Jiangsu Collaborative Innovation Center of Chinese Medicinal Resources Industrialization, Nanjing University of Chinese Medicine, Nanjing, 210023, China.
College of Pharmacy and Shaanxi Collaborative Innovation Center of Chinese Medicinal Resources Industrialization, Shaanxi University of Chinese Medicine, Xi'an, 712046, China.
Biomed Res Int. 2018 Sep 12;2018:4598067. doi: 10.1155/2018/4598067. eCollection 2018.
In the present study, the process of ultrasound-assisted extraction (UAE) followed by macroporous resin purification was successfully developed to achieve maximal recovery of functional components (flavonoids and ginkgolides) with minimal contents of toxic components (alkylphenols) from leaves. Three effective extracted factors including HAc%, EtOH%, and UAE power were screened by Plackett-Burman design (PBD). The important variables were further optimized by rotatable central composite design (RCCD). By combination of PBD and RCCD, the resulting optimal UAE conditions were as follows: HAc% of 1.8%, EtOH% of 63%, ultrasound power of 303 W, leaves powder amount of 1.0 g (solvent-to-solid ratio 40 mL/g), particle size of 60 mesh, extraction time of 40 min, and extraction temperature of 45°C. Under the optimum conditions, the yield of flavonoids was 25.1 ± 0.81 mg/g, ginkgolides was 10.6 ± 0.57 mg/g, and alkylphenols was 3.96 ± 0.31 mg/g. Moreover, the further enriching the functional components and removing toxic components from the obtained extracts of leaves using the above optimum UAE condition was successfully achieved by macroporous resin DA-201. After column adsorption and desorption on DA-201, the content of total flavonoids was 36.51 ± 1.53%, ginkgolides was 13.24 ± 0.85%, and alkylphenols was 7.0 ± 1.0 g/g from the obtained dry extracts (drug to extract ratio of 45-50:1) of leaves which were complied with Chinese pharmacopoeias.
在本研究中,成功开发了超声辅助提取(UAE)后大孔树脂纯化的工艺,从叶片中最大限度地回收功能成分(黄酮类和银杏内酯),同时最小化有毒成分(烷基酚)的含量。通过 Plackett-Burman 设计(PBD)筛选了 3 种有效的提取因素,包括 HAc%、EtOH%和 UAE 功率。通过旋转中心复合设计(RCCD)进一步优化了重要变量。通过 PBD 和 RCCD 的组合,得出的最佳 UAE 条件如下:HAc%为 1.8%、EtOH%为 63%、超声功率为 303 W、叶粉量为 1.0 g(溶剂-固比为 40 mL/g)、粒径为 60 目、提取时间为 40 min、提取温度为 45°C。在最佳条件下,黄酮类化合物的收率为 25.1±0.81 mg/g,银杏内酯的收率为 10.6±0.57 mg/g,烷基酚的收率为 3.96±0.31 mg/g。此外,通过使用上述最佳 UAE 条件从叶片提取物中进一步富集功能成分并去除有毒成分,成功地使用大孔树脂 DA-201 实现了这一目标。在 DA-201 柱上吸附和解吸后,从叶片获得的干提取物(药材与提取物的比例为 45-50:1)中总黄酮的含量为 36.51±1.53%,银杏内酯的含量为 13.24±0.85%,烷基酚的含量为 7.0±1.0 g/g,符合中国药典的要求。