pH-区带精制逆流色谱分离纯化丹参中的丹酚酸B

摘要

Salvianolic acid B,rosmarinic acid and methyl lithospermate were successfully separated from the roots of Salvia miltiorrhiza Bunge by pH-zone-refining high speed countercurrent chromatography in one step. The separation was performed with a two-phase system composed of petroleum ether-ethyl acetate-butanol-water(2:3:6:9,the volume ratio). The lower-phase was used as the mobile phase with a flow rate of 2. 0 mL/min,the apparatus rotated at 850 r/min and the effluents were detected at 254 nm. Salvianolic acid B(1 419. 15 mg),rosmarinic acid(171. 25 mg) and methyl lithospermate(52. 34 mg) were obtained from 6 g of the crude sample in one step. Their purities determined by high performance liquid chromatography(HPLC)were 94. 53%,96. 36% and 96. 83%,respectively. The structures of the target compounds was identified by electrospray ionization mass spectrometry ( ESI-MS ) ,1 H nuclear magnetic resonance ( 1 H NMR ) and 13C nuclear magnetic resonance ( 13C NMR) .%建立应用pH-区带高速逆流色谱分离纯化丹参中的丹酚酸B的方法. 以石油醚/乙酸乙酯/正丁醇/水(体积比2:3:6:9)为两相溶剂体系,在流速为2. 0 mL/min,主机转速为850 r/min,检测波长为254 nm的条件下进行分离,从6 g 丹参粗提物中一次性分离制备得到1 419. 15 mg丹酚酸B、171. 25 mg迷迭香酸和52. 34 mg紫草酸单甲酯,高效液相色谱分析纯度分别为94. 53%、96. 36%和96. 83%,通过质谱、核磁共振氢谱和核磁共振碳谱鉴定化合物的结构.