摘要
目的:建立同时测定银杏叶中6种有机酸类成分的含量测定方法,分析6种有机酸的组成状况。方法:采用ODS-3 C18色谱柱(250 mm×4. 6 mm,5μm),乙腈(A)-0. 4%磷酸溶液(B)为流动相,梯度洗脱(0~8 min,5%~6%A;8~13 min,6%~6%A;13~20 min,6%~7%A;20~24 min,7%~8%A;24~33 min,8%~15%A;33~43 min,15%~15%A;43~44 min,15%~100%A;44~54 min,100%~100%A);流速为1. 0 m L·min-1;柱温40℃;双波长检测;进样量10μL。结果:6种有机酸成分实现较好的分离。没食子酸、原儿茶酸、6-羟基犬尿喹啉酸、对羟基苯甲酸、对羟基肉桂酸、咖啡酸分别在0. 007~0. 071,0. 133~1. 333,0. 013~0. 129,0. 013~0. 129,0. 003~0. 027和0. 001~0. 013μg范围内,与色谱峰峰面积呈良好线性关系;平均回收率(n=9)分别为100. 39%,101. 26%,100. 29%,102. 15%,100. 33%和99. 41%;RSD分别为2. 73%,1. 82%,0. 56%,1. 94%,2. 00%和2. 01%。结论:所建立的有机酸含量测定方法简便、准确可靠、重复性好。11份银杏叶样品测定结果表明6种有机酸成分的含量分布情况由大到小依次为原儿茶酸> 6-羟基犬尿喹啉酸>没食子酸>对羟基苯甲酸>对羟基肉桂酸>咖啡酸,总含量平均值为0. 095%。
Objective:To establish a method for simultaneous determination of six organic acids and analyze the composition of six organic acids in Ginkgo leaves.Methods:The quantitative analysis was performed on an ODS-3 C18(250 mm×4.6 mm,5μm)column eluted with mobile phase consisting of acetonitrile(A)-0.4%phosphoric acid solution(B)in a gradient mode(0~8 min,5%~6%A;8~13 min,6%~6%A;13~20 min,6%~7%A;20~24 min,7%~8%A;24~33 min,8%~15%A;33~43 min,15%~15%A;43~44 min,15%~100%A;44~54 min,100%~100%A)at a flow rate of 1.0 m L·min-1.The column temperature was set at 40℃.And dual wavelength scanning was conducted for detection.The injection volume was 10μL.Results:The six organic acid components were completely separated.The calibration curves of gallic acid,protocatechuic acid,6-hydroxy canine quinolinic acid,hydroxybenzoic acid,p-hydroxycinnamic acid and caffeic acid showed a good linear relationship in the range of 0.007~0.071,0.133~1.333,0.013~0.129,0.013~0.129,0.003~0.027,and 0.001~0.013μg,respectively.The average recoveries were 100.39%,101.26%,100.29%,102.15%,100.33%and 99.41%,respectively.The RSDs were 2.73%,1.82%,0.56%,1.94%,2.00%and 2.01%(n=9),respectively.Conclusion:The established method for determining the contents of organic acids is simple,accurate,reliable,reproducible and feasible.The determination results of 11 Ginkgo leaves samples showed that the contents of the six organic acid components were in the following sequence:protocatechuic acid>6-hydroxy canine quinolinic acid>gallic acid>p-hydroxy benzoic acid>p-hydroxy cinnamic acid>caffeic acid.The average total content was 0.095%.
作者
殷海利
赵一懿
郭洪祝
陈有根
傅欣彤
YIN Hai-li;ZHAO Yi-yi;GUO Hong-zhu;CHEN You-gen;FU Xin-tong(College of Chinese Materia Medica,Beijing University of Chinese Medicine,Beijing 102488,China;Beijing Institute for Drug Control,Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine,Beijing 102206,China)
出处
《中国新药杂志》
CAS
CSCD
北大核心
2019年第12期1505-1510,共6页
Chinese Journal of New Drugs
基金
国家中医药管理局中药标准化资助项目(ZYBZH-C-HEB-16)
