School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Aug 15;879(24):2397-402. doi: 10.1016/j.jchromb.2011.06.035. Epub 2011 Jul 2.
An on-line method based upon dynamic microwave-assisted extraction (DMAE) coupled with high-speed counter-current chromatography (HSCCC) was developed for continuous isolation of nevadensin from Lyeicnotus pauciflorus Maxim. The DMAE parameters were optimized by means of the Box-Behnken design. The maximum extraction yield was achieved using 30:1 ml/g of liquid-solid ratio, 10 ml/min of solvent flow rate and 200 W of microwave power. The crude extracts were then separated by HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (7:3:5:5, v/v/v/v). 13.0mg of nevadensin was isolated from 15.0 g original sample by HSCCC with five times sample injection in 12h, and the isolation yield of nevadensin was 0.87 mg/g. The average purity of nevadensin was higher than 98.0%. The chemical structure of collected fraction was identified by HPLC, ESI-MS and (1)H NMR. The results indicated that this on-line method was effective and fast for high-throughput isolation of nevadensin from L. pauciflorus Maxim.
基于动态微波辅助提取 (DMAE) 与高速逆流色谱 (HSCCC) 联用的在线方法被开发出来，用于从少花龙舌兰中连续分离新穿心莲内酯。通过 Box-Behnken 设计优化了 DMAE 参数。采用 30:1 ml/g 的液固比、10 ml/min 的溶剂流速和 200 W 的微波功率，可获得最大提取收率。然后，用由正己烷-乙酸乙酯-甲醇-水（7:3:5:5，v/v/v/v）组成的两相溶剂体系通过 HSCCC 对粗提取物进行分离。通过 HSCCC 从 15.0 g 原始样品中五次进样，在 12 h 内分离得到 13.0mg 的新穿心莲内酯，其分离收率为 0.87 mg/g。新穿心莲内酯的平均纯度高于 98.0%。通过 HPLC、ESI-MS 和 (1)H NMR 对收集到的馏分进行了结构鉴定。结果表明，该在线方法对于从少花龙舌兰中高通量分离新穿心莲内酯是有效且快速的。
