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Method for preparing ellagic acid through basic hydrolysis of tannin in Platycarya strobilacea fruits

The technology of ellagic acid and tannin base is applied in the field of fine processing of plant tannin, which can solve the problems of complicated and complicated preparation process, expensive acid-resistant equipment, equipment corrosion, etc., and achieves a simple process, short reaction time and high production efficiency. Effect

Inactive Publication Date: 2016-04-27
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Application Information

AI Technical Summary

Problems solved by technology

Acid hydrolysis needs to be carried out at high temperature, acid-resistant equipment is expensive, and its practical application is limited
(3) Prepared by oxidation using gallic acid or its esters as raw materials; this method is a chemical synthesis method, and the preparation process is cumbersome and complicated
It has been reported that the method for preparing ellagic acid from the fragrant fruit extract is implemented by acid hydrolysis, but the high-temperature acid hydrolysis has serious environmental pollution and equipment corrosion

Method used

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  • Method for preparing ellagic acid through basic hydrolysis of tannin in Platycarya strobilacea fruits

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1 (extraction)

[0017] Crush the fragrant fruit and use water as the solvent to heat and extract. The extraction method can be conventional soaking, microwave-assisted extraction, ultrasonic-assisted extraction, the extraction temperature is 50-100°C, the number of extractions is 2-4 times, and the extraction time for each time After 1-3 hours, filter to remove the slag, heat and concentrate in a vacuum, and dry to obtain the fragrant fruit tannin. The details are as follows: 730g of the raw material of Huaxiang fruit sequence dried in the shade until the water content is 14.2wt%, remove the impurities, crush to 3-5mm, add 7300mL of pure aqueous solution at 70°C for 30min with ultrasonic assistance, filter the extract for solid-liquid separation, Repeat the extraction twice, discard the waste residue, and combine the extracts. The extract was cooled and allowed to settle overnight, and the precipitate was discarded. The supernatant was concentrated in vacuu...

Embodiment 2

[0019] Take 5g of citrus tannin, add 100mL of 0.75mol / L sodium hydroxide solution, and stir and hydrolyze for 60min at 100°C. Dilute hydrochloric acid was added to the reaction solution under stirring until the pH value of the reaction solution was 6, filtered, and the filter cake was washed with water to obtain a crude product of ellagic acid with a purity of 68.0% (HPLC method, the same below).

[0020] Add the crude product of ellagic acid into dilute sodium hydroxide solution, add activated carbon, react at 50°C for 1 hour, filter the reaction solution, wash the filter cake with water, combine the filtrate and washing solution; add dilute hydrochloric acid dropwise to adjust the pH of the solution When the pH value is 4, filter, and the filter cake is washed with water and dried to obtain 0.6 g of light yellow ellagic acid product with a content of 98.1%.

Embodiment 3

[0022] Take 10 g of citrus tannin, add 0.5 mol / L sodium hydroxide solution 300 mL, and stir and react at 90° C. for 60 min. Add dilute hydrochloric acid to the reaction solution while stirring until the pH value of the reaction solution is 5, filter, and wash the filter cake with water to obtain a crude product of ellagic acid with a purity of 65.6%. The crude product was refined and dried in the same manner as in Example 2 to obtain 1.2 g of a light yellow ellagic acid product with a content of 98.4%.

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Abstract

The invention discloses a method for preparing ellagic acid through basic hydrolysis of tannin in Platycarya strobilacea fruits. The tannin in the Platycarya strobilacea fruits is taken as a raw material, a base catalyst is added, and the mixture has an ultrasonically assisted hydrolysis reaction at the certain temperature; acid is added to a reaction liquid for adjustment of pH value, vacuum filtration is performed, a filter cake is washed, an ellagic acid crude product is obtained, and the purity measured with an HPLC (high performance liquid chromatography) is larger than 65 wt%; the crude product is refined and purified with a base dissolution, activated carbon decoloration and filtration and diluted acid reduction and sedimentation method, and the ellagic acid with the content higher than 98wt% is obtained. The preparation process is simple, and the product purity is high.

Description

Technical field: [0001] The invention belongs to the field of fine processing of vegetable tannins. In particular, it relates to a method for preparing ellagic acid by alkali hydrolysis of citrus tannin as a raw material. Background technique: [0002] Ellagic acid (Ellagic acid), also known as hexahydroxybiphenyl acid dilactone, is a fine chemical product with a high price. Ellagic acid has a variety of physiological activities, including antioxidant, anticancer / antimutagenic properties, and inhibition of human immunodeficiency virus. Widely used in medicine, cosmetics, and health food raw materials. According to the existing literature, the preparation routes of ellagic acid can be summarized into four types: (1) Separation from natural plants containing ellagic acid. Ellagic acid exists in a small amount in free form in nature, most of which exist in the form of 6,6-dicarbonyl-2,2,3,3,4,4-hexahydroxybiphenyl derivatives, so it is difficult to directly Ellagic acid is ...

Claims

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Application Information

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IPC IPC(8): C07D493/06
CPCC07D493/06
Inventor 汪咏梅徐曼张亮亮陈笳鸿胡新宇
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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