炎立消化学成分的分离与分析  

Chemical constituents isolation and analysis of Yanlixiao

作　　者：韩晶[1] 王建军[1] 王丹[1] 唐万侠[1] 赵明[1] 张树军[1] 

机构地区：[1]齐齐哈尔大学,齐齐哈尔161006

出　　处：《中华中医药杂志》2013年第1期217-220,共4页China Journal of Traditional Chinese Medicine and Pharmacy

基　　金：教育部留学回国基金项目(No.2005383)~~

摘　　要：目的:研究炎立消中主要化学成分,建立一种利用HPLC法测定炎立消中丁香苦苷和橄榄苦苷含量的方法,并用该方法测定不同厂家炎立消产品中丁香苦苷和橄榄苦苷的含量。方法:采用硅胶柱色谱和高效液相色谱法对炎立消甲醇提取物进行分离纯化,通过理化性质及波谱数据进行结构鉴定;在Agilent 1200高效液相色谱仪上,采用Agilent Eclipse XDB-C18(4.6mm×50mm,5μm)色谱柱,研究测定炎立消中丁香苦苷和橄榄苦苷含量的色谱分析法。结果:从炎立消中分离得到8个化合物,分别鉴定为对羟基苯乙醇(1)、乌苏酸(2)、β-谷甾醇葡萄糖苷(3)、橄榄苦苷(4)、丁香苦苷(5)、对羟基苯乙醇乙酸酯(6)、2-(3,4二羟基)苯乙醇乙酸酯(7)和葡萄糖(8);在乙腈1:水=20:80为流动相,在流速为1.0mL/min,柱温为25℃,进样量为5μL,检测波长变化为0→3min(356nm),3→15min(223nm)的色谱条件下,丁香苦苷在0.16-0.48g/L(r=0.99911)范围内线性关系良好,橄榄苦苷在0.24-0.56g/L(r=0.99908)范围内线性关系良好。化合物1、4、5、7和8为炎立消产品中的主要化学成分,其含量分别为:5.4、0.8、21.9、0.7和4.5mg/g。结论:利用该方法测定炎立消制剂及紫丁香叶中丁香苦苷和橄榄苦苷的含量准确、可靠,不同厂家生产的炎立消制剂中主要化学成分的含量存在较大差别。Objective： To study the chemical constituents of Yanlixiao and construct a method to analysis the content of syringopicroside and oleuropein in Yanlixiao by HPLC. Accordingly, this method was expanded to use to analysis the content of the major constituents of Yanlixiao derived from different companies. Methods： The MeOH extract of Yanlixiao was isolated and purified by silica column chromatography and HPLC. The structures of isolated compounds were elucidated by physicochemical properties and by analyzing spectroscopic data. The chromatography analysis methods were established by using Agilent 1200 combining the column of Agilent Eclipse XDB-C18 （4.6mm × 50mm, 5um）. Results： As the results, eight compounts, p-hydroxy phenylethanol（1）, ursolic acid（2）, -sitosterolglucoside（3）, oleuropein （4）, syringopicroside（5）, p-hydroxy phenylethanol acetate（6）, 2-（3,4-dihydroxyl）-phenylethanol acetate（7）, and glucose（8）, were isolated. Syringopicroside（5） and oleuropein （4） showed better linear relationship at the concentration of 0.16-0.48g/L （r=-0.99911） and 0.20-0.52g/L（r=-0.99908）, respectively, under the chromatography conditions of Acetonitrile-H2O（20/80, at a flow rate of 1.0mL/min）, column temperature of 25℃, injection amount of 5L, and UV detector of 0→3min （356nm）, 3→15min （223nm）. Conclusion： Compounds 1, 4, 5, 7, and 8 were the major chemical constituents of Yanlixiao with the concentration of 5.4mg/g, 0.8mg/g, 21.9mg/g, 0.7mg/g, and 4.5mg/g, respectively. This research provided an accurate method to analysis the concentration of syringopicroside and oleuropein in Yanlixiao. Analyzed by HPLC, the concentrations of major chemical constituents of Yanlixiao collected from different companies exhibited big difference.

关 键 词：炎立消 HPLC 丁香苦苷 橄榄苦苷 

分 类 号：R286.0[医药卫生—中药学]