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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 Δ
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李林杰 1,2* ,谢谭芳 ,王昱涵 ,王志萍 1,2 # ,黎 芳 ,王孝勋 ,冯 桥(1.广西中医药大学药学院,南宁
530200;2.广西高校中药制剂共性技术研发重点实验室,南宁 530200;3.广西国际壮医医院皮肤科,南宁
530200)
中图分类号 R284.1 文献标志码 A 文章编号 1001-0408(2022)04-0439-08
DOI 10.6039/j.issn.1001-0408.2022.04.10
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SPSS 21.0软件进行聚类分析,采用SIMCA 14.1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
2
杖苷、盐酸小檗碱检测质量浓度的线性范围分别为0.012 6~1.225 0、0.010 8~1.052 5、0.020 0~1.562 5 mg/mL(R 均为0.999 9),精
密度、稳定性(24 h)、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 1.221 0~7.011 6、2.251 1~4.462 9、1.252 4~3.328 7 mg/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。
关键词 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
Establishment of fingerprint,chemometric analysis and multi-component content determination of Zhuang
medicine Jinmu granules
LI Linjie 1 ,2 ,XIE Tanfang 1 ,2 ,WANG Yuhan 1 ,2 ,WANG Zhiping 1 ,2 ,LI Fang 1 ,2 ,WANG Xiaoxun ,FENG Qiao 3
1
(1. School of Pharmacy,Guangxi University of Chinese Medicine,Nanning 530200,China;2. Key Laboratory
of Generic Technology Research and Development of Traditional Chinese Medicine Preparations in Colleges and
Universities in Guangxi,Nanning 530200,China;3. Dept. of Dermatology,Guangxi International Zhuang
Medicine Hospital,Nanning 530200,China)
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 S3-S4 were grouped into one category;S5-S6 and S9 were grouped into one category;S2,S7-S8 and S10 were
grouped into one category. The results of principal component
Δ 基金项目:广西重点研发计划项目(No.2017AA10114)
analysis showed that the parameter of model interpretation was
*硕士研究生。研究方向:中药、民族药新制剂与新剂型的研
0.951 and that of prediction ability was 0.723. The classi-
发。电话:0771-4953513。E-mail:504629836@qq.com
# 通信作者:教授,硕士生导师,硕士。研究方向:中药、民族药新 fication results were basically consistent with cluster analysis.
制剂与新剂型的研发。电话:0771-4953513。E-mail:318007460@qq. The classification results of orthogonal partial least squares-
com discriminant analysis were also basically consistent with clus-
中国药房 2022年第33卷第4期 China Pharmacy 2022 Vol. 33 No. 4 ·439 ·