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Method for preparing salvianolic acid A

A technology of salvianolic acid and reaction kettle, which is applied in the field of efficient preparation of active ingredients of traditional Chinese medicine, can solve the problems of slow conversion speed, high cost, and low production efficiency, and achieve the effects of improved reproducibility, simple operation, and complete conversion

Active Publication Date: 2017-02-22
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both the direct preparation method and the indirect conversion method have the disadvantages of low preparation efficiency and slow conversion speed. At the same time, to obtain the components rich in salvianolic acid A needs to combine polyamide chromatography, macroporous resin, silica gel column chromatography and preparative liquid chromatography. Separation is time-consuming and labor-intensive, pollutes the environment, and the sample purity is low, and repeated column chromatography has irreversible adsorption on the sample. technology

Method used

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  • Method for preparing salvianolic acid A
  • Method for preparing salvianolic acid A
  • Method for preparing salvianolic acid A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Such as figure 1 The preparation flow chart of salvianolic acid A monomer is shown.

[0029] Salvianolic acid B ( image 3 ) Use NaHCO with pH 4.0 3 Water was prepared into a 40mg / mL salvianolic acid B solution, and 40mL of the above solution was placed in a 50mL subcritical water stainless steel reactor. After the heating furnace reached 180°C and stabilized, the reactor was placed in the heating furnace and the timing started. After 60 minutes, the reactor was quickly taken out and placed in an ice water bath to cool, the liquid was taken out, freeze-dried, and a crude product rich in salvianolic acid A ( Figure 4 ).

[0030] 2. Separation and purification of salvianolic acid A by high-speed countercurrent chromatography

[0031] The solvent system is petroleum ether: ethyl acetate: n-butanol: water = 2:3:1:9, the upper phase adds 10Mm trifluoroacetic acid as the stationary phase, the lower phase is 10mM ammonia as the mobile phase, and the column volume of the high-speed c...

Embodiment 2

[0040] Use salvianolic acid B with pH 3.5 NaHCO 3 Prepare 45mg / mL salvianolic acid B solution with water, take 40mL of the above solution and place it in a 50mL subcritical water stainless steel reactor. After the heating furnace reaches 182°C and is stable, put the reactor into the heating furnace and start timing. After 55 minutes, the reactor was quickly taken out and placed in an ice-water bath for cooling. The liquid was taken out and freeze-dried to obtain a crude product rich in salvianolic acid A.

[0041] Separation and purification of salvianolic acid A by high-speed countercurrent chromatography

[0042] The solvent system is petroleum ether: ethyl acetate: n-butanol: water = 2:3:1:9, the upper phase adds 10mM trifluoroacetic acid as the stationary phase, the lower phase is 10mM ammonia as the mobile phase, the column volume of the high-speed countercurrent chromatography It is 300mL, the loading volume is 1.0g, the rotating speed is 750rpm, the upper phase is the statio...

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Abstract

The invention discloses a method for preparing salvianolic acid A. The method includes the following steps that firstly, salvianolic acid B is prepared into a solution with the concentration of 35-45 mg / mL by means of NaOH or NaHCO3 with the pH value of 3.5-4.5, the solution is placed in a subcritical water reaction kettle, after the temperature of a heating furnace reaches 170-190 DEG C and is stabilized, the reaction kettle is placed into the heating furnace, the reaction kettle is taken out after 50-70 min and placed in ice water bath or cold water to be cooled, the liquid is taken out and subjected to freeze-drying, and a crude product rich in salvianolic acid A is obtained; secondly, salvianolic acid A is separated and purified by means of high-speed countercurrent chromatography, wherein a solvent system is prepared from petroleum ether, ethyl acetate, n-butyl alcohol and water according to the ratio of 2:3:1:9, 10 mM of trifluoroacetic acid is added to an upper phase to form a stationary phase, 10 mM ammonia water is a lower phase and serves as a mobile phase, the volume of a high-speed countercurrent chromatography column is 200-400 mL, the sample loading amount is 1.0-1.2 g, the rotation speed is 600-1000 rpm, the flow speed is 1-4 mL / min, and the detection wavelength is 280 nm. The method is low in cost, easy to operate and high in efficiency, salvianolic acid crude extracts can be converted on a large scale, and a salvianolic acid A monomeric compound with the purity higher than 98% is separated and prepared.

Description

Technical field [0001] The invention belongs to the technical field of efficient preparation of active ingredients of traditional Chinese medicine, and specifically relates to a preparation method of salvianolic acid A. Background technique [0002] Salvia miltiorrhiza is the dried roots and rhizomes of Salvia miltiorrhizaBge., a plant in the labiatae family. It has the functions of promoting blood circulation and removing blood stasis, regulating menstruation and relieving pain, clearing the heart and removing irritability, cooling blood and eliminating carbuncle. It is used for chest pain, abdominal pain, abdominal pain, accumulation of symptoms, heat pain, upset and insomnia, irregular menstruation, dysmenorrhea, amenorrhea, sore swelling and pain. In recent years, studies have found that Danshen has the functions of dilating coronary artery, resisting platelet aggregation, improving blood circulation, preventing thrombosis and atherosclerotic plaque formation, and promoting t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/333C07C67/58C07C69/732A61P9/10A61P7/02A61P9/08
CPCC07C67/333C07C67/58C07C69/732
Inventor 耿岩玲王岱杰王晓程燕郭兰萍
Owner SHANDONG ANALYSIS & TEST CENT
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