阅读说明：本技术 一种多级逆流萃取法精制丹参酮iia工艺 (Process for refining tanshinone IIA by multistage countercurrent extraction method ) 是由 吴学文 谢欢欢 史姣雯 欧阳小玉 粟寒星 李维 曹旭媛 熊艳 于 2020-06-09 设计创作，主要内容包括：本发明公开了一种多级逆流萃取法精制丹参酮IIA的工艺。其采用以下步骤制备而得：将丹参粗粉混悬于水溶液中(B相),呈一定浓度,置入多级逆流萃取罐中,以有机溶剂作为萃取相(S相),调节S相和B相流速,利用多级逆流萃取方式对丹参中的丹参酮IIA进行萃取,回收S相溶剂,得到红色固体,即为丹参酮IIA粗粉。本发明采用多级逆流萃取工艺,确保各物料与溶剂充分接触,保持了较大的浓度差,加快了萃取速率,节约了溶剂用量。此外,操作温度为室温,保证热不稳定性成分不分解,节省能耗,降低了萃取成本,提高了丹参酮IIA萃取效率。(The invention discloses a process for refining tanshinone IIA by a multistage countercurrent extraction method. The preparation method comprises the following steps: suspending the red sage root coarse powder in an aqueous solution (phase B) to a certain concentration, placing the red sage root coarse powder in a multistage countercurrent extraction tank, taking an organic solvent as an extraction phase (phase S), adjusting the flow rate of the phase S and the phase B, extracting tanshinone IIA in the red sage root by using a multistage countercurrent extraction mode, recovering an S phase solvent to obtain red solid, namely the tanshinone IIA coarse powder. The invention adopts a multi-stage countercurrent extraction process, ensures that all materials are fully contacted with the solvent, keeps larger concentration difference, accelerates the extraction rate and saves the dosage of the solvent. In addition, the operation temperature is room temperature, so that the thermal instability components are not decomposed, the energy consumption is saved, the extraction cost is reduced, and the extraction efficiency of the tanshinone IIA is improved.)

1. A process for refining tanshinone IIA by a multistage countercurrent extraction method is characterized by comprising the following steps: suspending Saviae Miltiorrhizae radix coarse powder in water solution (B phase) to a certain concentration, placing in a countercurrent extraction tank, adjusting flow rate of S phase and B phase with organic solvent as extractant (S phase), extracting tanshinone IIA in Saviae Miltiorrhizae radix by multistage countercurrent extraction process, volatilizing solvent, and drying to obtain red solid.

2. The process for refining tanshinone IIA by multistage countercurrent extraction as claimed in claim 1, wherein: the concentration of the red sage root coarse powder is 5-100 mg/mL.

3. The process for refining tanshinone IIA by multistage countercurrent extraction as claimed in claim 1, wherein: the S phase is organic solvent immiscible with water, such as ethyl acetate, chloroform, dichloromethane, n-butanol, etc., preferably ethyl acetate.

4. The process for refining tanshinone IIA by multistage countercurrent extraction as claimed in claim 1, wherein: the phase B solvent is water or alkaline aqueous solution, such as tap water, purified water, sodium bicarbonate aqueous solution, sodium carbonate aqueous solution, sodium hydroxide aqueous solution, lime aqueous solution, etc., preferably alkaline aqueous solution.

5. The process for refining tanshinone IIA by multistage countercurrent extraction as claimed in claim 1, wherein: the phase ratio is S phase (extractant): phase B (crude solvent) =1:5-5: 1.

6. The process for refining tanshinone IIA by multistage countercurrent extraction as claimed in claim 1, wherein: the countercurrent extraction mode is multistage, and the stage number can be single stage, two stages, three stages, four seasons, five stages and the like.

Technical Field

The invention belongs to the technical field of natural extract extraction and the field of medicines, and particularly relates to a process for refining tanshinone IIA by using a multistage countercurrent extraction method, which is applied to the field of medical health.

Background

Salvia miltiorrhiza is the dried root and rhizome of Salvia miltiorrhiza belonging to Labiatae, and is the most common Chinese medicine for promoting blood circulation and removing blood stasis in clinic. Salvia miltiorrhiza also has the effects of stimulating menstrual flow, relieving pain, clearing away heart-fire, relieving restlessness, cooling blood and resolving carbuncle. The salvia miltiorrhiza is applied to Chinese patent medicine preparations for treating cardiovascular diseases, such as tablets, capsules, granules and injection, has the functions of expanding blood vessels, reducing blood pressure and resisting thrombus, and has obvious curative effects on treating coronary heart disease, angina and tachycardia. Wherein tanshinone IIA is dissolved in organic solvent such as ethanol, acetone, diethyl ether, benzene, etc., and is slightly soluble in water. The extraction of tanshinone IIA has attracted great attention, and although a large number of literature reports exist on the extraction of tanshinone IIA, how to greatly improve the purity of tanshinone IIA is not high, which is the direction of development and research of related technicians.

In clinical practice, the traditional Chinese medicine salvia miltiorrhiza has been widely applied to the treatment of cardiovascular and cerebrovascular diseases and stroke diseases. Tanshinone IIA has potential therapeutic effect on cardiovascular disease, cerebrovascular disease, tumor, leukemia, etc.

Aiming at the low content of tanshinone IIA extracted from Salvia miltiorrhiza, the invention provides a process for refining tanshinone IIA by using a multi-stage countercurrent extraction method.

Disclosure of Invention

Aiming at the low content of tanshinone IIA extracted from Salvia miltiorrhiza, the invention provides a process for refining tanshinone IIA by using a multi-stage countercurrent extraction method.

The invention is realized by adopting the following technical scheme:

a process for refining tanshinone IIA by using a multistage countercurrent extraction method comprises the following steps: suspending Saviae Miltiorrhizae radix coarse powder in aqueous solution (phase B), placing into a multistage countercurrent extraction tank, taking organic solvent as extractant (phase S), adjusting flow rate of phase S and phase B, extracting and purifying tanshinone IIA in Saviae Miltiorrhizae radix by multistage countercurrent extraction, recovering solvent of phase S, and obtaining red solid.

In order to detect the content of tanshinone IIA in the tanshinone IIA extract, the content and purity of the extract are measured by the method, and the measuring method comprises the following steps:

chromatographic conditions and system applicability test, the chromatographic column is ODSC18 column; water-acetonitrile (20: 80) is used as a mobile phase; the detection wavelength is 272 nm; flow rate: 1.0 mL/min.

Preparation of a reference stock solution: accurately weighing 10.0 mg of tanshinone IIA reference substance dried under reduced pressure for 24 h, placing in a 10 mL brown volumetric flask, adding mobile phase for dissolving, fixing volume to scale, and shaking to obtain tanshinone IIA reference substance stock solution.

And (3) sample determination: precisely sucking 20 μ L of sample solution, injecting into high performance liquid chromatograph, and measuring by the method.

The invention has the following advantages:

the invention adopts the countercurrent extraction process, maintains larger concentration difference, increases the extraction driving force, accelerates the extraction rate, saves the solvent consumption, has low extraction temperature, ensures that the thermal unstable components are not decomposed by low-temperature extraction, saves energy consumption, greatly reduces the extraction cost, improves the concentration of the effective components in the final solvent, and improves the extraction efficiency of the tanshinone IIA. The organic solvent is adopted for extraction, so that the workload of subsequent separation and concentration procedures is reduced, the production period of products is shortened, the labor production efficiency is greatly improved, and the energy consumption is reduced.

Compared with the prior art, the method for purifying the tanshinone IIA extract disclosed by the invention is different from the method for purifying the tanshinone IIA extract by adopting resin purification or preparative chromatography and the like reported in general literatures, has the advantages of simplicity and effectiveness in operation, easiness in industrialization and the like, and can effectively avoid the use of organic reagents which are toxic and harmful to human bodies. The purified tanshinone II A extract is more beneficial to exerting the pharmacological activity and eliminating the side effect of ineffective impurities.

The invention adopts low-cost organic solvent as the purification reagent, improves the content of tanshinone IIA higher than other reagents, and greatly reduces the process cost.

Detailed Description

The following examples are intended to further illustrate the invention, but are not intended to limit the invention.