Rapid identification and preparative isolation of antioxidant components in licorice
Rapid identification and preparative isolation of antioxidant components in licorice
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DOI：
10.1002/jssc.200900620
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发表时间：
2010-03-01
影响因子：
3.1
通讯作者：
Lim, Soon Sung
中科院分区：
文献类型：
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作者：
Lee, Yeon Sil;Kim, Seon Ha;Lim, Soon Sung
本研究采用在线HPLC-2,2'-azinobis-(3-乙基苯并噻唑啉-6-磺酸根阳离子(ABTS(+.)))生物测定法快速测定甘草提取物中的抗氧化化合物。通过测量734 nm吸光度的下降来监测ABTS自由基清除检测系统的负峰，表明存在抗氧化活性。基于ABTS(+)的抗氧化活性谱显示三个峰表现出抗氧化活性，然后成功地应用制备级高速逆流色谱技术从甘草提取物中一步分离出三个峰。使用由正己烷-乙酸乙酯-甲醇-水(6.5:5.5:6:4，v/v)组成的两相溶剂体系进行高速逆流色谱，得到三个峰的产率，纯化后的脱氢甘草素C（I，纯度95.1%）、脱氢甘草素D（II，纯度96.2%）和异安古斯酮A（III，纯度99.5%）的化学结构分别为10.33%、10.43%和6.7%。 A(III)通过ESI-MS以及H-1-和C-13-NMR分析进行鉴定。
This study employed the online HPLC-2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonate radical cation (ABTS(+.)) bioassay to rapidly determine antioxidant compounds occurring in the licorice extract of Glycyrrhiza uralensis. The negative peaks of the ABTS radical scavenging detection system, which indicated the presence of antioxidant activity, were monitored by measuring the decrease in absorbance at 734 nm. The ABTS(+)-based antioxidant activity profile showed that three peaks exhibited antioxidant activity, and then the high-speed counter-current chromatography technique of preparative scale was successfully applied to separate the three peaks I-III in one step from the licorice extract. The high-speed counter-current chromatography was performed using a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (6.5:5.5:6:4, v/v). Yields of the three peaks, dehydroglyasperin C (I, 95.1% purity), dehydroglyasperin D (II, 96.2% purity), and isoangustone A (III, 99.5% purity), obtained were 10.33, 10.43, and 6.7% respectively. Chemical structures of the purified dehydroglyasperin C (I), dehydroglyasperin D (II), and isoangustone A (III) were identified by ESI-MS and H-1- and C-13-NMR analysis.