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Process for producing high-purity ellagic acid by desolvation crystallization method

A technology of ellagic acid and anti-solvent, which is applied in the technical field of producing high-purity ellagic acid by anti-solvent crystallization, can solve the problems of unfavorable industrial scale-up, low purity and low solubility of ellagic acid, and achieve simple operation and low cost Inexpensive, good color effect

Inactive Publication Date: 2017-05-10
NORTHEAST FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently, there are solvent washing and recrystallization methods for the purification of ellagic acid. The solvent washing method is the most widely used in industry. The solvent is water, ethanol solution, NaHCO according to the different preparation methods of ellagic acid. 3 , acid solution, etc., because the solubility of ellagic acid in the above solvents is not high, a large amount of solvent is required for purification, and the purity of the obtained ellagic acid is not high, generally lower than 95%.
Methanol recrystallization method is a very effective method for purifying ellagic acid. The obtained ellagic acid product has high purity and good color. However, the problem with this method is that a large amount of solvents are required for production, which is not conducive to industrial scale-up.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0023] Weigh 1g of crude ellagic acid with a purity of 40% (extracted from pomegranate peel) and add it to 10ml of N-methylpyrrolidone, stir to dissolve the ellagic acid completely, centrifuge to remove insoluble matter, and slowly add the supernatant to 300ml 17 ℃ constant temperature water, 1000rpm stirring crystallization 10min. After the crystallization, the suspension was centrifuged, the supernatant was removed, the precipitate was washed twice with water, and vacuum-dried at 40°C for 12 hours to obtain light yellow ellagic acid powder. The purity of ellagic acid obtained by HPLC was 98.3%. The rate is 95%.

example 2

[0025] Weigh 600 mg of crude ellagic acid with a purity of 40% (semi-synthesized from tannic acid) and add it to 4 ml of N-methylpyrrolidone, stir to dissolve the ellagic acid completely, remove the insoluble matter by centrifugation, and slowly add the supernatant to the In 80ml of 20°C constant-temperature ethyl acetate, stirring and crystallizing at 1000rpm for 15min. After the crystallization, the suspension was centrifuged, the supernatant was removed, the precipitate was washed twice with 10% alcohol, and vacuum-dried at 40°C for 12 hours to obtain light yellow ellagic acid powder. The purity of ellagic acid obtained by HPLC was 96.6 %, the yield is 90%.

example 3

[0027] Weigh 100mg of crude ellagic acid with a purity of 40% (extracted from pomegranate peel) and add it to 5ml dimethyl sulfoxide, stir to dissolve the ellagic acid completely, remove insoluble matter by centrifugation, and slowly add the supernatant to 50ml In dichloromethane at a constant temperature of 10°C, stirring and crystallizing at 1000rpm for 10min. After the crystallization, the suspension was centrifuged, the supernatant was removed, the precipitate was washed twice with 20% alcohol, and vacuum-dried at 40°C for 12 hours to obtain light yellow ellagic acid powder. The purity of ellagic acid obtained by HPLC was 96.3 %, the yield is 86.4%.

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Abstract

The invention discloses a process for producing high-purity ellagic acid by a desolvation crystallization method. The process is characterized in that firstly, low-purity ellagic acid is dissolved into any one kind of solvent of dimethyl sulfoxide or 1-Methyl-2-pyrrolidinone; then, the mixture is added into the set volume time of anti-solvent methanol, ethanol, methylene dichloride, trichloromethane, glacial acetic acid, ethyl acetate or water; at the set temperature, the anti-solvent is stirred for a period of time for crystallization; centrifugation or filtration is performed to obtain precipitates; the precipitates are cleaned several times by water or alcohol water; vacuum drying is performed; the high-purity primrose yellow ellagic acid is obtained. The process has the advantages that the operation is simple; the consumption of the solvent is low; the obtained ellagic acid has high purity and high yield; the process is suitable for industrial production.

Description

technical field [0001] The invention relates to a process for purifying ellagic acid by using an anti-solvent crystallization method. The ellagic acid produced by the process has high purity, and in particular relates to a high-purity ellagic acid production process with low production cost and simple process flow. [0002] technical background [0003] A large number of studies at home and abroad have shown that ellagic acid has unique effects in anti-cancer, anti-oxidation, antibacterial, etc., and also has activities such as whitening, moisturizing, and anti-aging. Therefore, ellagic acid has broad application prospects and huge market value in the fields of medicine and cosmetics. Most of the crude pomegranate peel extracts on the market are unpurified and relatively low in ellagic acid content. Currently, there are solvent washing and recrystallization methods for the purification of ellagic acid. The solvent washing method is the most widely used in industry. The solve...

Claims

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Application Information

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IPC IPC(8): C07D493/06
CPCC07B2200/13C07D493/06
Inventor 赵修华王力吴微微李媛媛刘艳杰
Owner NORTHEAST FORESTRY UNIVERSITY