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,5μm)色谱柱,甲醇-0.05%三氟乙酸溶液梯度洗脱,流速1.0 m L/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。
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 agood 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.
作者
苏磊
姜艳艳
陈路晓
刘静
刘斌
Su Lei;Jiang Yanyan;Chen Luxiao;Liu Jing;Liu Bin(School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing 102488, China)
出处
《北京中医药大学学报》
CAS
CSCD
北大核心
2018年第5期400-404,共5页
Journal of Beijing University of Traditional Chinese Medicine
基金
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)~~
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
Digupi （Chinese Wolfberry Root-bark
Cortex Lycii ）
high performance liquid chromato-graph
quantitative determination
N-caffeoylputrescine
kukoamine B
作者简介
苏磊，女，在读硕士生;通信作者：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
