College of Pharmacy, Dalian Medical University, Dalian, China.
J Sep Sci. 2012 Aug;35(15):1977-84. doi: 10.1002/jssc.201200011.
High-speed counter-current chromatography (HSCCC) coupled with ultraviolet (UV) detection or evaporative light-scattering detection was successfully applied for preparative separation of five bioactive compounds from Agrimonia pilosa Ledeb. In preliminary process, D101 macroporous resin was used to separate the crude extract of the plant and four fractions (20, 40, 50, and 60% aqueous ethanol elutions) were produced. Then, these fractions were directly subjected to HSCCC purification. Five chemicals including taxifolin-3-glucoside (6.4 mg), quercetin-3-rhamnoside (13.0 mg), tiliroside (14.7 mg), agrimonolide (21.4 mg), and tormentic acid (29.8 mg) with the purities of 94.24, 95.37, 97.42, 95.29, and 96.34% were separated from each 200 mg prepared fraction. The purities were analyzed by high-performance liquid chromatography, and the chemical structures of the products were identified by UV detection, mass spectrometry, nuclear magnetic resonance, and the standards. This paper used a simple method to separate five bioactive compounds from A. pilosa Ledeb, and it could provide a new idea for the purification of bioactive compounds from other medicinal plants.
高速逆流色谱(HSCCC)结合紫外(UV)检测或蒸发光散射检测成功地应用于从龙牙草(Agrimonia pilosa Ledeb)中分离五种生物活性化合物的制备分离。在初步过程中,使用 D101 大孔树脂分离植物的粗提取物,并产生四个馏分(20、40、50 和 60%水乙醇洗脱)。然后,这些馏分直接进行 HSCCC 纯化。从每个 200mg 制备馏分中分离出五种化学物质,包括杨梅素-3-葡萄糖苷(6.4mg)、槲皮素-3-鼠李糖苷(13.0mg)、三叶豆紫檀苷(14.7mg)、龙牙草苷(21.4mg)和鞣酸(29.8mg),纯度分别为 94.24%、95.37%、97.42%、95.29%和 96.34%。通过高效液相色谱分析纯度,并通过紫外检测、质谱、核磁共振和标准品鉴定产物的化学结构。本文采用简单的方法从龙牙草中分离出五种生物活性化合物,为从其他药用植物中分离生物活性化合物提供了新的思路。