中国药物警戒 ›› 2022, Vol. 19 ›› Issue (12): 1295-1302.
DOI: 10.19803/j.1672-8629.20220458

• 何首乌质量及安全性评价专栏（二） • 上一篇    下一篇

基于UPLC-MS/MS检测技术探讨清蒸时间对何首乌26种化学成分的影响

李妍怡1, 王莹2,△, 张南平2, 杨建波2, 刘越1, 汪祺2,#, 张玉杰1, 魏锋2, 马双成2,*   

  1. 1北京中医药大学中药学院,北京 102400;
    2中国食品药品检定研究院,北京 100050
  • 收稿日期:2022-08-05 出版日期:2022-12-15 发布日期:2022-12-21
  • 通讯作者: *马双成,男,研究员,中药民族药物质基础与质量安全评价。E-mail：msc@nifdc.org.cn; #为共同通信作者。
  • 作者简介:李妍怡,女,在读博士,中药分析。△为并列第一作者。
  • 基金资助:
    国家自然科学基金资助项目(81973476)

Effects of duration of steaming on 26 chemical compositions of Polygoni Multiflori Radix based on UPLC-MS/MS detection technology

LI Yanyi1, WANG Ying2,△, ZHANG Nanping2, YANG Jianbo2, LIU Yue1, WANG Qi2,#, ZHANG Yujie1, WEI Feng2, MA Shuangcheng2,*   

  1. 1School of Chinese Materia medica, Beijing University of Chinese Medicine, Beijing 102400, China;
    2National Institutes for Food and Drug Control, Beijing 100050, China
  • Received:2022-08-05 Online:2022-12-15 Published:2022-12-21

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摘要： 目的 探究《中华人民共和国药典》（2020年版）（简称“《中国药典》”）收载的清蒸炮制法,在不同炮制时间（0~48 h）下对何首乌中主要化学成分含量的影响。方法 制备《中国药典》清蒸样品;建立超高效液相色谱-三重四极杆质谱（UPLC-MS/MS）测定何首乌中26种成分的分析方法并进行检测。结果 建立了准确可靠的UPLC-MS/MS测定何首乌中蒽醌、二苯乙烯苷、黄酮、酚类化合物含量的方法;随着蒸制时间的延长,26种成分的含量发生了明显变化：游离蒽醌类成分（大黄素、大黄素甲醚）先降低后升高,结合蒽醌类成分（大黄素-8-O-β-D-葡萄糖苷、大黄素甲醚-8-O-β-D-葡萄糖苷、大黄素-1-O-葡萄糖苷、大黄素-6-O-葡萄糖苷）、大黄酸、大黄素-1-甲醚、cis-THSG、虎杖苷、表儿茶素和芦丁先升高后降低,大黄素二蒽酮、大黄素-8-O-（6’-甲基丙二酰）吡喃葡萄糖苷、大黄素甲醚-8-O-（6’-甲基丙二酰）吡喃葡萄糖苷、trans-THSG、白藜芦醇、2,3,5,4’-四羟基二苯乙烯-2-O-（2”-O-阿魏酰）-β-D-吡喃葡萄糖苷、儿茶素和决明酮-8-O-β-D-葡萄糖苷降低,酚类成分升高。结论 本方法操作简单、准确度高、重复性好,可以用于何首乌中26种化学成分的定量检测分析。制首乌中26种成分的含量与蒸制时间密切相关,蒽醌类、二苯乙烯苷类、黄酮类、酚类发生规律性变化,对何首乌质量产生重要影响。

关键词: 何首乌, 制首乌, 超高液相色谱-三重四极杆质谱法, 蒽醌类成分, 二苯乙烯苷类成分, 黄酮类成分, 酚类成分

Abstract: Objective To explore the effects of duration of steaming (0~48 h) and processing methods recorded in “Chinese Pharmacopoeia” on the contents of main chemical components of Polygoni Multiflori Radix（PM）. Methods Pharmacopoeia-defined steamed samples were prepared before an ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS) analytical method was established for determination of the 26 components in PM. Results An accurate and reliable UPLC-MS/MS method was established for the determination of anthraquinone, stilbene glycosides, flavonoids and phenolic compounds in PM. With the extension of steaming time, the contents of 26 components changed significantly. The contents of free anthraquinone components (emodin, physcion) decreased before they increased, while those of combined anthraquinone components (emodin-8-O-β-D-glucoside, Physcion- -8-O-β-D-glucoside, emodin-1-O-glucoside, emodin-6-O-glucoside), rhein, hydroxyemodin, emodin-1-methyl, cis-THSG, polydatin, epicatechin and rutin increased first and then decreased. The contents of emodin dianthrone, emodin-8-O-(6’-methylmalonyl)-glucopyranoside, physcion-8-O-(6’- methylmalonyl)-glucopyranoside, trans-THSG, resveratrol, 2,3,5,4’-tetrahydroxystilbene-2-0-(2”-O-feruloyl)-β-D-glucopyranoside, catechin and torachrysone-8-O-β-D-glucopyranoside decreased, while those of phenolic components increased. Conclusion This method is simple, accurate and repeatable, which can be used for quantitative detection and analysis of 26 chemical components in PM. The contents of the 26 components in PM are closely related to the duration of steaming. Anthraquinones, stilbene glycosides, flavonoids and phenols undergo regular changes, which have an impact on the quality of PM.

Key words: Polygoni Multiflori Radix, Polygonum Multiflorum Radix preparata, UPLC-MS/MS, anthraquinones, stilbene glycosides, flavonoids, phenols

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