[关键词]
[摘要]
目的 建立青风藤的液相色谱指纹图谱与含量测定方法,更全面、合理地控制青风藤药材的质量。方法 建立青风藤药材的液相色谱指纹图谱方法,对74批青风藤药材进行分析,使用《中药色谱指纹图谱相似度评价系统(2012版)》对74批青风藤药材进行相似度评价,确定共有峰,使用SIMCA-P(V 14.1)软件对74批青风藤药材的指纹图谱数据进行正交偏最小二乘判别分析(orthogonal partial least squares discriminant analysis,OPLS-DA),从活性物质中选择对青风藤产地及部位影响较大的共有成分作为青风藤的质量控制成分,对其进行含量测定,并分析测定结果。结果 方法学验证结果表明,所建方法适用于青风藤药材指纹图谱和含量测定;经化学计量学分析与文献调研,最终选择木兰花碱和青藤碱作为青风藤的质量控制成分含量测定。结果表明,不同药用部位的青风藤中青藤碱含量差异较大,而不同产地的青风藤中木兰花碱含量差异较大,青风藤根茎与根中的青藤碱含量较藤茎中青藤碱含量高,湖北产青风藤中木兰花碱较其他产地高。结论 所建立的青风藤指纹图谱和含量测定方法色谱峰分离度、拖尾因子、准确度、线性、精密度、稳定性、重现性等参数均符合《中国药典》2020年版要求,可对青风藤进行准确的定性和定量分析,适用于青风藤药材的质量控制。
[Key word]
[Abstract]
Objective To establish the HPLC fingerprints and content determination methods to control the quality of Qingfengteng (Sinomenii Caulis) more comprehensively and reasonably. Methods The HPLC fingerprints method of Sinomenii Caulis was established, and 74 batches of Sinomenii Caulis were analyzed. The similarities of 74 batches of Sinomenii Caulis were evaluated using the similarity evaluation software of traditional Chinese medicine chromatographic fingerprint (2012 Edition), and the common peaks were determined. SIMCA-P (V 14.1) was used to reduce the dimension of HPLC fingerprints of 74 batches of Sinomenii Caulis, and the orthogonal partial least squares discriminant analysis (OPLS-DA) was carried out. From the active substances, the common components which have a great influence on the origins and medicinal parts of Sinomenii Caulis were selected as the quality control components of Sinomenii Caulis, and their content was determined and the determination results were analyzed. Results The results of methodological verification showed that the method was suitable for fingerprint and content determination of Sinomenii Caulis. After chemometrics analysis and literature research, magnoflorine and sinomenine were selected as the quality markers of Sinomenii Caulis, and the contents of sinomenine and magnoflorine in 74 batches of Sinomenii Caulis were determined. The results showed that the medicinal parts had a great influence on the content of sinomenine, and the origins had a great influence on the content of magnoflorine in Sinomenii Caulis. The content of sinomenine in the rhizome and root of Sinomenii Caulis was higher than in the stem, and the content of magnoflorine in the samples from Hubei Province were higher than other origins. Conclusion The chromatographic peak resolution, tailing factor, accuracy, linearity, precision, stability, reproducibility and other parameters of the established HPLC fingerprints and content determination methods meet the requirements of Chinese Pharmacopoeia (2020 edition), which can be used for accurate qualitative and quantitative analysis of Sinomenii Caulis, and are suitable for the quality control of Sinomenii Caulis.
[中图分类号]
R286.2
[基金项目]
天津市科技计划项目(20ZYJDJC00090);国家重点研发计划资助项目(2018YFC1707904,2018YFC1707000);正清风痛宁(青风藤)全产业链关键技术研究项目(2020SK1020)