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壮药金母颗粒的指纹图谱建立、化学计量学分析及多组分含量测定
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| 篇名： | 壮药金母颗粒的指纹图谱建立、化学计量学分析及多组分含量测定 |
| TITLE： | Establishment of fingerprint ，chemometric analysis and multi-component content determination of Zhuang medi- cine Jinmu granules |
| 摘要： | 目的 建立壮药金母颗粒的指纹图谱并进行化学计量学分析，并测定其中3种成分的含量。方法采用高效液相色谱（HPLC）法，以芦丁为参照，采用《中药色谱指纹图谱相似度评价系统（2012版）》绘制10批金母颗粒的HPLC指纹图谱并进行相似度评价；通过与混合对照品进行比对，确定共有峰；采用SPSS21.0软件进行聚类分析，采用SIMCA14.1软件进行主成分分析、正交偏最小二乘-判别分析，以变量重要性投影（VIP）值＞1为标准筛选影响金母颗粒质量的标志成分；采用HPLC法测定金母颗粒中落新妇苷、虎杖苷和盐酸小檗碱的含量。结果10批金母颗粒共有22个共有峰，相似度为0.962～0.997；共指认出5个共有峰，分别为没食子酸（2号峰）、虎杖苷（9号峰）、芦丁（11号峰）、落新妇苷（13号峰）、山柰酚（20号峰）。聚类分析结果显示，10批金母颗粒可聚为3类，S1、S3～S4聚为一类，S5～S6、S9聚为一类，S2、S7～S8、S10聚为一类；主成分分析结果显示，模型解释参数为0.951，预测能力参数为0.723，分类结果与聚类分析结果基本一致。正交偏最小二乘-判别分析的分类结果也与聚类分析结果基本一致，VIP值＞1的共有峰依次为7号峰、11号峰（芦丁）、17号峰、13号峰（落新妇苷）、3号峰、8号峰、6号峰、16号峰。落新妇苷、虎杖苷、盐酸小檗碱检测质量浓度的线性范围分别为0.0126～1.2250、0.0108～1.0525、0.0200～1.5625mg/mL（R2均为0.9999），精密度、稳定性（24h）、重复性试验的RSD均小于3％，平均加样回收率分别为99.48％（RSD＝2.67％，n＝9）、98.57％（RSD＝1.77％，n＝9）、100.84％（RSD＝2.49％，n＝9），含量分别为1.2210～7.0116、2.2511～4.4629、1.2524～3.3287mg/g。结论所建指纹图谱和含量测定方法准确、稳定、简便，结合化学计量学分析，可用于壮药金母颗粒的质量控制和评价。 |
| ABSTRACT： | OBJECTIVE To establish the fingerprint of Zhuang medicine Jinmu granules and carry out chemometric analysis ， and determine the contents of three components . METHODS High performance liquid chromatography （HPLC） method was adopted. Using rutin as the reference ，HPLC fingerprints of 10 batches of Jinmu granules were drawn and similarity evaluation was performed by Similarity Evaluation of Chromatographic Fingerprint of Traditional Chinese Medicine （2012 edition）；the common peak was determined by comparing with mixed control ；SPSS 21.0 software was used for cluster analysis ，and SIMCA 14.1 software was used for principal component analysis and orthogonal partial least squares-discriminant analysis. The differential components affecting the quality of Jinmu granules were screened by taking the variable importance in projection （VIP）value ＞1 as the standard ；the HPLC method was used to determine the contents of astilbin ，polydatin and berberine hydrochloride in Jinmu granules. RESULTS There were 22 common peaks in 10 batches of Jinmu granules ，and the similarities were 0.962-0.997；five common peaks were identified ，namely gallic acid （peak 2），polydatin（peak 9），rutin（peak 11），astilbin（peak 13）and kaempferol （peak 20）. The results of cluster analysis showed that 10 batches of Jinmu granules could be clustered into 3 categories：S1 and S 3-S4 were grouped into one category ；S5-S6 and S 9 were grouped into one category ；S2，S7-S8 and S 10 were grouped into one category. The results of principal component analysis showed that the parameter of model interpretation was 0.951 and that of prediction ability was 0.723. The classification results were basically consistent with cluster analysis. The classifica tion results of orthogonal partial least squares- com discriminant analysis were also ba sically consistent with clus- ter analysis. The common peaks with VIP value ＞1 in the order were peak 7＞peak 11（rutin）＞peak 17＞peak 13（astilbin）＞ peak 3＞peak 8＞peak 6＞peak 16 respectively. The linear ranges of astilbin ，polydatin and berberine hydrochloride were 0.012 6- 1.225 0，0.010 8-1.052 5 and 0.020 0-1.562 5 mg/mL，respectively（all R 2＝0.999 9）. RSDs of precision ，stability（24 h）and repeatability tests were all less than 3％. The average recoveries were 99.48％（RSD＝2.67％，n＝9），98.57％（RSD＝1.77％，n＝ 9）and 100.84％（RSD＝2.49％，n＝9）. The contents were 1.221 0-7.011 6，2.251 1-4.462 9，1.252 4-3.328 7 mg/g，respectively. CONCLUSIONS Established fingerprint and the method of content determination are accurate ，stable and simple. Combined with chemometric analysis ，it can be used for the quality control and evaluation of Zhuang medicine Jinmu granules. |
| 期刊： | 2022年第33卷第04期 |
| 作者： | 李林杰，谢谭芳，王昱涵，王志萍，黎芳，王孝勋，冯桥 |
| AUTHORS： | LI Linjie，XIE Tanfang ，WANG Yuhan ，WANG Zhiping ，LI Fang，WANG Xiaoxun ，FENG Qiao |
| 关键字： | 壮药；金母颗粒；高效液相色谱法；指纹图谱；聚类分析；主成分分析；正交偏最小二乘法-判别分析；含量测定 |
| KEYWORDS： | Zhuang medicine ；Jinmu granules ；high performance liquid chromatography ；fingerprint；cluster analysis ； |
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