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Preparative Separation and Purification of Liquiritin and Glycyrrhizic Acid from Glycyrrhiza uralensis Fisch by High-Speed Countercurrent Chromatography.
Journal of Chromatographic Science ( IF 1.5 ) Pub Date : 2020-08-31 , DOI: 10.1093/chromsci/bmaa050
Hao Wang 1 , Hu Shan 2 , Haitao Lü 1
Affiliation  

The technique of high-speed countercurrent chromatography (HSCCC) was applied to the preparative isolation and purification of liquiritin and glycyrrhizic acid from a crude extract of Glycyrrhiza uralensis Fisch for the first time. Using single factor and orthogonal design experiments, the best extraction conditions were 70% ethanol, 1:25 ratio of solid-to-liquid (w/v) and extracted 1.5 h at 80°C. The contents of liquiritin and glycyrrhizic acid in the crude extract were 1.3 and 5.3%, respectively. Using the two-phase solvent system of ethyl acetate–methanol–water (5:2:5, v/v), 6.0 mg liquiritin (the purity was 96.7%, and the recovery was 89.3%), and 20.5 mg glycyrrhizic acid (the purity was 98.9%, and the recovery was 77.1%) were obtained from 500 mg crude extraction by HSCCC, respectively. The retention rate of stationary phase was 51.0%. Their structures were identified by high-performance liquid chromatography, melting points, ultraviolet radiation, Fourier transform infrared (FTIR), Electrospray ionization mass spectrometry (ESI-MS), 1H Nuclear Magnetic Resonance (NMR) and 13C NMR spectra. The scavenging abilities of glycyrrhizic acid to 1,1-diphenyl-2-picrylhydrazyl and hydroxyl free radicals were stronger than those of liquiritin.

中文翻译:

高速逆流色谱法从甘草中分离和纯化甘草酸和甘草酸。

高速逆流色谱(HSCCC)技术用于甘草粗提液中甘草酸和甘草酸的制备分离纯化第一次是Fisch。使用单因素和正交设计实验,最佳提取条件为70%乙醇,固液比1:25(w / v),并在80°C提取1.5 h。粗提物中的液体白蛋白和甘草次酸的含量分别为1.3%和5.3%。使用乙酸乙酯-甲醇-水(5:2:5,v / v)的两相溶剂系统,6.0 mg液体白蛋白(纯度为96.7%,回收率为89.3%)和20.5 mg甘草酸(从500毫克HSCCC粗提物中分别获得98.9%的纯度和77.1%的回收率。固定相的保留率为51.0%。通过高效液相色谱,熔点,紫外线,傅立叶变换红外(FTIR),电喷雾电离质谱(ESI-MS),1 H核磁共振(NMR)和13 C NMR光谱。甘草酸对1,1-二苯基-2-吡咯并肼基和羟基自由基的清除能力强于甘草酸。
更新日期:2020-09-29
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