Method for microwave-ultrasonic-assistant hydrolysis extraction of Caesalpinia spiosa pod gallic acid

A gallic acid and microwave ultrasonic technology, applied in the preparation of carboxylic acid esters/lactones, organic chemistry, etc., can solve the problems of restricted enzymatic hydrolysis speed, difficult control, slow solvent diffusion, etc., and achieve high economic and practical value and high yield Improvement and ease of recycling

Inactive Publication Date: 2016-04-27
NORTHEAST FORESTRY UNIVERSITY +1
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  • Abstract
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Problems solved by technology

[0007] Chinese patent CN1104627 "Method for preparing gallic acid by alkali hydrolysis of Beihua raw materials" and CN1057255 "Using tara powder to produce gallic acid" use alkali hydrolysis first and then acid neutralization, which increases the complexity of the operation
Direct enzymatic hydrolysis production is often limited due to slow solvent diffusion and reaction conditions. For example, in CN1083532 "Enzymatic Production of Gallic Acid", enzymatic hydrolysis with solvents has strict requirements on temperature, pH, and dissolved oxygen, which is difficult to control
Yang Shunkai et al. "Enzymatic Transformation of Gallic Tannic Acid to Produce Gallic Acid" also adopts the method of enzymatic hydrolysis in solution, the solvent diffusion is slow, and the enzymatic hydrolysis speed is restricted

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  • Method for microwave-ultrasonic-assistant hydrolysis extraction of Caesalpinia spiosa pod gallic acid

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Embodiment

[0023] (1) Tara fruit pod powder is used as raw material 100g, add 1L of deionized water, condense and reflux for 2h, and filter to obtain the filtrate. Take 50ml of filtrate, add 0.25g of anti-oxidant reagent TBHQ, 6g of strongly basic 201*7 ion exchange resin catalyst (dry weight), and heat with the aid of microwave ultrasound at a power of 385W for 15min to extract gallic acid. Solid-liquid separation after cooling and crystallization of the hydrolyzate, solid phase dissolving with hot water, after activated carbon decolorization, recrystallization, vacuum drying, gallic acid product 2.06g is obtained, and the product is 98.3% (wt%) through HPLC analysis purity, and the yield is 41.9%, and the product yield is 1.3 times that without adding acidic ion exchange resin catalyst.

[0024] (2) Tara pod powder is used as raw material 100g, add 1L of deionized water, condense and reflux for 2h, and filter to obtain the filtrate. Take 50ml of filtrate, add 0.25g of antioxidant reag...

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Abstract

The invention relates to a method for microwave-ultrasonic-assistant hydrolysis extraction of Caesalpinia spiosa pod gallic acid. The method comprises adding deionized water into Caesalpinia spiosa pod powder as a raw material, carrying out reflux condensation, carrying out filtration to obtain a filtrate, adding an ion exchange resin catalyst and an antioxidation reagent into the filtrate and carrying out microwave-ultrasonic-assistant heating extraction to obtain gallic acid, wherein in heating, under the action of ionic liquid catalysis, tannic acid is decomposed to form gallic acid so that a gallic acid yield is effectively improved. The ion exchange resin is convenient for recovery, can be recycled, is economic and environmentally friendly, is suitable for large scale production and has high economic and practical value.

Description

Technical field: [0001] The invention belongs to the high-tech field, and in particular relates to a method for extracting gallic acid from tara fruit pods through hydrolysis aided by microwave ultrasound. Background technique: [0002] Tara (Caesalpiniaspiosa), also known as tara and blue sumac, belongs to the genus of hematoxylin, mainly distributed in Peru, Ecuador, Colombia and other countries in the northwest of South America. , fertile and well-lit places, it can grow up to 8-10m; there are 10 varieties; the root system is developed, the main root is obvious; hermaphroditism, self-pollination; the fruit pods are flat, reddish-brown when mature, generally 8-15cm long , 1.5-2.1cm wide, with 2-10 seeds inside; 1,000-grain weight of the seeds is 306.8g; the seed tree can bloom and bear fruit in 3a, the full fruit period is 10a, and each high-yielding tree can set pods 100-400kg. The natural and geographical conditions for the normal growth of Tara are that the altitude is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C65/03C07C51/09
CPCC07C51/09C07C65/03
Inventor 杨磊高文博杨逢建祖元刚韩峰李双阳杜新琦赵连飞刘再枝
Owner NORTHEAST FORESTRY UNIVERSITY
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