摘要
特征成分化学属性是中药大品种制造质量控制的内容之一。该研究以中药大品种黄精赞育胶囊为研究载体,采用高效液相色谱方法,建立同时测定淫羊藿苷、大黄素、五味子甲素、二苯乙烯苷和蛇床子素5种特征成分化学属性的定量分析方法。5种特征成分化学属性的分析方法线性关系良好(r>0.999 9),日内、日间精密度相对标准偏差(relative standard deviation, RSD)为0.11%~2.0%和0.25%~2.8%,重复性RSD为1.8%~2.6%,48 h内稳定性RSD为0.19%~2.8%,加样回收率为95.52%~100.1%,表明该方法符合药物定量分析要求。进一步,采用区间估计法,直观反映特征成分化学属性含量异常的样品分布,其中10个样品超出置信水平95%控制线;同时采用多变量统计过程控制(multivariate statistical process control, MSPC)方法的Hotelling′s T^(2)和平方预测误差(squared prediction error, SPE)控制图,整体监测黄精赞育胶囊异常样本,2个样品超出Hotelling′s T^(2) 95%控制线,3个样品超出SPE 95%控制线,实现了特征成分化学属性的黄精赞育胶囊质量一致性控制。该文所建立的黄精赞育胶囊特征成分化学属性的质量控制方法,可靠有效,弥补了黄精赞育胶囊单一成分测定的质控不足,为黄精赞育胶囊制造过程质量控制提供科学依据,也为中药大品种制造的质量控制提供参考。
The chemical properties of characteristic components are significant to the manufacturing quality control of big brand traditional Chinese medicine. In this study, the Huangjing Zanyu Capsules were used as the research carrier to determine the content of five characteristic components including icraiin, emodin, schisandrin A, 2,3,5,4′-tetrahydroxystilbene-2-O-β-D-glucoside, and osthole simultaneously by high-performance liquid chromatography(HPLC). The results showed that the chemical properties of five cha-racteristic components had a good linear relationship(r>0.999 9) within the quantitative range;the relative standard deviations(RSD) was 0.11%-2.0% and 0.25%-2.8% respectively for intra-day and inter-day precision;the RSD of repeatability was 1.8%-2.6%;the RSD of stability within 48 hours was 0.19%-2.8%, and the average recovery rate was 95.52%-100.1%, all meeting the requirements of pharmaceutical quantitative analysis. Additionally, the interval estimation method was used to directly reflect the distribution of samples with abnormal chemical properties of characteristic components, and the results showed ten samples were detected beyound the 95% control line of confidence level. Multivariate statistical process control(MSPC) method was used to monitor the abnormal samples of Huangjing Zanyu Capsules collectively, and the results showed that two samples were beyond the 95% control line of Hotelling′s T^(2) and three samples beyond the 95% control line of squared prediction error(SPE), indicating consistent quality control of Huangjing Zanyu Capsules. In conclusion, the proposed method is not only accurate and efficient but also a compensation for the traditional single-component quality control method, providing a scientific basis for the quality control in manufacturing process of Huangjing Zanyu Capsules. Furthermore, it could also serve as a reference method for the quality control in manufacturing big brand traditional Chinese medicine.
作者
朱金媛
曾敬其
李倩倩
马丽娟
陆影
张瀚
郑燕飞
吴春媛
吴志生
ZHU Jin-yuan;ZENG Jing-qi;LI Qian-qian;MA Li-juan;LU Ying;ZHANG Han;ZHENG Yan-fei;WU Chun-yuan;WU Zhi-sheng(School of Chinese Materia Medica,Beijing University of Chinese Medicine,Beijing 102488,China;Engineering Research Center of Chinese Medicine Production and New Drug Development,Ministry of Education,Beijing 102488,China;School of Traditional Chinese Medicine,Beijing University of Chinese Medicine,Beijing 100029,China;Shanghai New Asiatic Pharmaceuticals Hanjiang Co.,Ltd.,Yangzhou 225100,China)
出处
《中国中药杂志》
CAS
CSCD
北大核心
2021年第7期1629-1635,共7页
China Journal of Chinese Materia Medica
基金
国家自然科学基金优秀青年基金项目(82022073)
国家自然科学基金项目(81773914)
国家“重大新药创制”科技重大专项(2018ZX09201011)
北京市自然科学基金项目(7202115)
江苏省产学研项目(2019110031004422)
国家自然科学青年基金项目(82003959)
国家博士后基金项目(2020M670240)。
关键词
中药大品种
关键质量属性
黄精赞育胶囊
特征成分化学属性
多变量统计过程控制
区间估计法
big brand traditional Chinese medicine
critical quality attribute
Huangjing Zanyu Capsules
chemical properties of characteristic components
multivariate statistical process control
interval estimation method