湖北农业科学 ›› 2023, Vol. 62 ›› Issue (10): 166-171.doi: 10.14088/j.cnki.issn0439-8114.2023.10.029

• 检测分析 • 上一篇    下一篇

HPLC测定青钱柳叶片中槲皮素、山奈酚的含量

李俊秀a, 廖夏云a,b, 赵立春a,b, 梁洁a,b   

  1. a.广西中医药大学,药学院,南宁 530200;
    b.广西中医药大学,广西壮瑶药工程技术研究中心,南宁 530200
  • 收稿日期:2021-12-13 发布日期:2023-11-14
  • 通讯作者: 赵立春(1980-),男,吉林长春人,研究员,博士,主要从事中药化学成分及活性研究,(电话)13481025799(电子信箱)hyzlc@126.com。
  • 作者简介:李俊秀(1994-),女,广西桂平人,硕士,主要从事中药化学成分及活性研究,(电子信箱)gxzyljx@126.com。
  • 基金资助:
    国家自然科学基金项目(81860691); 国家青年岐黄学者项目; 广西一流学科项目(2019XK104)

HPLC determination of quercetin and kaempferol in Qingqianliu leaves

LI Jun-xiua, LIAO Xia-yuna,b, ZHAO Li-chuna,b, LIANG Jiea,b   

  1. a. College of Pharmacy, Guangxi University of Chinese Medicine,Nanning 530200,China;
    b. Guangxi Zhuang Yao Medicine Engineering Technology Research Center, Guangxi University of Chinese Medicine,Nanning 530200,China
  • Received:2021-12-13 Published:2023-11-14

摘要: 研究青钱柳[Cyclocarya paliurus (Bata1.) Iljinskaja]叶片中2种黄酮苷元(槲皮素、山奈酚)的水解提取条件及其含量的高效液相色谱(HPLC)测定方法,为青钱柳叶片质量控制提供参考。以乙醇-盐酸混合溶液为溶剂,采用单因素试验和正交试验结合的方法考察提取水解条件;含量测定以Agilent C18色谱柱(250 mm×4.6 mm,5 μm)为分离柱,乙腈-0.1%甲酸水溶液(体积比为35∶65)为流动相,检测波长370 nm,柱温30 ℃,流速1.0 mL/min。结果表明,优化的提取水解条件为以乙醇-盐酸(体积比为8∶1)为溶剂,每次按料液比为1∶20的量加入,90 ℃恒温水浴回流60 min。槲皮素和山奈酚的进样量分别在0.080 8~0.808 7 μg(R2=0.999 7)、0.096 4~0.964 6 μg(R2=0.999 9)范围内呈良好的线性关系;槲皮素的平均加样回收率为100.97%、相对标准偏差(RSD)为2.93%,山奈酚的平均加样回收率为97.25%、相对标准偏差为3.29%。提取水解工艺可明显提高青钱柳叶片黄酮苷元含量;建立的检测方法快速、准确、重复性好,可为青钱柳叶片药材的质量评价提供技术参考。

关键词: 青钱柳[Cyclocarya paliurus (Bata1.) Iljinskaja]叶片, HPLC, 黄酮苷元, 槲皮素, 山奈酚

Abstract: The hydrolysis extraction conditions and content determination method of two flavonoid aglycones (quercetin and kaempferol) in Qingqianliu [Cyclocarya paliurus (Bata1.) Iljinskaja] leaves by high-performance liquid chromatography (HPLC) were studied to, provide reference for quality control of Qingqianliu leaves.Using ethanol-hydrochloric acid mixed solution as the solvent, the extraction and hydrolysis conditions were investigated using a combination of single factor and orthogonal experiments;content determination was conducted using Agilent C18 chromatographic column (250 mm × 4.6 mm, 5 μm) as the separation column and acetonitrile-0.1% formic acid aqueous solution (volume ratio 35∶65) as the mobile phase, with a detection wavelength of 370 nm, a column temperature of 30 ℃, and a flow rate of 1.0 mL/min. The results showed that the optimized extraction and hydrolysis conditions were as follows: Ethanol hydrochloric acid (volume ratio 8∶1) was used as the solvent, and the material-to-liquid ratio was 1∶20 each time, with a 90 ℃ constant temperature water bath reflux for 60 min. The injection volume of quercetin and kaempferol showed a good linear relationship, ranging from 0.080 8 to 0.808 7 μg (R2=0.999 7) and from 0.096 4 to 0.964 6 μg (R2=0.999 9), respectively;the average recovery rate of quercetin was 100.97%, with the relative standard deviation (RSD) of 2.93%. The average recovery rate of kaempferol was 97.25%, and the relative standard deviation was 3.29%. The extraction and hydrolysis process could significantly increase the content of flavonoid glycosides in Qingqianliu leaves;the established detection method was fast, accurate, and had good repeatability, which could provide technical reference for the quality evaluation of Qingqianliu leaves medicinal materials.

Key words: Qingqianliu [Cycloarya paliurus (Bata1.) Iljinskaja] leaves, HPLC, flavonoid aglycone, quercetin, kaempferol

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