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首页> 外文期刊>Separation and Purification Technology >Preparation of flavonoids and diarylheptanoid from Alpinia katsumadai hayata by microwave-assisted extraction and high-speed counter-current chromatography
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Preparation of flavonoids and diarylheptanoid from Alpinia katsumadai hayata by microwave-assisted extraction and high-speed counter-current chromatography

机译：微波辅助萃取-高速逆流色谱法从高山pin中制备黄酮和二芳基庚烷

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摘要

In the present work, five flavonoids and diarylheptanoid, namely, alpinetin, pinocembrin chalcone, pino-cembrin, cardamomin and l,7-diphenyl-4,6-heptadien-3-one, were simply and rapidly prepared from Alpinia katsumadai hayata (A katsumadai) by microwave-assisted extraction (MAE) followed with highspeed counter-current chromatography (HSCCC). The critical conditions of MAE and HSCCC were optimized. 2.0 g crude sample was extracted with MAE, and then directly separated and purified by HSCCC with a two-phase solvent system composed of hexane-ethyl acetate-methanol-water (3:7:6:4, v/v/v/ v), and 7.5 mg of alpinetin, 1.9 mg of pinocembrin chalcone, 2.6 mg of 1,7-diphenyl-4,6-heptadien-3-one with purities of 98.3%, 96.9% and 93.0% were obtained respectively in a single step within 4 h. 4.0 mg mixture of cardamomin and pinocembrin from HSCCC was further separated by prep-HPLC, 2.1 mg of 99.4% pinocembrin and 1.4 mg of 99.8% cardamomin were obtained respectively. The purities of compounds were determined by HPLC and their chemical structures were further identified by ESI-MS and ~1H NMR. The results demonstrated that MAE coupled with HSCCC was a feasible, economical and efficient technique for rapid extraction, separation and purification of effective compounds in natural products.
机译：在目前的工作中，从高山积木（Alpinia katsumadai hayata（A）高效液相色谱（HSCCC）进行微波辅助萃取（MAE）。优化了MAE和HSCCC的临界条件。用MAE提取2.0 g粗样品，然后直接分离并通过HSCCC进行纯化，使用由己烷-乙酸乙酯-甲醇-水（3：7：6：4，v / v / v / v组成的两相溶剂系统） ），一步法制得纯度分别为98.3％，96.9％和93.0％的7.5 mg高山铁素，1.9 mg松球蛋白查尔酮，2.6 mg 1,7-二苯基-4,6-庚二烯-3-酮4小时内通过制备型HPLC进一步从HSCCC中分离出4.0 mg豆蔻素和匹诺溴胺的混合物，分别获得2.1 mg的99.4％匹诺贝姆和1.4 mg的99.8％豆蔻素。通过HPLC测定化合物的纯度，并通过ESI-MS和〜1H NMR进一步鉴定其化​​学结构。结果表明，MAE与HSCCC结合使用是一种可行，经济且有效的技术，用于快速提取，分离和纯化天然产物中的有效化合物。

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