorin, paeoniflorin, chlorogenic acid, and ferulic acid in 14 batches of YC samples ranged from 1.733 to 2.853 mg/g, 4.674 to 8.127 mg/g, 1.128 to 2.417 mg/g and 0.586 to 1.232 mg/g, respectively, with a good linearity (r ≥ 0.999 3). The results of cluster heat map analysis showed that 14 batches of samples could be clustered into three categories. Conclusion The fingerprint method and the multi-component content determination method are accurate and reliable, which could be used for the quality evaluation of YC. The multi-batch product data combined with the chemometric method can be used for the stability control and quality evaluation of YC.

国家中医药管理局基于重点研究室研究领的中医药多学科研究能力提升项目——中药提取精制新技术；连云港市揭榜挂帅项目——中药口服固体制剂智能化连续制造关键技术研究