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Method for extracting shikimic acid from aniseed

A shikimic acid and star anise technology, applied in the chemical industry, can solve the problems of difficult purification steps, high energy consumption, and low extraction efficiency, and achieve the effects of reducing energy and time consumption, easy control, and simple process

Inactive Publication Date: 2009-10-21
中科检测技术服务(广州)股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the traditional method soaks the star anise in cold water, the extraction efficiency is not high due to the presence of fennel oil in the star anise; if the star anise is soaked in hot water, it will bring difficulties to the purification step because a large amount of non-effective components enter the extraction solution; in addition, rotary evaporation also consumes a lot of energy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Weigh 100 g of 20 mesh star anise and put it into supercritical CO 2 In fluid extraction equipment, CO 2 Inflate the device to remove air from the device. Set extraction pressure to 14MPa, extraction temperature to 30°C; primary separation pressure to 9MPa, primary separation temperature to 45°C; secondary separation pressure to cycle pressure, secondary separation temperature to normal temperature; extraction time to 120min; fennel oil yield to 8.5% ; from supercritical CO 2 The star anise powder after deoiling is taken out of the extraction equipment and extracted twice with pure water at 15°C, each time for 120 minutes, and the liquid-solid ratio is 15:1; the combined extracts are concentrated with a reverse osmosis membrane device, and the concentration condition is the front end of the reverse osmosis membrane The pressure is 1Mpa, the concentration temperature is 20°C, and the pH of the extract is 3.0; the concentrated extract is decolorized and crystallized, an...

Embodiment 2

[0017] Weigh 500 g of 40 mesh star anise and pack into supercritical CO 2 In fluid extraction equipment, CO 2 Inflate the device to remove air from the device. Set the extraction pressure to 16MPa, the extraction temperature to 35°C; the primary separation pressure to 9MPa, the primary separation temperature to 45°C, the secondary separation pressure to cycle pressure, and the secondary separation temperature to normal temperature; the extraction time is 120min; from supercritical CO 2 The deoiled star anise powder is taken out of the extraction equipment and extracted with pure water at 15°C for 3 times, each time for 90 minutes, and the liquid-solid ratio is 15:1; the combined extracts are concentrated with a reverse osmosis membrane device, and the concentration condition is the front end of the reverse osmosis membrane The pressure is 2Mpa, the concentration temperature is 25°C, and the pH of the extract is 3.2; the concentrated extract is decolorized and crystallized, a...

Embodiment 3

[0019] Weigh 40 mesh star anise 1000g and pack into supercritical CO 2 In fluid extraction equipment, CO 2 Inflate the device to remove air from the device. Set extraction pressure to 18MPa, extraction temperature to 35°C; primary separation pressure to 9MPa, primary separation temperature to 45°C; secondary separation pressure to cycle pressure, secondary separation temperature to normal temperature; extraction time to 120min; fennel oil yield to 9.9% ; from supercritical CO 2 Take out the deoiled star anise powder from the extraction equipment and extract 5 times with pure water at 20°C for 60 minutes each time, with a liquid-solid ratio of 15:1; combine the extracts and concentrate them with a reverse osmosis membrane device, the concentration condition is the front end of the reverse osmosis membrane The pressure is 2Mpa, the concentration temperature is 30°C, and the pH of the extract is 3.4; the concentrated extract is decolorized and crystallized, and the yield of shi...

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Abstract

The invention discloses a method for extracting shikimic acid from aniseed. The steps are as follows: firstly, supercritical CO2 fluid is used for extracting anise oil from the aniseed; secondly, room temperature water is used for steeping the deoiled aniseed; thirdly, a reverse osmosis membrane device is used for concentrating shikimic acid extract; and the shikimic acid can be obtained after the operations of decolourization and crystallization are carried out. The method has the advantages that the process is simple and stable and is easy to control, and the extraction percentage of the shikimic acid can be more than 9 percent; by adopting the reverse osmosis membrane device for concentration, the method reduces the consumption of energy and time.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for extracting shikimic acid from star anise. Background technique [0002] Shikimic acid (molecular formula C 7 h 10 o 5 ) is a hydroxy acid that can be used to synthesize the drug "Tamiflu" for the treatment of bird flu, which is mainly extracted from the fruit of star anise. The traditional method of extracting shikimic acid is to take the dried star anise fruit, crush it, extract it with water, and evaporate it by rotary evaporation to obtain the extract, then apply it to a silica gel column for gradient elution, add activated carbon to boil for decolorization, filter to obtain the filtrate, and recrystallize to obtain shikimic acid. If the traditional method soaks the star anise in cold water, the extraction efficiency is not high due to the presence of fennel oil in the star anise; if the star anise is soaked in hot water, it will bring difficulties to the purif...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C62/32C07C51/42B01D61/02
CPCY02P20/10Y02P20/50Y02P20/54
Inventor 哈成勇杨少凡哈启燊刘新伟沈敏敏胡志忠
Owner 中科检测技术服务(广州)股份有限公司
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