pH-区带精制逆流色谱分离纯化丹参中的丹酚酸B

doi:10.3969/j.issn.0253-2417.2015.06.008

林产化学与工业 ›› 2015, Vol. 35 ›› Issue (6): 47-52.doi: 10.3969/j.issn.0253-2417.2015.06.008

pH-区带精制逆流色谱分离纯化丹参中的丹酚酸B

刘浩^1,2, 杭伟¹, 陈义伦², 王晓^1,2, 刘伟¹

1.中药质量控制技术重点实验室;山东省分析测试中心, 山东济南 250014;
2.山东农业大学食品科学与工程学院, 山东泰安 271018

收稿日期:2014-11-05 出版日期:2015-12-25 发布日期:2015-12-28
通讯作者: 刘伟,副研究员,博士,从事中药资源研究;E-mail:liuwei0074@163.com E-mail:liuwei0074@163.com
作者简介:刘浩(1990—),男,山东泰安人,硕士,从事天然产物化学研究
基金资助:
国家自然科学基金资助项目(81102749,81130070)

Preparation of Salvianolic Acid B from Salvia miltiorrhiza Bunge by pH-Zone-refining Counter-current Chromatography

LIU Hao^1,2, HANG Wei¹, CHEN Yi-lun², WANG Xiao^1,2, LIU Wei¹

1. Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Jinan 250014, China;
2. College of Food Science and Engineering, Shandong Agriculture University, Tai'an 271018, China

Received:2014-11-05 Online:2015-12-25 Published:2015-12-28

摘要/Abstract

摘要： 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。

关键词: 丹酚酸B, 迷迭香酸, 紫草酸单甲酯, 高速逆流色谱

Abstract: 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), ¹H nuclear magnetic resonance (¹H NMR) and ¹³C nuclear magnetic resonance (¹³C NMR).

Key words: salvianolic acid B, rosmarinic acid, methyl lithospermate, pH-zone-refining countercurrent chromatography

中图分类号:

TQ35

刘浩, 杭伟, 陈义伦, 王晓, 刘伟. pH-区带精制逆流色谱分离纯化丹参中的丹酚酸B[J]. 林产化学与工业, 2015, 35(6): 47-52.

LIU Hao, HANG Wei, CHEN Yi-lun, WANG Xiao, LIU Wei. Preparation of Salvianolic Acid B from Salvia miltiorrhiza Bunge by pH-Zone-refining Counter-current Chromatography[J]. Chemistry and Industry of Forest Products, 2015, 35(6): 47-52.

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pH-区带精制逆流色谱分离纯化丹参中的丹酚酸B

Preparation of Salvianolic Acid B from Salvia miltiorrhiza Bunge by pH-Zone-refining Counter-current Chromatography

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