基于指纹图谱联合化学计量学评价不同产地百蕊草质量的研究<sup>*</sup>

严露, 蒲婧哲, 杨勇, 解松子, 王多梅, 李明天, 张亚中

doi:10.16155/j.0254-1793.2023.01.17

药物分析杂志 >

2023 , Vol. 43 >Issue 1: 141 - 152

DOI: https://doi.org/10.16155/j.0254-1793.2023.01.17

质量分析

基于指纹图谱联合化学计量学评价不同产地百蕊草质量的研究^*

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1.安徽中医药大学药学院,合肥 230012;
2.安徽省食品药品检验研究院,合肥 230051;
3.国家药品监督管理局中药质量研究与评价重点实验室,合肥 230051;
4.贵州中医药大学药学院,贵阳 550025

第一作者 Tel:15185066200;E-mail:791637318@qq.com

**Tel:(0551)63358119;E-mail:282483507@qq.com

收稿日期: 2022-03-14

网络出版日期: 2024-06-24

基金资助

*国家重点研发计划“中医药现代化研究”重点专项(2019YFC1711505)

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Study on quality evaluation of Thesii Herba from different producing areas based on fingerprint and chemometrics^*

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1. School of Pharmacy, Anhui University of Traditional Chinese Medicine, Hefei 230012, China;
2. Anhui Institute of Food and Drug Control, Hefei 230051, China;
3. NMPA Key Laboratory for Quality Research and Evaluation of Traditional Chinese Medicine, Hefei 230051, China;
4. School of Pharmacy, Guizhou University of Traditional Chinese Medicine, Guiyang 550025, China

Received date: 2022-03-14

Online published: 2024-06-24

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摘要

目的: 建立不同产地百蕊草的超高效液相色谱(UPLC)指纹图谱,结合化学计量学分析方法对不同产地百蕊草的质量进行有效的评价和分析。方法: 采用Waters Acquity UPLC BEH Shield RP18色谱柱(150 mm×2.1 mm,1.7 μm),流动相为乙腈-0.2%甲酸水溶液,梯度洗脱,流速0.4 mL·min^-1,检测波长330 nm,柱温30 ℃;对不同产地的百蕊草样品进行分析并建立指纹图谱;运用超高效液相色谱-四极杆飞行时间质谱联用(UPLC-Q TOF MS)技术对其化学成分进行鉴定,同时联合层次聚类(HCA)、正交偏最小二乘判别(OPLS-DA)分析方法筛选出造成不同产地质量差异的指标成分,以共有峰面积为指标构建灰色关联度模型对样品进行质量评价。结果: 30批百蕊草指纹图谱中有8个共有峰,与对照指纹图谱的相似度均在0.99以上,不同产地的百蕊草药材整体质量相对稳定。HCA与OPLS-DA结果显示各产地样品的部分化学成分差异明显,并筛选出对分组贡献值较大的2个差异性成分,分别为百蕊草素Ⅰ(峰6)和山柰酚-3-O-(2”-O-α-鼠李糖基-6”-O-丙二酰基)-β-葡萄糖苷(峰8),灰色关联度分析显示各省百蕊草质量优劣排序为甘肃、河南、陕西、山西。结论: 指纹图谱联合HCA、OPLS-DA、灰色关联度等化学计量学对百蕊草进行质量评价与分析,并对其共有峰进行鉴定的方法稳定、可靠,可全面评定不同产地百蕊草样品的质量情况,为百蕊草综合质量控制与评价、人工栽培引种等研究提供有效手段。

关键词： 百蕊草; 指纹图谱; 化学计量学; 灰色关联度法; 质量控制与评价; 超高效液相色谱; 超高效液相色谱-四极杆飞行时间质谱联用

本文引用格式

严露, 蒲婧哲, 杨勇, 解松子, 王多梅, 李明天, 张亚中 . 基于指纹图谱联合化学计量学评价不同产地百蕊草质量的研究^*[J]. 药物分析杂志, 2023 , 43(1) : 141 -152 . DOI: 10.16155/j.0254-1793.2023.01.17

Abstract

Objective: To establish ultrahigh performance liquid chromatography (UPLC) fingerprints of Thesii Herba from different places of origin, we combined chemometrics analysis methods to effectively evaluate and analyze the quality of Thesii Herba from different places of origin. Methods: Analysis was performed on a Waters Acquity UPLC BEH Shield RP18(150 mm×2.1 mm, 1.7 μm) column with acetonitrile-0.2% formic acid for gradient elution. The flow rate was 0.4 mL·min^-1,the detection wavelength was 330 nm,and the column temperature was 30 ℃. The samples of Thesii Herba from different habitats were analyzed and fingerprints were established. The chemical components were identified by ultra high performance liquid chromatography-quadrupole time of flight mass spectrometer (UPLC-Q TOF MS). At the same time, the index components causing the quality differences in different habitats were screened by combining hierarchical clustering analysis (HCA) and orthogonal partial least squares discriminant analysis (OPLS-DA). Finally, the grey correlation model was constructed with the common peak area as the index to evaluate the quality of the samples. Results: There were 8 common peaks in the fingerprints of 30 batches of Thesii Herba and the similarity with the control fingerprints was more than 0.99. The overall quality of Thesii Herba from different habitats was relatively stable. The results of HCA and OPLS-DA showed that there were significant differences in some chemical components of samples from different places, and two different components with large contribution value to the grouping were screened, which were thymosin Ⅰ(peak 6) and kaempferol-3-O-(2”-O-α-rhamnosyl-6”-O-malonyl)-β-glucoside (peak 8). The grey correlation analysis showed that the quality order of each province was Gansu, Henan, Shaanxi, Shanxi. Conclusion: The method of fingerprint combined with HCA, OPLS-DA, grey correlation degree and other chemometrics to evaluate and analyze the quality of Thesii Herba, and to identify its common peaks is stable and reliable. It can comprehensively evaluate the quality of Thesii Herba samples from different areas, and provide an effective means for the comprehensive quality control and evaluation of Thesii Herba artificial cultivation and introduction.

Key words： Thesii Herba; fingerprint; stoichiometry; grey correlation degree method; quality control and evaluation; UPLC; UPLC-Q TOF MS

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