主 办:北 京 中 医 药 大 学
ISSN 1006-2157 CN 11-3574/R

北京中医药大学学报 ›› 2018, Vol. 41 ›› Issue (5): 400-404.doi: 10.3969/j.issn.1006-2157.2018.05.008

• 中药化学 • 上一篇    下一篇

地骨皮中咖啡酰丁二胺、地骨皮乙素和绿原酸含量测定方法研究*

苏磊, 姜艳艳, 陈路晓, 刘静, 刘斌#   

  1. 北京中医药大学中药学院 北京 102488;
  • 收稿日期:2017-12-20 出版日期:2018-05-30 发布日期:2018-05-30
  • 通讯作者: # 刘斌,男,博士,教授,博士生导师,研究方向:中药(复方)有效成分(组分)发现与新药创制,E-mail:liubinyn67@163.com
  • 作者简介:苏磊,女,在读硕士生
  • 基金资助:
    *国家自然科学基金资助项目(No.81173520),北京中医药大学研究生自主选题资助项目(No. 2017-JYB-XS-142)

Quantitative determination of N-caffeoylputrescine, kukoamine B and chlorogenic acid in Digupi*

Su Lei, Jiang Yanyan, Chen Luxiao, Liu Jing, Liu Bin#
  

  1. School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing 102488, China;
  • Received:2017-12-20 Online:2018-05-30 Published:2018-05-30
  • Supported by:
    National Natural Science Foundation of China (No.81173520)

摘要: 目的 建立地骨皮中咖啡酰丁二胺、地骨皮乙素与绿原酸的含量测定方法。方法 采用单因素考察方法建立供试品溶液制备方法;采用高效液相色谱(HPLC)法测定咖啡酰丁二胺、地骨皮乙素与绿原酸的含量,色谱条件为Waters Xbridge C18(4.6 mm×250 mm,5 μm)色谱柱,甲醇-0.05%三氟乙酸溶液梯度洗脱,流速1.0 mL/min,检测波长为290 nm,柱温30 ℃。结果 地骨皮药材采用100倍量的70%甲醇回流提取60 min,制备供试品溶液;咖啡酰丁二胺在0.013 75 ~ 0.220 0 g/L范围内线性关系良好,r=0.999 5,平均加样回收率为99.25%,RSD=1.81%(n=6);地骨皮乙素在0.057 875~0.926 0 g/L范围内线性关系良好,r=0.999 8,平均加样回收率为101.01%,RSD=2.81%(n=6);绿原酸在0.009 25~0.148 0 g/L范围内线性关系良好,r=0.999 5,平均加样回收率为99.51%,RSD=2.32%(n=6)。结论 所建立的含量测定方法简便准确,重现性好,为地骨皮药材质量控制和评价奠定基础。

关键词: 地骨皮, 高效液相色谱法, 含量测定, 咖啡酰丁二胺, 地骨皮乙素, 绿原酸

Abstract: Objective To establish a method for quantitative determination of N-caffeoylputrescine, kukoamine B and chlorogenic acid in Digupi (Chinese Wolfberry Root-bark, Cortex Lycii). Methods The preparation method for solution of test sample was established by using single-factor investigation. HPLC procedure was performed for determining the content of N-caffeoylputrescine, kukoamine B and chlorogenic acid on chromatographic column of Waters Xbridge C18 (4.6 mm×250 mm, 5 μm), mobile phase was methanol-0.05% trifluoroacetic acid in gradient elution. The flow velocity was 1.0 mL/min and the detection wavelength was 290 nm at 30℃. Results The solution of test sample was prepared after Digupi was extracted with 100 times amount of 70% methanol by using reflux extraction for 60 min. N-caffeoylputrescine showed a good linear relationship at a range from 0.013 75 mg/mL to 0.220 0 g/L (r=0.999 5), and average recovery was 99.25% (RSD=1.81%, n=6). Kukoamine B showed a good linear relationship at a range from 0.057 875 g/L to 0.926 0 mg/mL (r=0.999 8), and average recovery was 101.01% (RSD=2.81%, n=6). Chlorogenic acid showed a good linear relationship at a range from 0.009 25 g/L to 0.148 0 g/L (r=0.999 5), and average recovery was 99.51% (RSD=2.32%, n=6). Conclusion The established quantitative determination method is easy and accurate with a good repeatability, which can lay a foundation for the quality control and reviewing of Digupi.

Key words: Digupi (Chinese Wolfberry Root-bark, Cortex Lycii), high performance liquid chromatograph, quantitative determination, N-caffeoylputrescine, kukoamine B

中图分类号: 

  • R284.1