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Method for extracting high-pure shikimic acid from scarlet octagonal fruit

A shikimic acid, high-purity technology, applied in the direction of pharmaceutical formulations, separation/purification of carboxylic acid compounds, medical preparations containing active ingredients, etc., can solve problems such as containing alkali and consuming large acidic cationic resins

Inactive Publication Date: 2008-08-27
GUANGXI TEACHERS EDUCATION UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that using a strong base as the eluent causes the crude product to contain alkali, and consumes a large amount of acidic cationic resin in the process of removing alkali and salt

Method used

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  • Method for extracting high-pure shikimic acid from scarlet octagonal fruit
  • Method for extracting high-pure shikimic acid from scarlet octagonal fruit
  • Method for extracting high-pure shikimic acid from scarlet octagonal fruit

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take 500 grams of dried star anise fruit powder and crush it to 30-40 meshes, use 1.5 L of petroleum ether (boiling range: 60°C-90°C) as a solvent, use a reflux device to reflux extract for 3 hours, and then vacuum separate it under the condition of 60-90°C The star anise oleoresin is deoiled star anise slag, and the star anise slag is dried in the air. Reflux the dried star anise slag with 1.5L, 1.25L, 1.0L, 1.0L of 85% ethanol for 3, 3, 2.5, 2 hours respectively, combine the extracts and concentrate in vacuo to a density of 1.3-1.4g / mL extract. Dissolve the obtained extract in 5 times the volume of hot water and heat at about 78°C for about one hour, remove a small amount of grease from the upper layer, cool, precipitate, and filter to obtain an orange-red liquid. The obtained liquid is subjected to column chromatography with 400 g of neutral macroporous adsorption resin 201*7 (type 717) that has been treated, and is eluted with water to a light color, and the eluate...

Embodiment 2

[0029]Take 800g of dried red star anise fruit powder and crush it to 30-40 meshes, use 2.2L of petroleum ether (boiling range: 60°C-90°C) as a solvent, and use a reflux device to reflux for 3 hours, and then vacuum-separate the star anise under the condition of 60-90°C Oleoresin obtained deoiled star anise slag, and the star anise slag was air-dried, and the dried star anise slag was refluxed with 2.4L, 2.0L, 1.6L, 1.6L 85% ethanol for 3, 3, 2.5 , 2 hours, the combined extracts were vacuum concentrated to an extract with a density of 1.3-1.4 g / mL. Dissolve the obtained extract in 7 times the volume of hot water and heat at about 80°C for about one hour, remove a small amount of grease from the upper layer, cool, precipitate, and filter to obtain an orange-red liquid. The obtained liquid is subjected to column chromatography with 560 g of neutral macroporous adsorption resin 201*7 (type 717) that has been treated, eluted with water to a light color, and the eluate is collected ...

Embodiment 3

[0031] Take 1Kg of dried star anise fruit powder and crush it to 30-40 meshes, use 3.2L of petroleum ether (boiling range: 60°C-90°C) as a solvent, and use a reflux device for reflux extraction for 3 hours, and then vacuum-separate the star anise under the condition of 60-90°C Oleoresin is deoiled star anise slag, and the star anise slag is dried in the air. Reflux the dried star anise slag with 3.0L, 2.5L, 2.0L, and 2.0L of 80% ethanol for 3, 3, 2.5, and 2 hours respectively, combine the extracts and concentrate in vacuum to a density of 1.3-1.4g / mL extract. Dissolve the obtained extract in 6 times the volume of hot water and heat at about 76°C for about one hour, remove a small amount of grease from the upper layer, cool, precipitate, and filter to obtain an orange-red liquid. The resulting liquid is subjected to column chromatography with 600 g of neutral macroporous adsorption resin 201*7 (type 717) that has been treated, eluted with water to a light color, and the eluate...

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Abstract

A method for extracting high-purity shikimic acid from red illicium comprises breaking dry illicium via general technique, deoiling and drying, refluxing via industrial alcohol to extract the deoiled illicium slag, combining and concentrating extract liquors into extractive, dissolving via hot water, bathing in hot water, absorbing oil and filtering, concentrating and removing impurity via neutral macroporous adsorption resin, purifying via alkali anion exchange resin, volatilizing the solvent in crude shikimic acid, dissolving in hot water, adding acetone, freezing and crystallizing, and recrystallizing to obtain fine shikimic acid product. The invention uses alcohol for extraction and uses different resins to absorbe impurity and shikimic acid, thereby reducing the effect of soluble impurity, and the extract liquor can be filtered easily to avoid ultrafiltration device, and the resins have high adsorption capacity and high chromatography speed, thereby saving organic solvent, reducing production cost and improving product quality.

Description

technical field [0001] The invention relates to a method for extracting high-purity shikimic acid from star anise fruit. Background technique [0002] Star anise (Illicium verum Hook.f.) is a plant of the genus Illicium in Magnoliaceae. It is an important economic tree species of "medicine and food from the same source" in southern my country. It is mainly distributed in Guangxi, Yunnan, Sichuan and other provinces in my country. The dried and mature fruits contain aromatic oil, Fatty oil, protein, resin, etc., are special spices and traditional Chinese medicines in my country, and are also necessary seasonings for households. They are widely used in the fields of food and spices. In addition, star anise also contains another important active ingredient shikimic acid (Shikimic Acid, 3,4,5-trihydroxy-1-cyclohexene-1-carboxylic acid), and its content in star anise is about It is 5% to 8%, and the content in poisonous star anise is more than 10%, but the resource of poisonous s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C62/04C07C51/42C07C51/47A61K36/57
Inventor 黄初升阳小勇刘红星何冬梅
Owner GUANGXI TEACHERS EDUCATION UNIV
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