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目的:研究沼生忍冬藤的化学成分并建立HPLC同时测定沼生忍冬不同药用部位中绿原酸,3,5二咖啡酰奎宁酸和4,5二咖啡酰奎宁酸含量的方法。方法:采用硅胶、反相硅胶、大孔树脂和LH-20羟丙基葡聚糖凝胶等多种色谱技术进行分离纯化,并通过理化性质及波谱数据鉴定化合物的结构。采用HPLC-UV法测定含量,色谱条件:Phenomenex C_(18)色谱柱(4.6 mm×250 mm,5μm),流动相乙腈(A)-0.2%磷酸水溶液(B)梯度洗脱(0~13 min,12%A;13~25 min,12%~22%A;25~45 min,22%A),流速1.0 mL·min~(-1),检测波长327 nm,柱温30℃,进样量10μL。结果:从沼生忍冬藤中分离得到10个化合物,分别鉴定为:3,7-二甲基槲皮素(1),3,3’-二甲基槲皮素(2),槲皮素(3),乌苏酸(4),马钱子苷(5),绿原酸(6),槲皮素5-O-β-D-葡萄糖苷(7),3,4-二咖啡酰奎宁酸(8),3,5-二咖啡酰奎宁酸(9)和4,5-二咖啡酰奎宁酸(10)。6,9和10三种成分均能达到基线分离,且线性关系良好,平均加样回收率分别为100.15%,99.68%和99.52%。沼生忍冬中3种成分的含量为花最高(3.99%,1.77%,2.33%),叶次之(2.62%,1.73%,0.90%),藤最低(0.74%,0.25%,0.15%)。结论:化合物1,2和7为首次从忍冬属植物中分离得到,其余化合物均为首次从该植物中分离得到;含量测定方法准确,简便,分离效果好,可用于沼生忍冬中绿原酸,3,5二咖啡酰奎宁酸和4,5二咖啡酰奎宁酸含量的测定。
OBJECTIVE: To study the chemical constituents of Houttuynia cordata Thunb.and establish HPLC method for the simultaneous determination of chlorogenic acid, dicaffeoylquaric acid and dicaffeoylquucanhydride in different medicinal parts. Methods: The compounds were separated and purified by silica gel, reverse phase silica gel, macroporous resin and LH-20 hydroxypropyl dextran gel. The structures of the compounds were identified by physicochemical properties and spectral data. The chromatographic conditions were as follows: Phenomenex C 18 column (4.6 mm × 250 mm, 5 μm), gradient elution with mobile phase of acetonitrile (A) -0.2% phosphoric acid (B) , 12% A, 13-25 min, 12-22% A, 25-45 min, 22% A) at a flow rate of 1.0 mL · min -1 .The detection wavelength was 327 nm. Amount of 10 μL. Results: Ten compounds were isolated from Lonicera japonicus and identified as 3,7-dimethylquercetin (1), 3,3’-dimethylquercetin (2), quercetin (3), ursolic acid (4), strychnine (5), chlorogenic acid (6), quercetin 5-O-β-D-glucoside (7) Quinic acid (8), 3,5-dicaffeoylquinic acid (9) and 4,5-dicaffeoylquinic acid (10). The three components of 6, 9 and 10 all achieved the baseline separation with a good linearity. The average recoveries were 100.15%, 99.68% and 99.52%, respectively. The contents of the three components in the marsh biomass were the highest (3.99%, 1.77%, 2.33%), followed by the leaves (2.62%, 1.73%, 0.90%) and the lowest was the vine (0.74%, 0.25%, 0.15%). CONCLUSION: Compounds 1, 2 and 7 are isolated from Honeysuckle for the first time, and the rest of the compounds are isolated from this plant for the first time. The assay method is accurate and simple, and the separation effect is good. , 3,5 decaffeoylquinic acid and 4,5 dicaffeoylquinic acid content determination.