车前子总黄酮的纯化及其成分的液相质谱联用分析

采用DPPH自由基清除法和邻苯三酚自氧化抑制法对车前子黄酮初提液的不同溶剂萃取液的体外抗氧化能力进行了比较,发现正丁醇萃取液具有与初提液相近的抗氧化能力,说明用正丁醇能萃取出大部分有效成分.并比较了AB-8、D101、NKA-2、NKA-9四种大孔吸附树脂对车前子黄酮的吸附及解吸性能,以选择合适的车前子黄酮纯化工艺.将纯化液进行液质联用分析其组成.结果表明,AB-8型树脂吸附和解吸率最高,适合萃取后的车前子黄酮的纯化,纯化后黄酮含量可从4%提高到30%以上.采用液质联用技术分析纯化液,确定其主要成分为苯乙醇苷类毛蕊花苷、异毛蕊花苷、大车前苷和黄酮类物质野漆树苷.

Purification of Semen Plantaginis Flavonoids and Components Analysis by LC-MS

The in vitro antioxidative activities of different solvent extracts were compared by examining the decoloration of the 1,1-diphenyl-2-picrylhydrazyl (DPPH) and the superoxide generated from autoxidation of pyrogallol. It is found that the antioxidative activities of n-butanol extract was most closed to ethanol extract, which means n-butanol is the best solvent to extract main functional components in ethanol extract. Then the performance of absorption and desorption for flavonoids from Semen Plantaginis with four types of macroreticular resins AB-8, D101, NKA-2, NKA-9 were determined, in order to select the better purification process of Semen Plantaginis flavonoids. The results showed that the AB-8 resin had the highest ratio of absorption and desorption and was the most suitable absorbent. The purify of flavonoids was raised from 4% to 30% after absorption and separation by this resin. It was determined by LC-MS chromatograms that the main components in the solution purified were several phenylethanoid glycosides such as Verbascoside, Isoverbascoside and Plantamajoside, an iridoid i.e. Geniposidic acid and two flavonoids i.e. Rhoifolin and Apigenin-7-O-glucoside.