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Method for preparing salvianolic acid A by catalytically converting salvianolic acid B

A technology of salvianolic acid and displacement chromatography, applied in the field of catalytic conversion of salvianolic acid B to prepare salvianolic acid A, can solve the problems of low conversion rate, increased equipment investment, reagent and artificial energy consumption, low separation and purification yield, etc. , to achieve the effect of increasing the yield and shortening the time of the fragile state

Inactive Publication Date: 2011-10-12
SUZHOU LEINA PHARMA RES DEV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] 1. Metal ions (such as iron, copper, aluminum, calcium, etc.) in the water extract will aggravate the destruction of salvianolic acid B and Dan A during the conversion process, seriously affecting the yield of Dan A;
[0008] 2. The affinity between salvianolic acid A and pseudo-colloidal impurities is greater than that of salvianolic acid B, which will increase the difficulty of subsequent separation;
[0010] 4. If the conversion volume is too large, it will increase equipment investment, reagent and artificial energy consumption
[0013] In summary, although the technology of heat treatment of salvia miltiorrhiza extract to prepare salvianolic acid A has basically solved the problem of the source of salvianolic acid A, it still has the problems of low conversion rate, unfavorable separation and purification and low yield of separation and purification.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Step 1: Resin Treatment

[0039] Put the ADS-5 and HPD100 macroporous adsorption resins used in this process into their respective chromatographic columns → add acetone to submerge the resin → vacuum degas → elute with acetone until the outflow of acetone is clear → elute with 95% ethanol until the outflow of ethanol without adding water Turbidity is the standard → eluted with deionized water until the effluent has no alcohol smell (generally 5 column volumes for elution) → soak in 4% NaOH overnight → eluted with 4% NaOH for 2 column volumes (BV) → wash with deionized water Remove to neutral → 4% HCl soak overnight → 4% HCl elution 2BV → deionized water elution to neutral (both flow rates are 2cm / min).

[0040] Step 2: Extraction of salvianolic acid B

[0041] Salvia miltiorrhiza (containing salvianolic acid B 6.1%)→dried, crushed and sieved (40 mesh, 40 kg)→water extraction (100°C, 480L×3)→water extract (2318 grams of salvianolic acid B, content 11.36%) , the total s...

Embodiment 2

[0047] Step 4: Crude salvianolic acid B (2.8g, 65.3% SB) → dissolve in 180mL water → add urea (0.08g, about 0.5 moles of salvianolic acid B) → dissolve → transform at 120°C for 4 hours → reduce to room temperature → Adjust pH to 3.0→salvianolic acid B conversion liquid [2.9 grams of solid total weight, containing 19% of salvianolic acid A, 0.56 grams in total, yield 30% (conversion rate 45%)].

[0048] Other steps are with embodiment 1.

Embodiment 3

[0050] Step 4: Crude salvianolic acid B (2.8g, 65.3% SB) → dissolve in 180mL water → add urea (0.05g, about 0.3 moles of salvianolic acid B) → dissolve → transform at 110°C for 4 hours → drop to room temperature → Adjust pH to 3.0→salvianolic acid B conversion solution [2.82 grams of solid total weight, containing 8.86% of salvianolic acid A, 0.25 grams in total, yield 13.67% (conversion rate 20%)].

[0051] Other steps are with embodiment 1.

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PUM

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Abstract

The invention discloses a method for preparing salvianolic acid A by catalytically converting salvianolic acid B. The method is characterized in that the converted raw material is a salvia miltiorrhiza aqueous extract (salvianolic acid B=>50%) primarily purified through combined chromatography; the concentration of the raw material salvianolic acid B is 0.5-2%; urea is taken as the catalyst; the mole ratio of urea to the salvianolic acid B is 0.3-0.7; the conversion reaction temperature is 100-125 DEG C; and the reaction time is 3-6 hours. The method has the following beneficial effects: urea is taken as the catalyst, thus greatly shortening the time for which the salvianolic acid B is in easily destroyed state and remarkably increasing the yield of the salvianolic acid A; the primarily purified salvia miltiorrhiza extract is taken as the converted raw material, thus not only removing the metal ions which are not beneficial to conversion but also removing most colloid-like impurities and frontal impurities which are not beneficial to following separation of the salvianolic acid; and the directional conversion rate of the salvianolic acid B to the salvianolic acid A prepared by the method is not less than 10% and even reaches 60%.

Description

technical field [0001] The invention relates to a method for preparing salvianolic acid A by catalytic conversion of salvianolic acid B. Background technique [0002] Salvia miltiorrhiza is the basic treatment drug for cardiovascular and cerebrovascular diseases in my country. Due to its definite curative effect, Danshen has become the traditional Chinese medicine with the largest consumption (15,000 tons / year), the highest sales, and the largest number of preparation factories in China (960 preparation factories, and the main dosage forms are: Danshen Dropping Pills, Danshen Injection, Danshen Tablets, Danshen Granules, Danshen Granules and Danshen Capsules), in addition, Danshen is also used in the treatment of pulmonary heart disease, hyperlipidemia, hyperviscosity syndrome, asthma, Bronchopneumonia, hepatitis, liver cirrhosis, nephrotic syndrome, arthritis, diabetic circulatory disorders, various bacterial and viral infections, anti-endotoxin, tumor, scleroderma, dermatiti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/732C07C67/317
Inventor 何克江刘珂韩飞陈栋刘军锋张祁
Owner SUZHOU LEINA PHARMA RES DEV
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