高速逆流色谱法从丹参中提取和制备丹参酮。

Extraction and preparative purification of tanshinones from Salvia miltiorrhiza Bunge by high-speed counter-current chromatography.

机构信息

College of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Jul 1;879(21):1899-904. doi: 10.1016/j.jchromb.2011.05.014. Epub 2011 May 14.

DOI:10.1016/j.jchromb.2011.05.014

PMID:21621488

Abstract

A method for extraction and preparative separation of tanshinones from Salvia miltiorrhiza Bunge was successfully established in this paper. Tanshinones from Salvia miltiorrhiza Bunge were extracted using ethyl acetate as the extractant under reflux. The extracts were then purified by high speed counter-current chromatography (HSCCC) with light petroleum-ethyl acetate-methanol-water (6:4:6.5:3.5, v/v) as the two phase solvent system. The upper phase was used as the stationary phase and the lower phase as the mobile phase. 8.2mg of dihydrotanshinone I, 5.8 mg of 1,2,15,16-tetrahydrotanshiquinone, 26.3mg of cryptotanshinone, 16.2mg of tanshinone I, 25.6 mg of neo-przewaquinone A, 68.8 mg of tanshinone IIA and 9.3mg of miltirone were obtained from 400mg of extracts from Salvia miltiorrhiza Bunge in one-step HSCCC separation, with the purity of 97. 6%, 95.1%, 99.0%, 99.1%, 93.2%, 99.3% and 98.7%, respectively, as determined by HPLC area normalization method. Their chemical structures were identified by ¹H NMR.

摘要

本文成功建立了从丹参中提取和制备分离丹参酮的方法。丹参酮采用乙酸乙酯作为回流提取剂进行提取。提取物然后通过高速逆流色谱（HSCCC）进行纯化，以轻石油-乙酸乙酯-甲醇-水（6:4:6.5:3.5，v/v）为两相溶剂系统。上相作为固定相，下相作为流动相。从 400mg 丹参提取物中，一步 HSCCC 分离可得到 8.2mg 二氢丹参酮 I、5.8mg 1,2,15,16-四氢丹参醌、26.3mg 隐丹参酮、16.2mg 丹参酮 I、25.6mg 新隐丹参酮 A、68.8mg 丹参酮 IIA 和 9.3mg 丹参酮甲酯，纯度分别为 97.6%、95.1%、99.0%、99.1%、93.2%、99.3%和 98.7%，均通过 HPLC 面积归一化法测定。通过 1H NMR 鉴定了它们的化学结构。