牛蒡叶化学成分及主要成分动态积累规律分析  

Analysis on Chemical Constituents and Dynamic Accumulation of Main Components in Arctium lappa Leaves

作　　者：梁韩晶 吕江南 冯庆梅 张玲霞[1] 刘秋艳[1] 代丽萍[1] 王智民[2] LIANG Han-jing;LYU Jiang-nan;FENG Qing-mei;ZHANG Ling-xia;LIU Qiu-yan;DAI Li-ping;WANG Zhi-min(Engineering Technology Research Center for Comprehensive Development and Utilization of Authentic Medicinal Materials in Henan Province,Henan University of Chinese Medicine,Zhengzhou 450046,China;Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China)

机构地区：[1]河南中医药大学河南省豫产道地药材综合开发利用工程技术研究中心,郑州450046 [2]中国中医科学院中药研究所,北京100700

出　　处：《中国实验方剂学杂志》2022年第3期139-146,共8页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：国家重点研发计划项目(2017YFC1701904);河南省中医药科学研究专项(20-21ZY1027)。

摘　　要：目的:明确牛蒡叶的化学成分;阐明其主要成分的动态积累规律,为牛蒡叶适宜采收期的确定提供依据。方法:采用硅胶,大孔吸附树脂,LH-20型羟丙基葡聚糖凝胶(Sephadex LH-20),十八烷基硅烷键合硅胶(ODS),微孔树脂(MCI)等柱色谱法和高效液相色谱法(HPLC)对牛蒡叶中主要化学成分进行系统分离,结合谱学技术对所分离的成分进行鉴定;采用HPLC-二极管阵列检测器(DAD),Shim-pack GIST C18色谱柱(4.6 mm×250 mm,5μm),流动相乙腈(A)-0.3%磷酸水溶液(B)梯度洗脱(0~9 min,13%A,9~10 min,13%~24%A;10~30 min,24%A),流速1.0 mL·min-1,柱温40℃,检测波长328 nm,对牛蒡叶中4个成分进行积累动态分析。结果:从牛蒡叶中分离并鉴定了17个化合物,分别为咖啡酸(1),芦丁(2),山柰酚-3-O-芸香糖苷(3),槲皮素-3-O-β-D-吡喃葡萄糖苷(4),山柰酚-3-O-β-D-吡喃葡萄糖苷(5),绿原酸(6),异绿原酸A(7),胡萝卜苷(8),熊果酸(9),anemarrhenoside B(10),开环异落叶松脂醇(11),vladinol D(12),melitensin(13),秦皮乙素(14),1(-2-乙基苯基)-1,2-乙二醇(15),1-(4-乙基苯基)-1,2-乙二醇(16),3-羟基-1-(4-羟基-3,5-二甲氧基苯)-1-丙酮(17);绿原酸、芦丁、山柰酚-3-O-芸香糖苷、异绿原酸A为牛蒡叶中4个主要成分,其中绿原酸、芦丁和山柰酚-3-O-芸香糖苷含量在4~8月呈上升趋势,8月达到峰值;异绿原酸A含量在4~8月呈先上升后下降趋势,7月份达到峰值。结论:化合物10,12~17首次从牛蒡属中分离得到;以4个主要成分(绿原酸、芦丁、山柰酚-3-O-芸香糖苷、异绿原酸A)的含量为指标,结合牛蒡根、牛蒡叶资源的综合开发利用考虑,建议8月中旬采收牛蒡叶。Objective:To determine the chemical constituents of burdock(Arctium lappa)leaves,and elucidate dynamic accumulation rule of four main components,in order to provide the basis for determining the suitable harvest time of burdock leaves.Method:Silica gel,macroporous resin,Sephadex LH-20,octadecylsilane chemically bonded silica(ODS),microporous resin(MCI)column chromatography and reversed-phase preparative high performance liquid chromatography(HPLC)were used to isolate the main chemical constituents in burdock leaves.Their chemical structures were elucidated by spectroscopic techniques.HPLC-diode array detector(DAD)was used to analyze the dynamic accumulation of four components in burdock leaf.HPLC-DAD was performed on a Shim-pack GIST C18 column(4.6 mm×250 mm,5μm)with mobile phase of acetonitrile(A)-0.3%phosphoric acid aqueous solution(B)(0-9 min,13%A;9-10 min,13%-24%A;10-30 min,24%A),flow rate of 1.0 mL·min-1,column temperature of 40℃,and detection wavelength at 328 nm.Result:Seventeen compounds were isolated from burdock leaves,and identified as caffeic acid(1),rutin(2),kaempferol-3-O-rutinoside(3),quercetin-3-O-β-D-glucopyranoside(4),kaempferol-3-O-β-Dglucopyranoside(5),chlorogenic acid(6),isochlorogenic acid A(7),daucosterol(8),ursolic acid(9),anemarrhenoside B(10),(-)-secoisolariciresinol(11),vladinol D(12),melitensin(13),esculetin(14),1-(-2-ethylphenyl)-1,2-ethanediol(15),1-(-4-ethylphenyl)-1,2-ethanediol(16),3-hydroxy-1-(4-hydroxy-3,5-dimethoxyphenyl)-1-propanone(17).The contents of chlorogenic acid,rutin and kaempferol-3-O-rutinoside in burdock leaves showed an upward trend from April to August,and reached the highest in August.And the content of isochlorogenic acid A firstly increased and then decreased from April to August,and reached the highest in July.Conclusion:Compounds 10,12-17 were isolated from Arctium for the first time.Taking the contents of chlorogenic acid,rutin,kaempferol-3-O-rutinoside,and isochlorogenic acid A as indicators,considering the comprehensive development and utilization o

关 键 词：牛蒡叶 化学成分 黄酮苷 咖啡酰奎宁酸类 柱色谱法 绿原酸 高效液相色谱法(HPLC) 

分 类 号：R22[医药卫生—中医基础理论] R28[医药卫生—中医学]