Shandong Analysis and Test Center, Shandong Academy of Sciences, 19 Keyuan Street, Jinan, Shandong 250014, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Oct 15;879(28):3023-7. doi: 10.1016/j.jchromb.2011.08.040. Epub 2011 Sep 2.
A microwave-assisted extraction (MAE) method is presented for the extraction of xanthones, α-mangostin and γ-mangostin from Garcinia mangostana. The MAE conditions including extraction temperature, liquid/solid ratio, extraction time and concentration of ethanol were optimized with an orthogonal test, and 5 g sample was extracted with the optimized conditions. The crude extraction of MAE was successfully isolated and purified by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-water (0.8:0.8:1:0.6, v/v) in one-step separation. The separation yielded 75 mg of α-mangostin at 98.5% purity, and 16 mg of γ-mangostin at 98.1% purity from 360 mg crude extract of G. mangostana in less than 7h. The purity of the two xanthones was determined by HPLC. Their structures were further identified by ESI-MS, (1)H NMR and (13)C NMR.
一种微波辅助提取（MAE）方法被提出用于从藤黄科植物藤黄中提取黄烷酮、α-倒捻子素和γ-倒捻子素。通过正交试验优化了 MAE 条件，包括提取温度、液固比、提取时间和乙醇浓度，并采用优化条件对 5g 样品进行了提取。粗提物通过高速逆流色谱（HSCCC）成功分离和纯化，采用石油醚-乙酸乙酯-甲醇-水（0.8:0.8:1:0.6，v/v）两相溶剂系统一步分离。从 360mg 藤黄粗提取物中分离得到 75mg 纯度为 98.5%的α-倒捻子素和 16mg 纯度为 98.1%的γ-倒捻子素，不到 7h。两种黄烷酮的纯度通过 HPLC 确定。通过 ESI-MS、（1）H NMR 和（13）C NMR 进一步鉴定了它们的结构。
