[关键词]
[摘要]
目的 建立3个主产地何首乌、炆何首乌、制何首乌共30批样品的HPLC指纹图谱及多成分含量测定方法,结合化学计量法对其进行质量评价。方法 采用HPLC建立何首乌及其炮制品的指纹图谱并进行6种成分的含量测定,通过层次聚类分析(clustering analysis,HCA)、主成分分析(principal component analysis,PCA)和正交偏最小二乘-判别分析(orthogonal partial least squares-discriminant analysis,OPLS-DA)评价不同批次何首乌的质量差异,找寻不同炮制品间质量差异性的主要成分。结果 30批何首乌、炆何首乌、制何首乌的HPLC指纹图谱中有20个共有峰,指认了6个共有峰,峰面积占比均在75%以上。没食子酸(峰1)、二苯乙烯苷(峰8)、大黄素-8-O-葡萄糖苷(峰14)、大黄素甲醚-8-O-葡萄糖苷(峰16)、大黄素(峰19)、大黄素甲醚(峰20)质量分数分别在0.59~5.86、4.64~25.83、0.03~3.11、0.01~0.59、0.07~1.98、0.25~1.81 mg/g。方法 学考察结果显示,各成分在线性关系良好(r≥0.999 7),平均回收率为97.80%~101.51%。指纹图谱相似度结果显示,何首乌及其2种炮制品各自10批的相似度均在0.99以上,但不同类型炮制品的相似度降低。HCA可将3者聚为3类,PCA结果提取了3个主成分,OPLS-DA能有效地将3种饮片明显区分,并根据VIP>1的原则筛选出了6种主要差异成分,共指认了大黄素甲醚-8-O-葡萄糖苷、大黄素-8-O-葡萄糖苷、没食子酸、大黄素甲醚4种与何首乌炮制品质量相关性较强的化学成分。结论 建立的何首乌及其炮制品HPLC指纹图谱结合化学计量法的方法简便准确,可为特色饮片炆何首乌的质量控制和品质评价提供参考依据。
[Key word]
[Abstract]
Objective To establish fingerprints and multi-component content determination method of 30 batches of Polygoni Multiflori Radix (PMR) from three main origins, braised Polygoni Multiflori Radix (BPMR), and Polygoni Multiflori Radix Praeparata (PMRP) by HPLC, so as to evaluate its quality in combination with chemometrics method. Methods The fingerprints of PMR and its processed products were established by HPLC and the content of six components was determined. Clustering analysis (HCA), principal component analysis (PCA) and orthogonal partial least squares-discrimination analysis (OPLS-DA) were used to evaluate the quality difference of different batches of PMR, and find the main components of the quality difference between different processed products. Results There were 20 common peaks in the fingerprints of 30 batches of PMR, BPMR and PMRP, and six common peaks were identified, the peak area ratios were all above 75%. The mass fractions of gallic acid (peak 1), stilbene glycosides (peak 8), emodin-8-O-glucoside (peak 14), emodin methyl ether-8-O-glucoside (peak 16), emodin (peak 19), and emodin methyl ether (peak 20) ranged from 0.59-5.86, 4.64-25.83, 0.03-3.11, 0.01-0.59, 0.07-1.98 and 0.25-1.81 mg/g, respecitively. The results of methodological investigation showed that the components had a good linear relationship (r ≥ 0.999 7), and the average recoveries ranged from 97.80%-101.51%. The results of the similarity of fingerprints showed that the similarity of 10 batches of PMR, BPMR and PMRP were all above 0.99, while the similarity between different types of processed products decreased. HCA can cluster PMR and its two processed products into three categories, PCA results extract three main components, OPLS-DA can effectively distinguish the three kinds of decoction pieces, and six main kinds were screened out according to the principle of VIP greater than 1. Four chemical components with strong correlation with the quality of processed PMR were identified, including emodin methyl ether-8-O-glucoside, emodin-8-O-glucoside, gallic acid and emodin methyl ether. Conclusion In this study, the HPLC fingerprint of PMR and its processed products combined with chemometric method is simple and accurate, which can provide a reference for the quality control and quality evaluation of the characteristic decoction pieces of BPMR.
[中图分类号]
R283.6
[基金项目]
国家自然科学基金资助项目(82060724);江西省重点研发计划(20192BBG70073);江西省卫生健康委员会科技计划项目(202120015);江西省中药学一流学科专项(NO.JXSYLXK-ZHYAO039/141);2022年国家级大学生创新创业训练计划项目(202210412288);企业技术开发项目(2020)