芪桂苓合剂质量控制方法研究
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篇名: 芪桂苓合剂质量控制方法研究
TITLE: Study on quality control method of Qiguiling mixture
摘要: 目的 建立芪桂苓合剂的指纹图谱和毛蕊异黄酮葡萄糖苷等4种活性成分含量的测定方法,以控制芪桂苓合剂的质量。方法采用高效液相色谱(HPLC)法建立12批芪桂苓合剂的指纹图谱;采用SPSS25.0软件进行聚类分析、主成分分析,采用SIMCA14.1软件进行正交偏最小二乘法-判别分析,并以变量重要性投影(VIP)值大于1.0为标准,筛选差异性成分。以橙皮苷为内参物,采用一测多评法计算毛蕊异黄酮葡萄糖苷、甘草苷、甘草酸含量,并与外标法的测定结果进行比较。结果12批样品指纹图谱中共确认了17个共有峰,相似度均大于0.940;共指认出4个共有峰,分别为毛蕊异黄酮葡萄糖苷(6号峰)、甘草苷(8号峰)、橙皮苷(12号峰)和甘草酸(17号峰)。12批样品可聚类分为2类,其中S4、S7~S9、S11~S12聚为一类,其他聚为一类;6个主成分的累计方差贡献率为85.840%;15、14、4、8(甘草苷)、9号峰的VIP值均大于1.0。毛蕊异黄酮葡萄糖苷、甘草苷、甘草酸含量的一测多评法结果与外标法所得结果的相对误差均小于5%(n=3)。结论本研究建立的HPLC指纹图谱和含量测定方法,可用于芪桂苓合剂的质量控制;甘草苷等5种成分是其差异性成分。
ABSTRACT: OBJECTIVE To establish the fingerprint of Qiguiling mixture and the method for the content determination of 4 kinds of active components such as calycosin-7-glucoside, so as to control the quality of Qiguiling mixture. METHODS The fingerprints of 12 batches of Qiguiling mixture were established by HPLC. SPSS 25.0 software was used for cluster analysis and principal component analysis, and SIMCA 14.1 software was used for orthogonal partial least squares-discriminant analysis. The variable importance in projection (VIP) value greater than 1.0 was used as the index to screen the differential components. The contents of calycosin-7-glucoside, glycyrrhizin and glycyrrhizic acid were calculated by the quantitative analysis of multi- components by single marker (QAMS) with hesperidin as the internal reference, and the results were compared with external standard method. RESULTS In the fingerprints of 12 batches of samples, 17 common peaks were identified, and the similarities were more than 0.940. A total of 4 common peaks were identified, which were calycosin-7-glucoside (peak 6), glycyrrhizin (peak 8), hesperidin (peak 12), and glycyrrhizic acid (peak 17). The 12 batches of samples could be clustered into two categories, S4, S7-S9 and S11-S12 were clustered into one category, and the other batches of samples were clustered into one category. The cumulative variance contribution rate of the six principal components was 85.840%, and VIP values of peaks 15, 14, 4, 8 (glycyrrhizin) and 9 were all greater than 1.0. The relative error between the results of QAMS and external standard method was less than 5% (n=3) for the contents of calycosin-7-glucoside, glycyrrhizin and glycyrrhizic acid. CONCLUSIONS Established HPLC fingerprint and content determination method in this study can be used for quality control of Qigiling mixture. Five components such as glycyrrhizin are the differential components.
期刊: 2023年第34卷第10期
作者: 于晓涛;王博;王佳;陈可嘉;王瑞
AUTHORS: YU Xiaotao,WANG Bo,WANG Jia,CHEN Kejia,WANG Rui
关键字: 芪桂苓合剂;指纹图谱;高效液相色谱法;一测多评法;含量测定;质量控制
KEYWORDS: Qiguiling mixture; fingerprint; HPLC; quantitative analysis of multi-components by single marker; content
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