摘要
目的建立硅胶柱色谱结合高速逆流色谱(HSCCC)法分离纯化丹参中丹参酮的方法。方法丹参粗提物经硅胶柱色谱分离,得到组分F1、F2,分别采用石油醚-醋酸乙酯-甲醇-水(4∶3∶4∶2)、(8∶5∶8∶3)的溶剂系统进行HSCCC分离,下相为流动相,体积流量2.0 mL/min,转速850 r/min,检测波长254 nm,所得产物采用ESI-MS、NMR进行结构鉴定。结果 80 mg组分F1分离得到丹参酮I(14 mg)、二氢丹参酮I(22 mg)、丹参酮IIA(26 mg);80 mg组分F2分离得到二氢丹参酮(11 mg)、三叶鼠尾酮B(15 mg)、隐丹参酮(30 mg);6个化合物进行HPLC分析,质量分数均大于96%。结论硅胶柱色谱结合HSCCC是一种有效的分离制备丹参酮的方法。
Objective To develop a method for separation and purification of tanshinone from Salvia miltiorrhiza by combination of silica gel and high-speed counter-current chromatography（HSCCC）.Methods The crude extract of S.miltiorrhiza was separated by silica gel chromatography and F1 and F2 were obtained.Then,F1 and F2 were separated by HSCCC with a two-phase solvent system composed of petroleum ether-methanol-water（4：3：4：2 and 8：5：8：3）,respectively.The lower phase was used as the mobile phase with a flow rate of 2.0 mL/min,while the apparatus rotated at 850 r/min and the eluates were detected at 254 nm.The structures of the target compounds were identified by ESI-MS and NMR.Results From 80 mg of F1,three compounds with tanshinone I（14 mg）,dihydrotanshinone I（22 mg）,and tanshinone IIA（26 mg） were obtained.And from 80 mg of F2,dihydrotanshinone（11 mg）,trijuganone B（15 mg）,and cryptotanshinone（30 mg） were obtained.The purities of these six compounds determined by HPLC were all over 96%,respectively.Conclusion Combination of silica gel and HSCCC is an efficient method for separation of tanshinone from S.miltiorrhiza
出处
《中草药》
CAS
CSCD
北大核心
2011年第3期466-469,共4页
Chinese Traditional and Herbal Drugs
基金
国家自然科学基金资助项目(20872083)
山东省科技攻关项目(2010GSF10287)
山东大学高校院所自主创新计划(201004011)
关键词
丹参
高速逆流色谱(HSCCC)
硅胶柱色谱
丹参酮
二氢丹参酮
隐丹参酮
Salvia miltiorrhiza Bunge
high-speed counter-current chromatography （HSCCC）
silica gel chromatography
tanshinone
dihydrotanshinone
cryptotanshinone
