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Extraction, purification and preparation method of high-purity salvianolic acid B

A purification method and technology of salvianolic acid, which are applied in the field of preparation of high-purity salvianolic acid B extraction and separation, can solve the problems of reduced extraction rate of salvianolic acid B, increased impurities, and less sample amount, and achieve improved dissolution rate and Extraction efficiency, simple extraction method, less damage or loss

Active Publication Date: 2012-02-15
GUANGZHOU HANFANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The deficiencies in the prior art of extraction and separation of salvianolic acid B are mainly manifested in: the extraction process is mainly based on thermal extraction, and the heated salvianolic acid B is prone to degradation, resulting in a decrease in the extraction rate of salvianolic acid B, and an increase in impurities. The Difficulty of Purifying Salvianolic Acid B
The use of alcohol precipitation or flocculant in the impurity removal process will cause a large loss of salvianolic acid B; the use of organic solvents for extraction is easy to produce emulsification, and the amount of organic solvents used is large, which not only increases the cost, but also avoids the residue of organic solvents
Finally, the refined part is purified, using semi-preparative countercurrent chromatography and preparative high-performance liquid chromatography separation technology. Although salvianolic acid B with a content of 95% and above has been obtained, the sample volume of these two technologies is small and the equipment requirements are high. In the laboratory stage, it is difficult to achieve industrialized mass production

Method used

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  • Extraction, purification and preparation method of high-purity salvianolic acid B
  • Extraction, purification and preparation method of high-purity salvianolic acid B
  • Extraction, purification and preparation method of high-purity salvianolic acid B

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035]1. Extraction: take 500g of Danshen medicinal material crushed into fine powder, add 10 times the volume (V / W) of 60% ethanol, soak at 5°C for 24 hours, and then ultrasonically extract for 30 minutes. During the extraction process, use circulating water to cool and control the temperature of the extract Centrifuge at no more than 20°C, and recover ethanol from the extract until it has no alcohol smell.

[0036] 2. Adsorption and separation of macroporous resin: the clarified non-alcoholic extract is placed on a D-101 macroporous resin column, and the ratio of the loaded sample (calculated based on the dry weight of the original medicinal material) to the amount of resin is 1:2 (W / V). Impurities were first eluted with 2 column volumes of water, and then 5 column volumes of 30% ethanol aqueous solution.

[0037] 3. Industrial chromatographic column chromatography: the eluted part of macroporous resin with 30% ethanol aqueous solution is concentrated to remove alcohol, and ...

Embodiment 2

[0040] Same as Example 1, the difference is that the medicinal material is added with 12 times the volume (V / W) of ethanol aqueous solution, and finally salvianolic acid B with a purity of 91.5% is obtained.

Embodiment 3

[0042] Same as Example 1, the difference is that the medicinal material is added with 15 times the volume (V / W) of the ethanol aqueous solution of the medicinal material, and finally salvianolic acid B with a purity of 92.5% is obtained.

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Abstract

The invention discloses an extraction, purification and preparation method of high-purity salvianolic acid B. The method comprises the following steps: (1) smashing a salvia miltiorrhiza medical material into fine powder, and screening with a sieve of 20-60 meshes; (2) adding an ethanol solution, soaking at the temperature below 5 DEG C, and carrying out ultrasonic extraction, wherein the extraction process temperature is controlled below 25 DEG C; (3) centrifuging extract, filtering, recovering ethanol at reduced pressure until the extract has no alcohol odor, concentrating the extract and filtering; (4) clarifying the extract, enriching through macroporous resin, and purifying through chromatographic column chromatography so as to obtain salvianolic acid B fraction; and (5) carrying out vacuum drying or freeze drying so as to obtain extractive. In the new process disclosed by the invention, cost is low, only ethanol is used as an organic solvent, and more than 90% of salvianolic acid B can be obtained through separation and purification, thus the method disclosed by the invention is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method for extracting and separating high-purity salvianolic acid B. Background technique [0002] Salvia miltiorrhiza is a plant in the labiatae family Salvia miltiorrhiza ( Salvia million rhiza The dried roots and rhizomes of Bge) mainly have the effects of dispelling blood stasis and relieving pain, promoting blood circulation and regulating menstruation, nourishing blood and calming the nerves, and are widely used in the treatment of cardiovascular diseases. [0003] The important active components of Salvia miltiorrhiza are water-soluble salvianolic acids, and salvianolic acids are mainly represented by salvianolic acid B. Pharmacological studies have shown that salvianolic acid B has strong pharmacological effects in scavenging oxygen free radicals, protecting heart and brain ischemia-reperfusion injury, resisting lipid peroxidation, and reducing liver tissue fibrosis. Its molecular formula is C 36 h ...

Claims

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Application Information

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IPC IPC(8): C07D307/86
Inventor 汪涛李金华刘忠云葛发欢许定舟黄裕杨丽钟鸣张聪琪
Owner GUANGZHOU HANFANG PHARMA
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