Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Qilu University of Technology (Shandong Academy of Sciences), Jinan 250014, China.
College of Pharmacy, Shandong University of Traditional Chinese Medicine, Jinan 250355, China.
Molecules. 2017 Nov 23;22(12):2024. doi: 10.3390/molecules22122024.
Ten compounds, including three lignan glycosides and seven lignans, were purified from L. in 8 h using an efficient strategy based on high-speed counter-current chromatography (HSCCC). The two-phase solvent system composed of petroleum-ethyl acetate-methanol-H₂O (1:0.7:1:0.7, /) was firstly employed to separate the crude extract (320 mg), from which 19.3 mg of justicidin B (), 10.8 mg of justicidin A (), 13.9 mg of 6'-hydroxyjusticidin C (), 7.7 mg of justicidin E (), 6.3 mg of lignan J₁ () were obtained with 91.3 mg of enriched mixture of compounds -. The enriched mixture (91.3 mg) was further separated using the solvent system consisting of petroleum-ethyl acetate-methanol-H₂O (3:3.8:3:3.8, /), yielding 12.1 mg of procumbenoside E (); 7.6 mg of diphyllin-1--β-d-apiofuranoside (); 7.4 mg of diphyllin (); 8.3 mg of 6'-hydroxy justicidin B (); and 7.9 mg of diphyllin acetyl apioside (). The purities of the 10 components were all above 94%, and their structures were identified by NMR and ESI-MS spectra. The results demonstrated that the strategy based on HSCCC for the separation of lignans and their glycosides was efficient and rapid.
从 L. 中分离得到了 10 种化合物，包括 3 种木脂素糖苷和 7 种木脂素，采用基于高速逆流色谱（HSCCC）的有效策略，在 8 小时内即可完成。该两相溶剂系统由石油醚-乙酸乙酯-甲醇-水（1:0.7:1:0.7，/）组成，首先用于分离粗提取物（320mg），从中得到 19.3mg 正义丁素 B（）、10.8mg 正义丁素 A（）、13.9mg 6'-羟基正义丁素 C（）、7.7mg 正义丁素 E（）、6.3mg 木脂素 J₁（）和 91.3mg 化合物 - 的富集混合物。使用石油醚-乙酸乙酯-甲醇-水（3:3.8:3:3.8，/）溶剂系统进一步分离富集混合物（91.3mg），得到 12.1mg 前布森苷 E（）、7.6mg 二叶素-1--β-d-阿比呋喃糖苷（）、7.4mg 二叶素（）、8.3mg 6'-羟基正义丁素 B（）和 7.9mg 二叶素乙酰阿比糖苷（）。10 种成分的纯度均高于 94%，其结构通过 NMR 和 ESI-MS 谱确定。结果表明，基于 HSCCC 的分离木脂素及其糖苷的策略高效快速。
