天然产物研究与开发 ›› 2021, Vol. 33 ›› Issue (增刊1): 52-59.doi: 10.16333/j.1001-6880.2021.S.007

• 研究论文 • 上一篇    下一篇

桃儿七药材的HPLC指纹图谱研究及其4种主要成分的含量测定

LIU Ying-ying,XU Xian-li,FENG Hai-sheng,LI Cai-xia,MA Shi-zhen   

  1. 1中国科学院西北高原生物研究所;2青海省青藏高原特色生物资源研究重点实验室,西宁 810008;3中国科学院大学,北京 100049

  • 出版日期:2021-08-28 发布日期:2021-09-08
  • 基金资助:
    青海省应用基础研究(2019-ZJ-7061);青海省重点实验室专项“青海省藏药药理学和安全性评价研究重点实验室”(2017-ZJ-Y08)

Study on HPLC fingerprint of Sinopodophyllum hexandrum and content determination of its four main constituents

LIU Ying-ying1,2,3,XU Xian-li1,2,3,FENG Hai-sheng1,2,LI Cai-xia1,2*,MA Shi-zhen1,2*   

  1. 1Northwest Institute of Plateau Biology,Chinese Academy of Sciences;2 Qinghai Key Laboratory of Qinghai-Tibet Plateau Biological Resources,Xining 810008,China3University of Chinese Academy of Sciences,Beijing 100049,China

  • Online:2021-08-28 Published:2021-09-08

摘要:

为了建立桃儿七药材的HPLC指纹图谱,并同时测定其中4种主要成分含量。采用JADE-PAK ODS(4.6 mm×250 mm,5 μm)色谱柱;以乙腈(A)-0.04%甲酸水(B)为流动相进行梯度洗脱,体积流量1.0 mL/min,检测波长254 nm,柱温30 ℃,进样量10 μL。最终建立了12批桃儿七样品的HPLC指纹图谱,进行了相似度比较,确定了11个共有峰,并指认了其中4′-去甲基鬼臼毒素、槲皮素、山奈酚、鬼臼毒素4种成分。建立了4′-去甲基鬼臼毒素、槲皮素、山奈酚、鬼臼毒素4种成分同时测定方法,该方法在进样量范围内与峰面积线性关系良好,精密度、稳定性、重复性、加样回收率的RSD均符合要求。含量测定结果表明各产地桃儿七药材中4种主要成分含量差异明显,西藏地区桃儿七中4种主要成分含量均达到最高。本研究建立了不同产地桃儿七药材HPLC指纹图谱结合多成分含量测定方法,该方法专属性强、重复性好,为完善桃儿七药材的质量控制提供了参考。

关键词: 桃儿七, HPLC, 指纹图谱, 鬼臼毒素, 4′-去甲基鬼臼毒素, 山奈酚, 槲皮素

Abstract:

To establish the HPLC fingerprint of Sinopodophyllum hexandrum,and to determine the contents of four constituents.JADE-PAK ODS(4.6 mm×250 mm,5 μm)column was used.Acetonitrile (A)-0.04% formic acid (B) was used as the mobile phase for gradient elution.The flow rate was 1.0 mL/min.The eluate was monitored by UV absorption at 254 nm.The column temperature was 30 ℃,and the injection volume was 10 μL.Results:HPLC fingerprint of S. hexandrum was established,and the similarity of 12 batches of S. hexandrum samples were compared.And 11 common peaks were identified,among which 4′-demethylpodophyllotoxin,quercetin,kaempferol and podophyllotoxin were identified.A method for simultaneous determination of 4′-demethylpodophyllotoxin,quercetin,kaempferol and podophyllotoxin was established,and the linear relationship between the peak area and the range of the injection volume was good,respectively.The RSD of precision,stability,repeatability,and sample recovery all meet the requirements.The content determination results showed that the contents of four main constituents in S. hexandrum from different regions were significantly different,and the contents of four main constituents in S. hexandrum from Tibet reached the highest level.This study established a method for HPLC fingerprint and multi-component content determination of S. hexandrum from different origins.This method has strong specificity and good repeatability,providing a reference for improving the quality control of S. hexandrum.

Key words: Sinopodophyllum hexandrum, HPLC, fingerprint, podophyllotoxin, 4′-demethylpodophyllotoxin, kaempferol, quercetin

中图分类号:  R284