TLC Identification and Extraction Process of Rubiasin-1-methyl Ether from Yao Medicine Chuanlianzhu

[Objectives]To establish a thin-layer chromatography(TLC)method for the determination of rubiadin-1-methyl ether in Yao Medicine Chuanlianzhu(Damnacanthus giganteus).[Methods]A silica gel G thin-layer plate was adopted for TLC.Petroleum ether(60-90℃)-chloroform-methanol-water(7:15:3:1)was used as the developing solvent and inspected under ultraviolet lamp(365 nm).The content was determined by Inertsil ODS-3 C 18 column(4.60 mm×250 mm,5μm),mobile phase:acetonitrile-0.2%phosphoric acid gradient elution,detection wavelength 277 nm,flow rate 1.0 mL/min,column temperature 30℃,injection volume 10μL.[Results]The spots of 10 Chuanlianzhu samples from different origins showed the same color at the same position as the control,and the spots were clear and specific.The injection volume of rubiadin-1-methyl ether showed a good linear relationship in the range of 2.90-145μg(R=0.9996).The average recovery rate of rubiadin-1-methyl ether in the low,medium and high dose groups of Yao Medicine Chuanlianzhu was 98.72%,and RSD=1.78%.[Conclusions]This method can effectively identify Yao Medicine Chuanlianzhu medicinal materials and accurately determine the content of rubiadin-1-methyl ether in the medicinal materials.It provides a scientific basis for the development and utilization of Yao Medicine Chuanlianzhu medicinal resources.

海南虎刺枝叶中化学成分及其抗类风湿性关节炎活性研究

目的 研究茜草科虎刺属植物海南虎刺Damnacanthus hainanensis枝叶中的化学成分及其抗类风湿性关节炎活性。方法 综合运用硅胶柱色谱、反相硅胶柱色谱、SephadexLH-20凝胶柱色谱以及制备型HPLC等色谱技术进行系统分离和纯化,根据分离得到化合物的理化性质及其波谱数据,并通过与文献中报道的波谱数据进行比对,鉴定化合物的结构;采用MTS法通过对分离得到化合物的体外抑制滑膜细胞增殖的活性进行测试以评价其抗类风湿性关节炎活性。结果 从海南虎刺枝叶的甲醇提取物中分离得到了18个化合物,分别鉴定为naucleidinal(1)、1,2,3,4-tetrahydronorharman-1-one(2)、19-O-methyl-3,14-dihydroangustoline(3)、latifoliamide B(4)、latifoliamide D(5)、bacilsubteramide A(6)、vinmajine I(7)、naucleofficine D(8)、1-甲氧甲酰-β-咔巴啉(9)、naphthisoxazol A(10)、1,6-dihydroxy-2-methyl-9,10-anthraquinone(11)、rubiadin-1-methylether(12)、1,3,6-trihydroxy-2-methoxymethyl-9,10-anthraquinone(13)、3,6-dihydroxy-2-hydroxymethyl-9,10-anthra quinone(14)、7-羟基色原酮(15)、5,7-二羟基色原酮(16)、6,4’-dihydroxy-3’-methoxyaurone(17)和farnisin(18)。抗类风湿性关节炎活性评价结果表明,化合物11~14、17和18对滑膜成纤维MH7A细胞增殖抑制活性的半数抑制浓度(median inhibition concentration,IC50)值为(8.93±0.09)~(152.58±0.32)μmol/L。结论 所有化合物均为首次从虎刺属植物中分离得到。化合物11~14、17和18表现出了较为显著的抗类风湿性关节炎活性。