A kind of preparation method of aescin b

A technique of aescin and crystallization, which is applied in the field of preparation of aescin B, can solve the problems of strong stimulating effect, time-consuming process route, large amount of solvent used, etc., and achieves excellent anti-inflammatory, low muscle and mucosal irritation, Addressing the effects of uniformity and safety

Active Publication Date: 2017-11-10
WUHAN AIMIN PHARMA
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  • Description
  • Claims
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Problems solved by technology

[0003] During the long-term use of sodium aescinate, it was found that the drug has a strong stimulating effect on muscles and mucous membranes, and patients are prone to side effects such as phlebitis
However, due to the extremely similar structures of aescin A and aescin monomer B, they are cis-trans isomers of each other, and the separation is very difficult. It has been proved by experiments that reversed-phase silica gel column chromatography can separate aescin monomer A and aescin The separation of phylloside monomer B is almost impossible to achieve, and only a very small amount of aescin monomer B can be barely obtained by greatly prolonging the separation time and using a large amount of elution solvent
Therefore, this process route is time-consuming, laborious, and the amount of solvent used is large, and the yield of aescin B monomer is low, so it is difficult to be used in industrialized production

Method used

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  • A kind of preparation method of aescin b

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) Extraction: take 1 kg of saffron seed powder and extract twice, each time with 10 L of ethanol aqueous solution with a mass concentration of 70%, stir and extract at 45°C for 2 hours, filter, combine the filtrates filtered twice, and rotate and recover under reduced pressure solvent and concentrated to 2L.

[0024] 2) Extraction: adjust the pH of the concentrated solution obtained in step 1) to 2 with 1 mol / L hydrochloric acid, extract 3 times with 2 L of water-saturated n-butanol, combine the organic layers and concentrate to 400 mL;

[0025] 3) The first crystallization: Add the concentrated solution obtained in step 2) into a mixed solvent of 960mL acetone and 240mL methyl tert-butyl ether, heat to reflux under stirring, then cool to 20°C to precipitate a white precipitate, filter, 45°C Dried to obtain 49g of white crystals;

[0026] 4) The second crystallization: Dissolve 49g of crystals obtained in step 3) in 200mL of hot water at 100°C, stir for 20min, then co...

Embodiment 2

[0034] 1) Extraction: take 1 kg of saffron powder and reflux extract three times, each time with 6L of 30% ethanol aqueous solution, filter, combine the filtrates, spin to recover the solvent under reduced pressure and concentrate to 2L.

[0035] 2) Extraction: adjust the pH of the concentrated solution obtained in step 1) to 3 with 3 mol / L hydrochloric acid, extract 3 times with n-butanol saturated with water, combine the organic layers and concentrate to 200 mL;

[0036] 3) The first crystallization: Add the concentrated solution obtained in step 2) into a mixed solvent of 300mL acetone and 100mL methyl tert-butyl ether, heat to reflux under stirring, then cool until a white precipitate precipitates, filter and dry to obtain a white crystal 38g;

[0037] 4) Second crystallization: Dissolve 38g of aescin crystals obtained in step 3) in 100ml of hot water at 80°C, stir for 60min, then cool the solution to precipitate a white solid, filter it with suction, and dry the solid to ...

Embodiment 3

[0041] 1) Extraction: take 1 kg of the saffron seed powder and reflux for extraction twice, each time with 15 L of 50% ethanol aqueous solution, filter, combine the filtrates, spin to recover the solvent under reduced pressure and concentrate to 3 L.

[0042] 2) Extraction: adjust the pH of the concentrated solution obtained in step 1) to 3 with 0.5 mol / L hydrochloric acid, extract 5 times with n-butanol saturated with water, combine the organic layers and concentrate to 300 mL;

[0043] 3) The first crystallization: Add the concentrated solution obtained in step 2) into a mixed solvent of 1200mL acetone and 150mL methyl tert-butyl ether, heat to reflux under stirring, then cool until a white precipitate precipitates, filter and dry to obtain a white crystal 43g;

[0044] 4) Second crystallization: Dissolve 43g of aescin crystals obtained in step 3) in 215mL of boiling water, stir for 30min, then cool the solution to precipitate a white solid, centrifuge, and dry the solid to ...

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Abstract

The invention discloses a preparation method for aescin B. The preparation method comprises the steps of extracting buckeye, extracting n-butyl alcohol, the first crystallization, the second crystallization and L-proline induced crystallization. The chiral amino acid and L-proline induced crystallization method is used for separating and obtaining the aescin monomer B, the purity of the aescin monomer B is over 97%, and the yield is up to about 60%. The preparation method has the advantages of simple production process, short production cycle, low production cost and so on.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular relates to a preparation method of aescin B. Background technique [0002] Aescin, also known as aescinic acid, is a general term for total saponins, β-aescin or isoaescin, etc. extracted from the seeds of plants of the genus Aescin, belonging to triterpenoid saponins. The water solubility of aescin is poor, in order to increase its solubility, it is often made into sodium salt. Aescin contains many kinds of saponin compounds. According to the national standard of our country, they are named as aescin A, aescin B, aescin C and aescin D in sequence according to the peak of liquid phase. They are isomers of each other (see attached figure 1 ), the sodium aescinate currently used clinically is a sodium salt mixture composed of aescin A, aescin B, aescin C and aescin D and other components. [0003] During the long-term use of sodium aescinate, it was found that the drug has a strong stim...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00A61P29/00A61P7/10
CPCC07J63/008
Inventor 石召华关小羽付强强陈书涵李群张晓存
Owner WUHAN AIMIN PHARMA
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