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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 main chemical constituents in Yanliuqing and to establish a HPLC method for the determination of syringin and oleuropein in Yanliu consumption. The method was used to determine the contents of syringin and olives Glycoside content. Methods: Silica gel column chromatography and high performance liquid chromatography (HPLC) were used to separate and purify the methanol extracts of YL. The structures were elucidated on the basis of physicochemical properties and spectral data. On an Agilent 1200 HPLC system, Agilent Eclipse XDB-C18 4.6mm × 50mm, 5μm) column chromatography to study the determination of syringomycin and oleuropein content chromatographic analysis. Results: Eight compounds were isolated from Yanliuhu and identified as p-hydroxybenzeneethanol (1), ursolic acid (2), β-sitosterol glucoside (3), oleuropein (4) Glycoside (5), p-hydroxyphenethyl acetate (6), 2- (3,4 dihydroxy) phenethyl acetate acetate (7) and glucose Phase at a flow rate of 1.0 mL / min, a column temperature of 25 ° C., an injection volume of 5 μL and a detection wavelength of 0 → 3 min (356 nm) and 3 → 15 min (223 nm) 0.48g / L (r = 0.99911) in the range of good linear relationship, oleuropein 0.24-0.56g / L (r = 0.99908) within a good linear relationship. Compounds 1, 4, 5, 7 and 8 are the main chemical components of Yanliu products, and their contents are respectively 5.4, 0.8, 21.9, 0.7 and 4.5mg / g. Conclusion: The content of syringomycin and oleuropein in YLI and Lilac leaves can be determined accurately and reliably by this method. There are great differences in the content of main chemical constituents in YLD produced by different manufacturers.