Summary of the invention
The object of the invention is to overcome the shortcoming that exists in the prior art, a kind of energy-efficient, cost is low, technique is simply extracted shikimic acid from anise method is provided.
Purpose of the present invention is achieved through the following technical solutions:
A kind of method of extracting shikimic acid from anise is to use first supercritical CO
2Olium anisi in the fluid extraction anise; Then be soaked in water and extract anise after the oil removing, obtain the shikimic acid extracting solution; Again with the concentrated shikimic acid extracting solution of reverse osmosis membrane apparatus; Obtain shikimic acid through decolouring, crystallization.
Described supercritical CO
2Olium anisi in the fluid extraction anise is first star aniseed powder to be broken to 20~80 orders before extraction; Extracting pressure is 14~24MPa, 30~45 ℃ of extraction temperature; Flash trapping stage pressure 9MPa, the flash trapping stage temperature 45 C; The second-order separation pressure cycling is pressed, the second-order separation temperature normal temperature.The highest olium anisi oil yield can reach more than 10%; Through above-mentioned supercritical CO
2The anistree powder that extracts the olium anisi processing can extract shikimic acid for the present invention.
Anise after the described extraction oil removing that is soaked in water, anise: the weight ratio of water is 1: 15~20, and soaking temperature is 15~25 ℃, and soaking number of times is 1~5 time, and each soak time is 60~180 minutes.
Described reverse osmosis membrane concentrated extracting solution, reverse osmosis membrane forefront pressure are 1~5Mpa, and 20~45 ℃ of thickening temperatures, the pH value of extracting solution are 3~4, and the shikimic acid extract yield can reach more than 9%.
The present invention adopts supercritical CO
2Olium anisi in the fluid extraction anise, on the one hand so that remove that easier being flooded of water soluble component in the anise puts forward behind the oiliness composition, can open on the other hand anistree cell walls, easier being flooded of water soluble component in the anise puts forward behind the oiliness composition so that remove, and extracts shikimic acid for cold water soak and lays the foundation.
The present invention compared with prior art has following advantage and effect:
(1) technique of the present invention simple, stablize, be easy to control, the shikimic acid extraction yield can reach more than 9%.
(2) the present invention adopts the reverse osmosis membrane apparatus concentrated extracting solution, has reduced the consumption of the energy and time.
Embodiment
Below in conjunction with embodiment the present invention is done further detailed description, but embodiments of the present invention are not limited to this.
Embodiment 1
Take by weighing the anistree 100g of the 20 orders supercritical CO of packing into
2In the fluid extraction equipment, use CO
2The equipment that is filled with is with the air in the remover apparatus.The setting extracting pressure is 14MPa, 30 ℃ of extraction temperature; Flash trapping stage pressure 9MPa, the flash trapping stage temperature 45 C; The second-order separation pressure cycling is pressed, the second-order separation temperature normal temperature; Extraction time is 120min; Olium anisi oil yield 8.5%; From supercritical CO
2Take out anistree powder after the de-oiling in the extraction equipment with 15 ℃ of Aqua pure extracts 2 times, extract 120min at every turn, liquid-solid ratio is 15: 1; United extraction liquid, concentrated with reverse osmosis membrane apparatus, concentrated condition is that the reverse osmosis membrane forefront pressure is 1Mpa, and thickening temperature is 20 ℃, and the PH of extracting solution is 3.0; Extracting solution after concentrated is through decolouring, crystallization, and the shikimic acid yield is 8.8%.
Embodiment 2
Take by weighing the anistree 500g of the 40 orders supercritical CO of packing into
2In the fluid extraction equipment, use CO
2The equipment that is filled with is with the air in the remover apparatus.The setting extracting pressure is 16MPa, 35 ℃ of extraction temperature; Flash trapping stage pressure 9MPa, the flash trapping stage temperature 45 C; The second-order separation pressure cycling is pressed, the second-order separation temperature normal temperature; Extraction time is 120min; Olium anisi oil yield 8.9%; From supercritical CO
2Take out anistree powder after the de-oiling in the extraction equipment with 15 ℃ of Aqua pure extracts 3 times, extract 90min at every turn, liquid-solid ratio is 15: 1; United extraction liquid, concentrated with reverse osmosis membrane apparatus, concentrated condition is that the reverse osmosis membrane forefront pressure is 2Mpa, and thickening temperature is 25 ℃, and the PH of extracting solution is 3.2; Extracting solution after concentrated is through decolouring, crystallization, and the shikimic acid yield is 9.1%.
Embodiment 3
Take by weighing the anistree 1000g of the 40 orders supercritical CO of packing into
2In the fluid extraction equipment, use CO
2The equipment that is filled with is with the air in the remover apparatus.The setting extracting pressure is 18MPa, 35 ℃ of extraction temperature; Flash trapping stage pressure 9MPa, the flash trapping stage temperature 45 C; The second-order separation pressure cycling is pressed, the second-order separation temperature normal temperature; Extraction time is 120min; Olium anisi oil yield 9.9%; From supercritical CO
2Take out anistree powder after the de-oiling in the extraction equipment with 20 ℃ of Aqua pure extracts 5 times, extract 60min at every turn, liquid-solid ratio is 15: 1; United extraction liquid, concentrated with reverse osmosis membrane apparatus, concentrated condition is that the reverse osmosis membrane forefront pressure is 2Mpa, and thickening temperature is 30 ℃, and the PH of extracting solution is 3.4; Extracting solution after concentrated is through decolouring, crystallization, and the shikimic acid yield is 9.2%.
Embodiment 4
Take by weighing the anistree 1500g of the 60 orders supercritical CO of packing into
2In the fluid extraction equipment, use CO
2The equipment that is filled with is with the air in the remover apparatus.The setting extracting pressure is 20MPa, 40 ℃ of extraction temperature; Flash trapping stage pressure 9MPa, the flash trapping stage temperature 45 C; The second-order separation pressure cycling is pressed, the second-order separation temperature normal temperature; Extraction time is 120min; Olium anisi oil yield 10.1%; From supercritical CO
2Take out anistree powder after the de-oiling in the extraction equipment with 20 ℃ of Aqua pure extracts 5 times, extract 60min at every turn, liquid-solid ratio is 20: 1; United extraction liquid, concentrated with reverse osmosis membrane apparatus, concentrated condition is that the reverse osmosis membrane forefront pressure is 3Mpa, and thickening temperature is 35 ℃, and the PH of extracting solution is 3.6; Extracting solution after concentrated is through decolouring, crystallization, and the shikimic acid yield is 9.1%.
Embodiment 5
Take by weighing the anistree 800g of the 60 orders supercritical CO of packing into
2In the fluid extraction equipment, use CO
2The equipment that is filled with is with the air in the remover apparatus.The setting extracting pressure is 22MPa, 45 ℃ of extraction temperature; Flash trapping stage pressure 9MPa, the flash trapping stage temperature 45 C; The second-order separation pressure cycling is pressed, the second-order separation temperature normal temperature; Extraction time is 120min; Olium anisi oil yield 9.3%; From supercritical CO
2Take out anistree powder after the de-oiling in the extraction equipment with 25 ℃ of Aqua pure extracts 4 times, extract 80min at every turn, liquid-solid ratio is 20: 1; United extraction liquid, concentrated with reverse osmosis membrane apparatus, concentrated condition is that the reverse osmosis membrane forefront pressure is 4Mpa, and thickening temperature is 40 ℃, and the PH of extracting solution is 3.8; Extracting solution after concentrated is through decolouring, crystallization, and the shikimic acid yield is 8.9%.
Embodiment 6
Take by weighing the anistree 300g of the 80 orders supercritical CO of packing into
2In the fluid extraction equipment, use CO
2The equipment that is filled with is with the air in the remover apparatus.The setting extracting pressure is 24MPa, 45 ℃ of extraction temperature; Flash trapping stage pressure 9MPa, flash trapping stage temperature 45 C the second-order separation pressure cycling is pressed, the second-order separation temperature normal temperature; Extraction time is 120min; Olium anisi oil yield 9.1%; From supercritical CO
2Take out anistree powder after the de-oiling in the extraction equipment with 25 ℃ of Aqua pure extracts 3 times, extract 90min at every turn, liquid-solid ratio is 20: 1; United extraction liquid, concentrated with reverse osmosis membrane apparatus, concentrated condition is that the reverse osmosis membrane forefront pressure is 5Mpa, and thickening temperature is 45 ℃, and the PH of extracting solution is 4.0; Extracting solution after concentrated is through decolouring, crystallization, and the shikimic acid yield is 8.8%.