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Extraction separation tech. of octagonal shickimmi oxalic acid

A separation technology, the technology of shikimic acid, is applied in the separation/purification of carboxylic acid compounds, medical preparations containing active ingredients, plant/algae/fungus/moss components, etc. Production, low utilization of raw materials, etc., to achieve the effect of high product recovery rate, reduced impact, and improved utilization level

Inactive Publication Date: 2007-07-18
HONGHE COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This causes two problems in the process: 1. Industrial impurities are mixed in the star anise oil, which greatly reduces the utilization value of the star anise oil, and the utilization rate of raw materials is low
Second, the production cost is high and the benefit is low, which is not conducive to the production of enterprises

Method used

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  • Extraction separation tech. of octagonal shickimmi oxalic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Use 1 kg of dry star anise produced in Luchun County, Yunnan, crush it to 30 meshes, use a supercritical carbon dioxide extraction device (extraction kettle 10L, separation kettle 10L), under the conditions of 40°C, 25MPa, and a carbon dioxide flow rate of 15kg / h Extract for 1 hour, separate oil and fat under the conditions of 40°C and 12MPa, and obtain 0.16 kg of star anise oil, which can be directly used as food flavoring. The extracted star anise slag was heated and refluxed for 3 times with 3-4 times its volume of commercially pure methanol, the leaching temperature was 50°C, and the reflux time was 3, 2, and 1 h respectively. The three extracts were combined, and the methanol was recovered to obtain leaching Paste 0.15kg. The extract was heated and extracted with 0.3L ethyl acetate, the extraction temperature was 50°C, the extraction times were 2 times, the extracts were combined, and the ethyl acetate was recovered. Heat and stir the extract with 0.5L of methanol...

Embodiment 2

[0022] 5 kg of star anise raw material, crushed to 150 mesh, using a supercritical carbon dioxide extraction device, extracted at 43°C, 30MPa, and a carbon dioxide flow rate of 17kg / h for 1.5h, separated oil and fat at 43°C, 14MPa, and obtained 0.95kg of star anise oil . The extracted star anise slag is heated and refluxed for 3 times with industrially pure methanol 3 to 4 times its volume. The leaching temperature is 55°C, and the reflux time is 3, 2, and 1 h respectively. The three extracts are combined, and the methanol is recovered to obtain leaching Cream 0.7kg. The extract is heated and extracted with ethyl acetate 2 to 4 times its volume, the extraction temperature is 53°C, the extraction times are 3 times, the extracts are combined, and the ethyl acetate is recovered. Heat and stir the extract with 3L of methanol at 55°C to dissolve, filter while hot, let the filtrate stand naturally, cool and crystallize to obtain 205g of crude shikimic acid. The crude product of sh...

Embodiment 3

[0024] 5 kg of star anise raw material was crushed into 200 meshes, extracted by supercritical carbon dioxide extraction device at 45°C, 35MPa, and carbon dioxide flow rate of 20kg / h for 2 hours, and oil was separated at 45°C and 14MPa to obtain 0.96kg of star anise oil. The extracted star anise slag is heated and refluxed for 3 times with industrially pure methanol 3 to 4 times its volume. The leaching temperature is 55°C, and the reflux time is 3, 2, and 1 h respectively. The three extracts are combined, and the methanol is recovered to obtain leaching Cream 0.7kg. The extract is heated and extracted with ethyl acetate 2 to 4 times its volume, the extraction temperature is 53°C, the extraction times are 3 times, the extracts are combined, and the ethyl acetate is recovered. Heat and stir the extract with 3L of methanol at 55°C to dissolve, filter while hot, let the filtrate stand naturally, cool and crystallize to obtain 207g of crude shikimic acid. The crude product of shi...

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Abstract

This invention relates to an extraction and separation technology of anise tree shikimic acid. The main steps are : Using supercritical carbon dioxide to defat the crushed dry anise tree at 40 ~ 45 deg C, 25 ~ 35MPa to gain food spices; then heating back with methanol at 50 ~ 60 deg C to leach extract; under 50-55 deg C using acetic ether to extract, filtration and separation to remove acetic ether, remaining solid extract; methanol will be used in 50 ~ 60 deg C to heat and stir with extract until dissolved, by hot filtration, liquid natural still, cooling crystallization, then gain crude shikimic acid; chloroform and methanol mixed solvent used under 45 ~ 50 deg C to dissolve crude shikimic acid, through natural still, cooling and crystallization , and recrystallization to gain purified product, with purity greater than 95% pure. This invention use supercritical carbon dioxide to extract and degrease. The product spices can be directly consumed, non-toxic and harmless to humans.

Description

technical field [0001] The invention relates to a technique for extracting and separating shikimic acid from dried star anise. Background technique [0002] Shikimic acid, derived from the dry mature fruit of Magnolia plant star anise (Illicium verum Hook.f.), the molecular formula of shikimic acid is C 7 h 10 o 5 , Molecular weight 174.16. Melting point 191-192°C. The pharmacological effects of shikimic acid include: anti-inflammatory, analgesic, as an intermediate of anticancer drugs, the latest application of shikimic acid shows that shikimic acid can effectively deal with the deadly H5N1 bird flu virus drug" Tamiflu" is an important raw material with huge potential value. Yunnan is the second largest production area of ​​star anise in China. In recent years, the planting area of ​​star anise has developed rapidly. The planting area in Luchun County alone has reached 250,000 mu, and the planting area in Honghe Prefecture has exceeded 400,000 mu. Calculated as 50 kilogr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/42C07C62/04A61K36/57A61K131/00
CPCY02P20/54
Inventor 闵勇刘卫杨金
Owner HONGHE COLLEGE
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