Separation of flavonoids from Millettia griffithii with high-performance counter-current chromatography guided by anti-inflammatory activity.
Separation of flavonoids from Millettia griffithii with high-performance counter-current chromatography guided by anti-inflammatory activity.
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DOI：
10.1002/jssc.201401068
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发表时间：
2015-02
影响因子：
3.1
通讯作者：
Huan Tang;Bo Wu;Kai Chen;Heying Pei;Wenshuang Wu;Liang Ma;A. Peng;Haoyu Ye;Li-juan Chen
中科院分区：
文献类型：
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作者：
Huan Tang;Bo Wu;Kai Chen;Heying Pei;Wenshuang Wu;Liang Ma;A. Peng;Haoyu Ye;Li-juan Chen
崖豆藤是我国特有的一种植物，产于云南省南部。迄今为止，还没有关于其植物化学成分及相关生物活性的研究报道。在我们前期的研究中，崖豆藤正己烷粗提物在100 μg/mL浓度下显示出显著的抗炎活性，激发了我们对崖豆藤抗炎活性成分的探索。以正己烷/乙酸乙酯/甲醇/水（8：9：8：9，v/v）为溶剂体系，采用高效逆流色谱法从正己烷粗提物中分离得到4个组分（I、II、III和A），并对其抗炎活性进行了研究。以正己烷/乙酸乙酯/甲醇/水（8：4：8：4，v/v）为溶剂体系，将抑制活性最强的组分A进一步分离，得到另外4个组分（IV，V，VI和B）。化合物V和组分B具有明显的抗炎活性，一氧化氮抑制率分别为80%和65%，值得进一步分离。然后，用由正己烷/乙酸乙酯/甲醇/水（8：1：8：1，v/v）组成的溶剂系统从级分B中分离出三个级分（VII、VIII和IX），其中化合物VIII表现出最强的抑制活性（80%）。最后，化合物V和VIII的IC 50值分别为38.2和14.9 μM。通过电喷雾电离质谱和（1）H和（13）C NMR谱鉴定了结构。
Millettia griffithii is a unique Chinese plant located in the southern part of Yunnan Province. Up to now, there is no report about its phytochemical or related bioactivity research. In our previous study, the n-hexane crude extract of Millettia griffithii revealed significant anti-inflammatory activity at 100 μg/mL, inspiring us to explore the anti-inflammatory constituents. Four fractions (I, II, III, and A) were fractionated from n-hexane crude extract by high-performance counter-current chromatography with solvent system composed of n-hexane/ethyl acetate/methanol/water (8:9:8:9, v/v) and then were investigated for the potent anti-inflammatory activity. Fraction A, with the most potent inhibitory activity was further separated to give another four fractions (IV, V, VI, and B) with solvent system composed of n-hexane/ethyl acetate/methanol/water (8:4:8:4, v/v). Compound V and fraction B exhibited remarkable anti-inflammatory activity with nitric oxide inhibitory rate of 80 and 65%, which was worth further fractionation. Then, three fractions (VII, VIII, and IX) were separated from fraction B with a solvent system composed of n-hexane/ethyl acetate/methanol/water (8:1:8:1, v/v), with compound VIII demonstrating the most potent inhibitory activity (80%). Finally, the IC50 values of compound V and VIII were tested as 38.2 and 14.9 μM. The structures were identified by electrospray ionization mass spectrometry and(1)H and (13)C NMR spectroscopy.