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Method for preparing high-purity tanshinoneIIA

A tanshinone and high-purity technology is applied in the field of preparation of high-purity tanshinone IIA, which can solve problems such as harm to health, complicated operation, and excessively long process flow, so as to reduce the harm of operators, simplify operation procedures, and reduce environmental pollution. Effect

Inactive Publication Date: 2008-06-18
上海朗萨医药科技有限公司
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

[0003] However, as one of the main active ingredients, Tanshinone IIA generally has problems such as low yield, large solvent consumption, and high energy consumption in the currently commonly used extraction and separation methods. It is reported that after extraction with a certain concentration of ethanol to obtain the extract, the water-soluble components in the extract are washed away with hot water, and then the purer monolayer is separated by alumina column chromatography with benzene and other organic solvents. Body Composition [Wang Qingwei, Yang Pin, Zhang Liwei. Effective Separation of Tanshinone. Journal of Shanxi University (Natural Science Edition), 1994, 17(3): 294-298]
Due to the complex operation and many steps of this method, and the solvent used is highly toxic, it pollutes the environment and endangers people's health. application
There are also reports of extracting Danshen with ethanol to obtain extract, then dissolving in methanol to remove insoluble impurities, and separating methanol solubles with Sephadex LH-20 to obtain Tanshinone IIA [Dong Rui, Zheng Yinan. Separation and identification of tanshinone components in Danshen. Jilin Journal of Normal University (Natural Science Edition), 2004, 5(2): 100-104], but because Sephadex LH-20 material is expensive and the sample load is small, it is mostly in the laboratory research stage at present
[0004] Tanshinone IIA, Tanshinone IIB, Tanshinone I, Cryptotanshinone and a series of compounds with very similar chemical structures make the purification of Tanshinone IIA very difficult

Method used

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  • Method for preparing high-purity tanshinoneIIA
  • Method for preparing high-purity tanshinoneIIA

Examples

Experimental program
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Effect test

Embodiment 1

[0039] 1. Extraction of total ketones of salvia miltiorrhiza

[0040] Take 10 kg of Salvia miltiorrhiza (about 1 cm in diameter), add 8 times the amount of 95% ethanol for reflux extraction at 80°C for 2 hours, filter, add 6 times the amount of 95% ethanol for reflux extraction for 2 hours, filter, and combine the filtrates, statically at 2°C Set aside for 24 hours, analyze the gel, filter, concentrate to 8 times the volume of the medicinal materials, slowly add water and stir fully to make the alcohol concentration reach about 50%, stir thoroughly, then stand for 24 hours (2°C), and vacuum filter and dry to obtain the total ketone in vacuum. Add water to the mother liquor to precipitate, let stand for 24 hours (2° C.) and suction filter to dry the total ketones. The yield of total ketones is about 1.05%. The flowchart is shown in Figure 3.

[0041] 2. Isolation of Tanshinone IIA

[0042] The total ketones obtained in the above process are weighed to obtain 105g total ketone...

Embodiment 2

[0044] 1. Extraction of total ketones of salvia miltiorrhiza

[0045] Take 20kg of salvia miltiorrhiza (about 1 cm in diameter), and operate the same process as in Example 1 to obtain 238 g of salvia miltiorrhiza ketones, with a yield of 1.19%.

[0046] 2. Isolation of Tanshinone IIA

[0047] 238g of total ketones obtained in the above process were loaded into the spherical chromatographic system with 5 times the amount of silica gel (wet loading of cyclohexane), and the total ketones and silica gel were mixed 1:1 before sample loading, and added to the bottom flask. An appropriate amount of cyclohexane and dichloromethane 98:2 (volume ratio) mixed solvent is heated to 50°C under vacuum to start eluting, so that the reflux velocity and the velocity of the liquid droplet are balanced, and the ratio of the solvent system is changed after extraction for 5 hours. Cyclohexane and methylene chloride were eluted at a ratio of 95:5, the eluate was concentrated, and recrystallized rep...

Embodiment 3

[0049] 1. Extraction of total ketones of salvia miltiorrhiza

[0050] Take 30kg of salvia miltiorrhiza (about 1 cm in diameter), and operate the same process as in Example 1 to obtain 366 g of salvia miltiorrhiza ketones, with a yield of 1.22%.

[0051] 2. Isolation of Tanshinone IIA

[0052] 366g of total ketones obtained in the above process were loaded into the pear-shaped chromatographic system with 6 times the amount of silica gel (cyclohexane wet loading), and the total ketones and silica gel were mixed 1: 1 before sample loading, and then placed in the bottom flask Add an appropriate amount of cyclohexane and dichloroethane 99:1 (volume ratio) mixed solvent, heat to 50°C under vacuum to start elution, so that the reflux speed and the speed of the droplets are balanced, and the ratio of the solvent system is changed after 5 hours of extraction , eluted with cyclohexane and dichloroethane 97:3, concentrated eluate, and repeated recrystallization with 95% ethanol to obtai...

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Abstract

The invention relates to a preparation method of tanshinone II with high purity. The method comprises the following procedures, firstly the root of Salvia Miltiorrhiza and the rhizome thereof are extracted by alcohols, concentrated and crystallized the colloid, filtered or centrifuged to remove the impurity; secondly, water is added to obtain tanshinone precipitation, and the precipitation is filtered and dried; thirdly, the tanshinone is separated by the positive phase chromatographic analysis and the multi-purpose chromatographic analysis system, the eluent is concentrated and recrystallized to obtain tanshinone II with high purity. The method has the advantages of high yield and purity, low cost and being suitable for the large scale production.

Description

technical field [0001] The invention belongs to the field of preparation methods of tanshinone IIA, in particular to a preparation method of high-purity tanshinone IIA. Background technique [0002] Salvia miltiorrhiza is the dry root and rhizome of Salvia miltiorrhiza Bunge, which has the effects of promoting blood circulation, removing blood stasis, cooling blood and reducing swelling, clearing heart and eliminating troubles. The structure of Tanshinone IIA (Tanshinone IIA, Tan) is shown in Figure 1. It has a relatively high content in Danshen and is one of the main medicinal components. It has potential therapeutic effects on cardiovascular and cerebrovascular diseases, tumors, leukemia, etc., and has attracted scholars at home and abroad. [Li Ruihuan, Wang Ling. Progress in Pharmacological Research of Tanshinone IIA. Modern Journal of Integrated Traditional Chinese and Western Medicine, 2006, 15(23): 3303-3305]. [0003] However, as one of the main active ingredients, T...

Claims

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Application Information

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IPC IPC(8): C07J73/00A61K36/53A61K125/00
Inventor 周长新朱志彬赵霞尹金瑶
Owner 上海朗萨医药科技有限公司
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