Rapid preparative separation of six bioactive compounds from Gentiana crassicaulis Duthie ex Burk. using microwave-assisted extraction coupled with high-speed counter-current chromatography.
Rapid preparative separation of six bioactive compounds from Gentiana crassicaulis Duthie ex Burk. using microwave-assisted extraction coupled with high-speed counter-current chromatography.
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DOI：
10.1002/jssc.201300897
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发表时间：
2013-12
影响因子：
3.1
通讯作者：
Sun, Wenji
中科院分区：
文献类型：
--
作者：
Liang, Jinru;Ito, Yoichiro;Zhang, Xinxin;He, Jiao;Sun, Wenji
关键词：
采用微波辅助萃取-高速逆流色谱法对藏药粗茎龙胆中的6种活性成分进行了制备性分离，包括马钱酸（I）、异orientin-4 '-O-葡萄糖苷（II）、6'-O-β-D-吡喃葡萄糖基龙胆苦苷（III）、当药苦苷（IV）、龙胆苦苷（V）、当药苦苷（VI）。采用星点设计-效应面法对微波辅助萃取工艺参数进行了预测。即5.0g干根;粗茎龙胆用50 mL 57.5%乙醇水溶液在630 W下提取3.39 min，提取物（龙胆总苷）经高速逆流色谱分离，色谱柱为正丁醇/乙酸乙酯/甲醇/1%乙酸水（7.5：0.5：0.5：3.5，v/v/v/v），上相为移动的，采用尾-头洗脱模式。16.3从500 mg原始样品在一次操作中获得高纯度的化合物I-VI 10 mg、8.8 mg、12.8 mg、25.1 mg、40.7 mg和21.8 mg。分离组分的纯度和身份使用HPCL与光电二极管阵列检测和四极杆飞行时间MS和NMR光谱法进行确认。结果表明，响应面法优化提取工艺简便、预测性强，微波辅助萃取-高速逆流色谱联用技术可作为民族药中植物化学成分的快速提取分离方法。
A rapid method combining microwave-assisted extraction and high-speed counter-current chromatography was applied for preparative separation of six bioactive compounds including loganic acid (I), isoorientin-4'-O-glucoside (II), 6'-O-β-d-glucopyranosyl gentiopicroside (III), swertiamarin (IV), gentiopicroside (V), sweroside (VI) from traditional Tibetan medicine Gentiana crassicaulis Duthie ex Burk. Microwave-assisted extraction parameters were predicted by central composite design-response surface methodology. That is, 5.0 g dried roots of G. Crassicaulis was extracted with 50 mL 57.5% aqueous ethanol under 630 W for 3.39 min. The extract (gentian total glycosides) was separated by high-speed counter-current chromatography with n-butanol/ethyl acetate/methanol/1% acetic acid water (7.5:0.5:0.5:3.5, v/v/v/v) using upper phase mobile in tail-to-head elution mode. 16.3 mg, 8.8 mg, 12.8 mg, 25.1 mg, 40.7 mg and 21.8 mg of compounds I–VI were obtained with high purities in one run from 500 mg of original sample. The purities and identities of separated components were confirmed using HPCL with photo diode array detection and quadrupole time-of-flight MS and NMR spectroscopy. The study reveals that response surface methodology is convenient and highly predictive for optimizing extraction process, microwave-assisted extraction coupled with high-speed counter-current chromatography could be an expeditious method for extraction and separation of phytochemicals from ethnomedicine.
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