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Method for purifying shikimic acid in Chinese star anise

A purification method, shikimic acid technology, applied in the field of shikimic acid purification, can solve the problems of high cost, high loss of shikimic acid, cumbersome and time-consuming operation, etc., achieve high recovery rate, avoid excessive loss, and reduce operation difficulty

Pending Publication Date: 2020-06-16
陕西嘉禾药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the technical problems of high shikimic acid loss, complicated operation, time-consuming and high cost in the existing purification method of shikimic acid in star anise, and to provide a purification method of shikimic acid in star anise

Method used

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  • Method for purifying shikimic acid in Chinese star anise
  • Method for purifying shikimic acid in Chinese star anise
  • Method for purifying shikimic acid in Chinese star anise

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 1) extract

[0041] Crush and sieve the fresh star anise raw material, the mesh size of the sieve is 60 mesh; add water-saturated n-butanol, heat and stir for extraction, a total of 3 extractions, and the water-saturated n-butanol used for each extraction is 8 times the quality of the star anise raw material Quantity, extraction time is 2h, extraction temperature is 80 ℃, extracts are combined and suction filtered to obtain star anise extract;

[0042] 2) Purification

[0043] The star anise extract obtained in step 1) was concentrated under reduced pressure for the first time under the conditions of a vacuum of -0.08Mpa and a temperature of 80°C to obtain a first concentrate with a specific gravity of 1.05; the first concentrate was heated at 25°C Leave to crystallize for 24 hours, and filter with suction to remove oily precipitates and impurity crystals to obtain the first filtrate and precipitate A;

[0044]The precipitate A was rinsed with saturated n-butanol, com...

Embodiment 2

[0049] 1) extract

[0050] Crush and sieve the fresh star anise raw material, the mesh size of the sieve is 40 mesh; add water-saturated n-butanol, heat and stir for extraction, a total of 2 extractions, the water-saturated n-butanol used for each extraction is 6 times the quality of the star anise raw material Quantity, extraction time is 1.5h, extraction temperature is 70 ℃, the extracts are combined and suction filtered to obtain star anise extract;

[0051] 2) Purification

[0052] The star anise extract obtained in step 1) was concentrated under reduced pressure for the first time under the conditions of a vacuum of -0.08MPa and a temperature of 75°C to obtain a first concentrate with a specific gravity of 1.01; the first concentrate was heated at 20°C Leave to crystallize for 18 hours, and filter with suction to remove oily precipitates and impurity crystals to obtain the first filtrate and precipitate A;

[0053] The precipitate A was rinsed with saturated n-butanol, ...

Embodiment 3

[0058] 1) extract

[0059] Crush and sieve the fresh star anise raw material, the mesh size of the sieve is 80 mesh; add water-saturated n-butanol, heat and stir for extraction, a total of 4 extractions, and the water-saturated n-butanol used for each extraction is 10 times the quality of the star anise raw material Quantity, extraction time is 3h, extraction temperature is 90 ℃, the extracts are combined and suction filtered to obtain star anise extract;

[0060] 2) Purification

[0061] The star anise extract obtained in step 1) was concentrated under reduced pressure for the first time under the conditions of a vacuum of -0.07Mpa and a temperature of 85°C to obtain a first concentrate with a specific gravity of 1.1; the first concentrate was heated at 30°C Leave to crystallize for 26 hours, and filter with suction to remove oily precipitates and impurity crystals to obtain the first filtrate and precipitate A;

[0062] The precipitate A was rinsed with saturated n-butanol...

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Abstract

The invention relates to a purification method of shikimic acid, in particular to a method for simply and conveniently extracting and purifying shikimic acid from Chinese star anise. The invention aims to solve the technical problems of high shikimic acid loss, complicated and time-consuming operation and high cost in the existing method for purifying shikimic acid in Chinese star anise, and provides a method for purifying shikimic acid in Chinese star anise. The method comprises the following steps: 1) extraction: crushing and sieving a Chinese star anise raw material, adding water-saturatedn-butyl alcohol, heating, stirring for extraction, and carrying out suction filtration on an extraction solution to obtain a Chinese star anise extract liquid; 2) purification: concentrating the Chinese star anise extract liquid under reduced pressure, standing for precipitation and crystallization, and performing suction filtration to obtain a first filtrate and a precipitate A; leaching the precipitate A with water saturated n-butyl alcohol, combining the leacheate and the first filtrate, concentrating under reduced pressure, and standing for crystallization to obtain a coarse crystal B; and3) recrystallization: completely dissolving the coarse crystal B with ethanol, adding activated carbon for decolorization, carrying out vacuum concentration, standing for crystallization, and dryingto obtain a shikimic acid fine product with the purity of more than or equal to 98%.

Description

technical field [0001] The invention relates to a method for purifying shikimic acid, in particular to a method for simply and conveniently extracting and purifying shikimic acid from star anise. Background technique [0002] Star anise (scientific name: Illicium verum Hook.f.) is a plant of the star anise family and the genus Illicium, mainly distributed in Southeast Asia and North America. Star anise is a famous seasoning spice and also for medicinal purposes. Its peel, seeds, and leaves all contain aromatic oil, which is an important raw material for the manufacture of cosmetics, mulled wine, and beer. The dry and mature fruit of star anise contains aromatic oil, fatty oil, protein, resin, etc., its extract is fennel oil, its seeds contain 1.7%-2.7% fennel oil, and the content of fennel oil in dried fruit and dried leaves is 12%- 13%, 1.6%-1.8%. Star anise has the functions of invigorating the stomach, dispelling wind, analgesic, regulating Qi, dispelling cold and damp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/43C07C51/47C07C62/32
CPCC07C51/43C07C51/47C07C2601/16C07C62/32
Inventor 李宁胡洪来邓尚勇杨凯王前刚
Owner 陕西嘉禾药业有限公司
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