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基于多元统计方法的栀子炮制前后抗氧化谱效关系研究*

  • 惠博平 ,
  • 肖菁 ,
  • 唐婷 ,
  • 冯传平 ,
  • 黄建华 ,
  • 李俊强
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  • 1.湖南中医药高等专科学校,株洲 412012;
    2.湖南中医药大学,长沙 410208;
    3.湖南省中医药研究院,长沙 410006;
    4.湖南省药品检验检测研究院,长沙 410001;
    5.山东省烟台市食品药品检验检测中心,烟台 264000
第一作者 Tel:19307485420;E-mail:huiboping0904@163.com
** Tel:18660021183;E-mail:ytljq@qq.com

收稿日期: 2024-07-31

  网络出版日期: 2025-08-25

基金资助

*国家自然科学基金面上项目(82474502); 湖南省高新技术产业科技创新引领计划(2022GK4015); 湖南省中医药管理局十四五第二批学科带头人(中药药剂学)项目(No.:11); 湖南中医药大学研究生创新课题(2023CX57)

Spectrum-effect relationship on antioxidant activity of Gardeniae Fructus before and after processing based on multivariate statistical analysis*

  • HUI Bo-ping ,
  • XIAO Jing ,
  • TANG Ting ,
  • FENG Chuan-ping ,
  • HUANG Jian-hua ,
  • LI Jun-qiang
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  • 1. Hunan Traditional Chinese Medical College, Zhuzhou 412012, China;
    2. Hunan University of Chinese Medicine, Changsha 410208, China;
    3. Hunan Academy of Traditional Chinese Medicine, Changsha 410006, China;
    4. Hunan Institute for Drug Control, Changsha 410001, China;
    5. Yantai Center for Food and Drug Control, Yantai 264000, China

Received date: 2024-07-31

  Online published: 2025-08-25

摘要

目的: 建立栀子炮制前后的HPLC指纹图谱,并研究其与抗氧化活性间的谱效关系。方法: 使用Agilent 1200高效液相色谱仪,采用Agilent ZORBAX SB-C18(250 mm×4.6 mm,5 μm)色谱柱,以0.1%甲酸水-甲醇溶液为流动相,紫外检测波长254 nm,柱温25 ℃,供试品溶液提取溶剂为70%甲醇溶液,进样量5 μL,流速1 mL · min-1,建立6个批次栀子炮制前后的指纹图谱,采用DPPH法评价栀子炮制前后的抗氧化活性,并结合灰色关联分析和偏最小二乘回归分析研究谱效关系。结果: 确定了指纹图谱中23个共有峰,通过对照品比对指认其中5个色谱峰,分别为京尼平苷酸(峰3)、京尼平龙胆双糖苷(峰9)、栀子苷(峰11)、西红花苷-Ⅰ(峰21)和西红花苷-Ⅱ(峰22)。5种栀子炮制前后样品(生栀子、炒栀子、酒栀子、栀子炭和姜栀子)对DPPH自由基的半数抑制浓度(IC50)均值分别为0.25、28.61、6.34、11.79和0.68 mg · mL-1。结合3种统计学方法,峰3、9、11、21和22是与清除DPPH自由基关联较大的共有峰。结论: 6个批次栀子炮制前后抗氧化活性是多个组分共同作用的结果,峰3、9、11、21和22是与抗氧化密切相关的成分。本研究结果为栀子炮制前后抗氧化物质基础研究与临床应用提供了参考依据。

本文引用格式

惠博平 , 肖菁 , 唐婷 , 冯传平 , 黄建华 , 李俊强 . 基于多元统计方法的栀子炮制前后抗氧化谱效关系研究*[J]. 药物分析杂志, 2025 , 45(3) : 426 -439 . DOI: 10.16155/j.0254-1793.2024-0496

Abstract

Objective: To establish the HPLC fingerprint of Gardeniae Fructus before and after processing, and to study the relationship between the fingerprint and antioxidant activity. Methods: Agilent 1200 high-performance liquid chromatograph was used, and the column was Agilent ZORBAX SB-C18 (250 mm×4.6 mm, 5 μm). The mobile phase system was 0.1% formic acid water-methanol solution. The ultraviolet detection wavelength was 254 nm. The column temperature was 25 ℃. The extraction solvent of the test solution was 70% methanol solution. The injection volume was 5 μL. The flow rate was 1 mL · min-1, and the fingerprints of six batches of gardenia before and after processing were established, and the antioxidant activity of gardenia before and after processing was evaluated by DPPH method, and the spectral effect relationship was studied by grey correlation analysis and partial least squares regression analysis. Results: 23 common peaks were identified in the fingerprint, and five chromatographic peaks were identified by comparison of reference substances, including geniposidic acid (peak 3), genipin gentiobiside (peak 9), gardenside (peak 11), crocetin I (peak 21), and crocetin Ⅱ (peak 22). The mean half inhibitory concentration (IC50) of DPPH radical in 5 different processed products (raw gardenia, fried gardenia, wine gardenia, gardenia charcoal and ginger gardenia) were 0.25 mg · mL-1, 28.61 mg · mL-1, 6.34 mg · mL-1, 11.79 mg · mL-1, and 0.68 mg · mL-1, respectively. Combined with the three statistical methods, peaks 3, 9, 11, 21, and 22 were the common peaks associated with DPPH radical scavenging. Conclusion: The antioxidant activity of 6 batches of Gardeniae Fructus before and after processing is the result of the interaction of multiple components, and peaks 3, 9, 11, 21, and 22 are closely related to antioxidant activity. The results of this study provide a reference for the basic research and clinical application of antioxidant substances in Gardeniae Fructus before and after processing.

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