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Separating preparation process of salvianolic acid B

A technology of salvianolic acid and acidic solution, which is applied in the field of preparation and separation of countercurrent chromatography, can solve the problems of low separation efficiency, small amount of sample loading, cumbersome operation, etc., and achieve the effects of saving solvent, no sample loss, and short separation time

Active Publication Date: 2007-07-11
山东蓝城分析测试有限公司
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0003] At present, the separation of salvianolic acid components mostly adopts column chromatography, but the operation is very cumbersome, and the separation efficiency is not high; there are also preparative high-performance liquid phase separations, but the sample volume is too small; high-speed countercurrent chromatography is a A liquid-liquid distribution separation technology, its separation principle is to use the principle of one-way hydrodynamic equilibrium, so that two immiscible solvent phases are distributed in one direction in a high-speed rotating spiral tube, and one of the phases is used as a stationary phase. The constant flow pump transports the sample-laden mobile phase through the stationary phase, and uses the difference in the distribution coefficient (K) of the sample in the two phases to achieve separation

Method used

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  • Separating preparation process of salvianolic acid B
  • Separating preparation process of salvianolic acid B

Examples

Experimental program
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Effect test

Embodiment 1

[0016] Example 1: take 2200 g of Danshen decoction pieces and pulverize them, and then extract with 95% ethanol under reflux for 4 times (each time for 1 h), filter with suction, and concentrate the filtrate under reduced pressure to obtain a concentrate. Add double the amount of water to the concentrated solution, adjust the pH to 7.5 with sodium bicarbonate solution, and extract with ether. The aqueous phase was adjusted to pH 3 with 1 mol / L hydrochloric acid, extracted with diethyl ether, and the diethyl ether was recovered to obtain 57.19 g of the crude extract of Salvia miltiorrhiza in red powder form. This crude extract is separated and prepared salvianolic acid B by the method of the present invention.

[0017] Salvianolic acid B was separated and prepared from the crude extract of Salvia miltiorrhiza by using a semi-preparative countercurrent chromatography with tert-butyl methyl ether and water as the solvent. Firstly, the above-mentioned solvent system was arranged ...

Embodiment 2

[0019] Example 2: Take 1000 g of Danshen decoction pieces and pulverize them, then reflux extract with 80% ethanol for 4 times (1 hour each time), filter with suction, and concentrate the filtrate under reduced pressure to obtain a concentrate. Add double the amount of water to the concentrated solution, adjust the pH to 7.5 with 1mol / L sodium hydroxide solution, and extract with ether. The water phase was adjusted to pH 3 with 1 mol / L dilute sulfuric acid solution, extracted with ether, and the ether was recovered to obtain 25.52 g of the crude extract of Salvia miltiorrhiza in red powder form. This crude extract is separated and prepared salvianolic acid B by the method of the present invention. Salvianolic acid B was separated and prepared from the crude extract of Salvia miltiorrhiza by using a semi-preparative countercurrent chromatograph with tert-butyl methyl ether and water as the solvent. Firstly, the above-mentioned solvent system was arranged in a separatory funnel...

Embodiment 3

[0020]Example 3: take 1000 g of Danshen decoction pieces and pulverize them, then reflux extract with 70% ethanol for 4 times (1 hour each time), filter with suction, and concentrate the filtrate under reduced pressure to obtain a concentrate. Add double the amount of water to the concentrated solution, adjust the pH to 7.5 with sodium bicarbonate solution, and extract with ether. The aqueous phase was adjusted to pH 3 with 1 mol / L hydrochloric acid, extracted with diethyl ether, and the diethyl ether was recovered to obtain 23.13 g of the crude extract of Salvia miltiorrhiza in red powder form. Salvianolic acid B was separated and prepared from the crude extract of Salvia miltiorrhiza by using a semi-preparative countercurrent chromatograph with ether and water as the solvent. Firstly, the above-mentioned solvent system was arranged in a separatory funnel at a volume ratio of 1:2, shaken evenly, and allowed to stand for stratification. After a period of equilibrium, the upper...

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Abstract

The invention discloses a separating method of salviol acid in the salvia miltiorrhizae extract, which is characterized by the following: grinding medicine materical crude slice of radix salvia miltiorrhizae; extracting through alcohol; sucking; decompressing filtrate; condensing; adding water in the condensate; adjusting pH value through alkaline to 7. 5; extracting through ether; adjusting pH value through water to 3; extracting through ether; recycling solvent; obtaining red powder-shaped rough extract of radix salvia miltiorrhizae; applying counter-current chromatographic fractionation method of pH value band to make salviol acid B.

Description

technical field [0001] The invention relates to a preparation and separation method of countercurrent chromatography, in particular to a method for separating and preparing salvianolic acid B from the crude extract of salvia miltiorrhiza by applying pH zone refining countercurrent chromatography. Background technique [0002] Salvia miltiorrhiza is the dry root and rhizome of Salvia miltiorrhiza Bge. The main active components of Danshen are water-soluble salvianolic acid compounds and fat-soluble tanshinone compounds. Salvianolic acid is a kind of water-soluble component with both caffeoyl depsipphenolic acid structure and neolignan skeleton. Modern pharmacological studies have shown that salvianolic acid compounds have a strong antioxidant effect and can remove superoxide in the body. Anions and hydroxyl radicals inhibit lipid peroxidation and improve microcirculation. Among the salvianolic acid compounds, salvianolic acid B is one of the main representative active ingre...

Claims

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Application Information

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IPC IPC(8): C07D307/80A61K36/53A61K125/00
Inventor 王晓刘建华耿岩玲李福伟程传格
Owner 山东蓝城分析测试有限公司
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