中国药物警戒 ›› 2022, Vol. 19 ›› Issue (5): 522-526.
DOI: 10.19803/j.1672-8629.2022.05.10

• 基础与临床研究 • 上一篇    下一篇

HPLC测定不同产区生何首乌和不同炮制工艺制何首乌中蒽醌类成分含量

高慧宇1, 杨建波1,△, 孙华2, 宋云飞1, 程显隆1, 王雪婷1, 魏锋1,#, 汪祺1, 王莹1, 靳洪涛2, 马双成1,*   

  1. 1中国食品药品检定研究院,北京 100050;
    2中国医学科学院药物研究所,北京 100050
  • 收稿日期:2021-04-19 出版日期:2022-05-15 发布日期:2022-05-18
  • 通讯作者: *马双成,男,研究员,中药民族药质量标准及安全性评价。E-mail：masc@nifdc.org.cn;#为共同通信作者。
  • 作者简介:高慧宇,女,在读硕士,药物分析学。△为并列第一作者。
  • 基金资助:
    国家自然科学基金资助项目（81773874 、81973476）

Determination of anthraquinones in Polygoni Multiflori Radix from different origins and processed differently by HPLC

GAO Huiyu1, YANG Jianbo1,△, SUN Hua2, SONG Yunfei1, CHENG Xianlong1, WANG Xueting1, WEI Feng11,#, WANG Qi1, WANG Ying1, JIN Hongtao2, MA Shuangcheng1,*   

  1. 1National Institutes for Food and Drug Control, Beijing 100050, China;
    2Institute of Materia Medica, Chinese Academy of Medical Science, Beijing 100050, China
  • Received:2021-04-19 Online:2022-05-15 Published:2022-05-18

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摘要： 目的 采用高效液相色谱法（HPLC）同时测定不同产地何首乌和不同炮制工艺制何首乌中大黄素8-O-β-D-葡萄糖苷、大黄素、大黄素甲醚、游离蒽醌和结合蒽醌的含量。 方法 采用Agilent 5 TC-C18（2）色谱柱（250 mm×4.6 mm, 5 μm）,以甲醇-0.1%甲酸水为流动相梯度洗脱,流速1.0 mL·min-1,检测波长254 nm,测定大黄素8-O-β-D-葡萄糖苷、大黄素和大黄素甲醚的含量;按照《中华人民共和国药典》（2020年版）中何首乌项下方法,测定游离蒽醌和结合蒽醌的含量。 结果 大黄素8-O-β-D-葡萄糖苷、大黄素和大黄素甲醚分别在0.674 5~21.584 5、0.426 7~13.655 0和0.200 3~6.968 5 μg·mL-1范围内具有良好线性关系（R2≥0.999 1）,平均回收率分别为98.42%、100.08%和96.60%。不同产区何首乌大黄素8-O-β-D-葡萄糖苷、大黄素、大黄素甲醚含量范围分别为0.13~2.62、0.08~0.13和0.05~0.72 mg·g-1;游离蒽醌和结合蒽醌含量范围分别为0.1~1.7和1.0~8.7 mg·g-1。 结论 本方法操作简单、准确度高、重复性好,可以用于何首乌中蒽醌类成分含量测定。

关键词: 何首乌, 高效液相色谱法, 蒽醌类成分, 含量测定, 产地, 炮制工艺

Abstract: Objective To simultaneously determine the contents of emodin-8-O-β-D glucoside, emodin, physcion, free anthraquinone and bound anthraquinone in Polygoni Multiflori Radix from different origins and processed with different methods. Methods The contents of emodin-8-O-β-D glucoside, emodin and physcion were determined on an Agilent 5 TC-C18 (2) (250 mm×4.6 mm, 5 μm) column with a mobile phase composed of methanol and 0.1% formic acid solution with gradient elution at 1.0 mL?min-1. The detection wavelength was 254 nm, the column temperature 30℃, and the injection volume was 10 μL. The contents of free anthraquinone and bound anthraquinone were determined using the method for Polygonum multiflorum specified in Chinese Pharmacopoeia (2020 Edition). Results Emodin-8-O-β-D glucoside, emodin, physcion had good linear relationships in the ranges of 0.674 5~21.584 5, 0.426 7~13.655 0 and 0.200 3- 6.968 5 μg?mL-1, respectively (R2≥0.9991). The recovery was 98.42%, 100.08% and 96.60% respectively. The contents of emodin-8-O-β-D glucoside, emodin, physcion, free anthraquinone and bound anthraquinone in Polygoni Multiflori Radix from different origins were 0.13~2.62, 0.08~0.13, 0.05~0.72, 0.1~1.7 and 1.0~8.7 mg?g-1, respectively. Conclusion This method is simple, accurate and reproducible, which can be used for the determination of anthraquinones in Polygonum multiflorum.

Key words: Polygoni Multiflori Radix, high performance liquid chromatography, anthraquinones; content determination, Origin; processe

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