沼生忍冬藤化学成分及3种成分的含量测定  

Chemical Constituents and Simultaneous Determination of Three Compounds from Lonicera alberti Caulis

作　　者：李思远[1] 滕亮[1] 詹羽姣 徐芳 赵军 

机构地区：[1]新疆医科大学药学院,乌鲁木齐830011 [2]新疆药物研究所维吾尔药重点实验室,乌鲁木齐830004

出　　处：《中国实验方剂学杂志》2017年第19期94-99,共6页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：新疆维吾尔自治区科技人才培养项目(QN2016YX0689)

摘　　要：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 investigate the chemical constituents from caulis of Lonicera alberti and establish an HPLC method for simultaneously determining the contents of chlorogenic acid, 3,5-O-dicaffeoylquinic acid and 4,5-O-dicaffeoylquinic acid in different pharmaceutical parts of L. alberti. Method： Chemical constituents were isolated and purified by various chromatographic techniques such as silica gel, reversed-phase silica gel, macroporous resin, and Sephadex LH-20 column chromatography. Their structures were elucidated by physicochemical properties and spectroscopic data. The chromatographic conditions were as follows：Phenomenex C18 column （4.6 mm×250 mm, 5 μm）, with acetonitrile （A） and 0.2% phosphoric acid solution （B） as the mobile phase for gradient elution （0-13 min, 12%A; 13-25 min, 12%-22%A; 25-45 min, 22%A）. The flow rate was 1.0 mL·min^-1, detection wavelength at 327 nm, column temperature at 30℃,and injection volume at 10 μL. Result： Ten compounds were separated from L. alberti, and identified as 3,7-dimethylquercetin （1）, 3,3＇-dimethylquercetin （2）, quercetin （3）, ursolic acid （4）, loganin （5）, chlorogenic acid （6）, quercetin 5-O-β-D-glucoside （7）, 3,4-O-dicaffeoylquinic acid （8）, 3,5-O-dicaffeoylquinic acid （9） and 4,5-O-dicaffeoylquinic acid （10）. Compounds 6, 9 and 10 achieved baseline separation and showed good linearity, and the average recoveries were 100.15%, 99.68% and 99.52% respectively. The content of three compounds from L. alberti flower（3.99%, 1.77%,2.33%） was more than that of leaves （2.62%, 1.73%, 0.90%） and caulis （0.74%,0.25%, 0.15%）. Conclusion： Compounds 1, 2 and 7 were isolated from Lonicera genus for the first time, and other compounds were found from this plant for the first time. The content determination method was accurate, reliable and convenient, so it could be used for content determination of chlorogenic acid, 3,5-dicaffeoylquinic acid and 4,5-dicaffeoylquinic acid in L. alberti.

关 键 词：忍冬属 沼生忍冬 3 7-二甲基槲皮素 3 3'-二甲基槲皮素 檞皮素5-O-β-D-葡萄糖苷 

分 类 号：R284.1[医药卫生—中药学]