CN101371700A - Method for unitedly extracting anise tree volatile oil and shikimic acid crude extract - Google Patents
Method for unitedly extracting anise tree volatile oil and shikimic acid crude extract Download PDFInfo
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- CN101371700A CN101371700A CNA2008101985927A CN200810198592A CN101371700A CN 101371700 A CN101371700 A CN 101371700A CN A2008101985927 A CNA2008101985927 A CN A2008101985927A CN 200810198592 A CN200810198592 A CN 200810198592A CN 101371700 A CN101371700 A CN 101371700A
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- volatile oil
- shikimic acid
- crude extract
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a method for jointly extracting star anise volatile oil and shikimic acid crude extract; the specific steps are as follows: star anise is firstly dried and smashed; secondly, the star anise is extracted by supercritical carbon dioxide fluid under the specific condition, and then the volatile oil is obtained; finally, the star anise fine powder which is extracted with the volatile oil is soaked with water, filtered and concentrated, and then the shikimic acid crude extract is obtained. The method provided by the invention is easy to be operated; the star anise volatile oil with high productive rate and high quality can be obtained; compared with the traditional method, the transfer rate of leach extract is high, thus effectively improving the comprehensive utilization rate of the star anise.
Description
Technical field
The invention belongs to anistree plant resources comprehensive utilization field, particularly a kind of method of extracting anise tree volatile oil and shikimic acid crude extract of uniting.
Background technology
Anise is a kind of plant of Chinese anise order Illiciaceae Illicium, and formal name used at school lllicium verum claims aniseed and anise again.The anise of mentioning in the daily life is meant its dry fruit of the same name (below mention that anise all is meant its dry fruit), and it is one of flavoring of Chinese dishes and south east asia culinary art, also can be used as medicine.
At present, anise is in the Chemical Manufacture of raw material, with two compositions serves as to extract target, the one, extract the volatile ingredient------volatile oil in the anise, main component of essential oil comprises anisole (Anethole), safrole (Safrole), anisaldehyde (Anisaldehyde) and fenchone (Anisylacetone) etc., the 2nd,------shikimic acid, shikimic acid are the precursors of the medicine Tamiflu of human avian influenza to the water soluble ingredient in the extraction anise, and two compositions all have higher economic value.
In the bibliographical information to the anise extraction, mostly be to be to extract target with the separate constituent, as " technical study of shikimic acid in the microwave assisted extraction fennel (food technology science and technology, 2007; 28 (3): 137～142) ", all do not consider the extraction of uniting of volatile oil, shikimic acid in their research.And in reality production and using, must consider making full use of with economic interests of anistree resource maximized, when design volatile oil, shikimic acid list composition extraction process, to coordinate mutually, mutual restriction, unite extraction to realize efficient, the convenient extraction of volatile oil, two kinds of compositions of shikimic acid.Therefore, around volatile oil and two compositions of shikimic acid, also developed some combined extraction technologies, at present the extraction process of main flow as shown in Figure 1, wherein, in " water logging bubble " unit operations, methods such as water temperature is below 60 ℃, and this soaks with high temperature, microwave is auxiliary are compared, and make shikimic acid fully not to be dissolved in the water, the rate of transform of shikimic acid descends, and shikimic acid can not fully extract.If the raising soaking temperature can cause the oxidation of volatile ingredient in the anise again, reduced the quality of steam distillation product star anise oil.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of method of extracting anise tree volatile oil and shikimic acid crude extract of uniting efficiently, easily is provided.
Purpose of the present invention realizes by following technical scheme: a kind of method of extracting anise tree volatile oil and shikimic acid crude extract of uniting specifically may further comprise the steps:
(1) anistree pre-treatment: anistree drying handled to water content be lower than 10%, be crushed to 20～100 order left and right sides powder;
(2) volatile oil extracts: the anistree powder of handling through step (1) carries out supercritical carbon dioxide extraction and obtains anise tree volatile oil, extraction conditions is: extracting pressure 12～24MPa, 35～45 ℃ of extraction temperature, one-level separating pressure 8～10MPa, 40～55 ℃ of one-level separation temperatures, secondary separation temperature normal temperature is pressed in the circulation of secondary separating pressure, flow 4.5～6L/h extracted 1～2 hour;
(3) extract the shikimic acid crude extract: the anistree powder that step (2) has been extracted volatile oil is soaked in water; 60～90 ℃ of water temperature range; Soak time 20 minutes～2 hours; The solid-liquid weight ratio is 1: 4～10; Filter, filtrate concentrating obtains the shikimic acid crude extract.
To better implement the present invention:
In the step (1): the dry water content of handling of anise is lower than 7%, is crushed to 20～40 order left and right sides powder; Drying method can be that nature dries in the shade or industry universal method such as freeze drying; Breaking method can be shear to pulverize or beat the industry universal method such as to grind
In the step (3): soaking water is soft water such as deionized water; More excellent 75～85 ℃ of water temperature range; Soak time more preferably 40 minutes～60 minutes; Solid-liquid weight ratio more preferably 1: 5～7; Can also adopt extractive techniques such as ultrasonic coupling in the water logging bubble process; Water logging bubble unit operations can be intermittently, continuously or industry universal method such as counter-flow extraction.
The present invention compared with prior art has following outstanding advantage and beneficial effect:
1, the supercritical carbon dioxide extraction anise tree volatile oil can carry out under lower temperature, and extraction selectivity is strong, and the noresidue solvent obtains high yield, high-quality anise tree volatile oil.
2, the anistree powder that has extracted volatile oil is soaked in water, or other extractive techniques such as combining ultrasonic, extracting water temperature range can make shikimic acid fully be dissolved in the water from room temperature to 100 ℃, has improved the rate of transform of shikimic acid, has made full use of anistree resource.
Description of drawings
Fig. 1 is that present main flow is united the process chart that extracts anise tree volatile oil and shikimic acid crude extract method.
Fig. 2 is that the present invention unites the process chart that extracts anise tree volatile oil and shikimic acid crude extract method.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment, but the working of an invention mode is not limited thereto.
Embodiment 1
Fig. 2 is technological process of the present invention, and concrete steps are as follows:
(1) anistree pre-treatment
Anistree dry in the shade naturally, drying is handled to water content 9.6% (use the detection of pharmacopeia toluene band water law, below identical), and mechanical crushing to 20 order is stand-by.
(2) volatile oil extracts
Get the anistree powder of 100 grams, put into 0.5L supercritical carbon dioxide extraction instrument, extracting pressure is 12MPa, 35 ℃ of extraction temperature, one-level separating pressure 10MPa, 55 ℃ of one-level separation temperatures, secondary separation temperature normal temperature, flow 4.5L/h are pressed in the circulation of secondary separating pressure, extracted fuel-displaced 7.8 grams 2 hours.Extract the anistree powder of volatile oil, water content 0.3% is placed, and is stand-by.
(3) extract the shikimic acid crude extract
Get anistree powder 100 grams of said extracted volatile oil, deionized water 400 grams, 75 ℃ were soaked 60 minutes, filtered; Filter cake soaks with 400 gram deionized waters again, and 75 ℃ were soaked 60 minutes, filtered; Repeat again once; Above-mentioned three filtrates are concentrated, decompression, distillation is anhydrated, and obtains the shikimic acid crude extract.The shikimic acid rate of transform 90.3% (having considered to extract the influence of volatile oil, down together) to data.
Embodiment 2
Fig. 2 is technological process of the present invention, and concrete steps are as follows:
(1) anistree pre-treatment
Anistree freeze drying, drying is handled to water content 7.8%, beats to grind to 40 orders, and is stand-by.
(2) volatile oil extracts
Get the anistree powder of 100 grams, put into 0.5L supercritical carbon dioxide extraction instrument, extracting pressure is 18MPa, 45 ℃ of extraction temperature, one-level separating pressure 9MPa, 45 ℃ of one-level separation temperatures, secondary separation temperature normal temperature, flow 6L/h are pressed in the circulation of secondary separating pressure, extracted fuel-displaced 9.2 grams 1.5 hours.Extract the anistree powder of volatile oil, water content 0.1% is placed, and is stand-by.
(3) extract the shikimic acid crude extract
Get anistree powder 100 grams of said extracted volatile oil, deionized water 600 grams, 60 ℃ of adverse currents were soaked 2 hours, and ultrasonic coupling is simultaneously filtered, filtrate decompression, distillation is anhydrated, and obtains the shikimic acid crude extract.The shikimic acid rate of transform 87.7%.
Embodiment 3
Fig. 2 is technological process of the present invention, and concrete steps are as follows:
(1) anistree pre-treatment
Anise dries in the shade naturally, and drying is handled to water content 5.3%, and mechanical crushing to 100 order is stand-by.
(2) volatile oil extracts
Get the anistree powder of 100 grams, put into 0.5L supercritical carbon dioxide extraction instrument, extracting pressure is 24MPa, 40 ℃ of extraction temperature, one-level separating pressure 8MPa, 40 ℃ of one-level separation temperatures, secondary separation temperature normal temperature, flow 4.5L/h are pressed in the circulation of secondary separating pressure, extracted fuel-displaced 9.5 grams 1 hour.Extract the anistree powder of volatile oil, water content 0% is placed, and is stand-by.
(3) extract the shikimic acid crude extract
Get anistree powder 100 grams of said extracted volatile oil, deionized water 1000 grams, 90 ℃ were soaked 20 minutes, filter, filtrate decompression, distillation is anhydrated, and obtains the shikimic acid crude extract.The shikimic acid rate of transform 86.2%.
Embodiment 4
Among the embodiment 3, in the step (3), get anistree powder 100 grams of said extracted volatile oil, deionized water 500 grams, the water logging condition is got 80 ℃ and was soaked 50 minutes, and the gained shikimic acid rate of transform is close with embodiment 3.
Embodiment 5
Among the embodiment 3, in the step (3), get anistree powder 100 grams of said extracted volatile oil, deionized water 700 grams, the water logging condition is got 85 ℃ and was soaked 40 minutes, and the gained shikimic acid rate of transform is close with embodiment 3.
The comparative example 6
Anistree mechanical crushing to 20 order, stand-by.Anistree powder 100 grams, deionized water 600 grams, 40 ℃ were soaked 40 minutes, filtered; Filter cake soaks with 600 gram deionized waters again, and 40 ℃ were soaked 40 minutes, filtered; Repeat again once; Above-mentioned three filtrates are concentrated, decompression, distillation is anhydrated, and obtains the shikimic acid crude extract.The shikimic acid rate of transform 66.3%.The filter cake steam distillation is obtained 4.8 gram volatile oil.
Comparative example 6 is low than embodiment 1～5 at the volatile oil yield and the shikimic acid rate of transform.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spiritual essence of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (8)
1. unite the method for extracting anise tree volatile oil and shikimic acid crude extract for one kind, it is characterized in that comprising following concrete steps:
(1) anistree pre-treatment: anistree drying handled to water content be lower than 10%, be crushed to 20～100 orders;
(2) volatile oil extracts: the anistree powder of handling through step (1) carries out supercritical carbon dioxide extraction and obtains anise tree volatile oil, extraction conditions is: extracting pressure 12～24MPa, 35～45 ℃ of extraction temperature, one-level separating pressure 8～10MPa, 40～55 ℃ of one-level separation temperatures, secondary separation temperature normal temperature is pressed in the circulation of secondary separating pressure, flow 4.5～6L/h extracted 1～2 hour;
(3) extract the shikimic acid crude extract: the anistree powder that step (2) has been extracted volatile oil is soaked in water; 60～90 ℃ of water temperature range; Soak time 20 minutes～2 hours; The solid-liquid weight ratio is 1: 4～10; Filter, filtrate concentrating obtains the shikimic acid crude extract.
2. according to the described method of extracting anise tree volatile oil and shikimic acid crude extract of uniting of claim 1, it is characterized in that: in the described step (1), anistree drying handled to water content be lower than 7%, be crushed to 20～40 orders.
3. according to claim 1 or the 2 described methods of extracting anise tree volatile oil and shikimic acid crude extract of uniting, it is characterized in that: drying method is that nature dries in the shade or freeze drying in the described step (1), and breaking method is to shear to pulverize or beat to grind.
4. a kind of method of extracting anise tree volatile oil, shikimic acid crude extract of uniting according to claim 1, it is characterized in that: in the described step (3), water temperature range is 75～85 ℃; Soak time is 40 minutes～60 minutes; The solid-liquid weight ratio is 1: 5～7.
5. according to the described method of extracting anise tree volatile oil and shikimic acid crude extract of uniting of claim 1, it is characterized in that: in the described step (3), the immersion water is a soft water.
6. according to the described method of extracting anise tree volatile oil and shikimic acid crude extract of uniting of claim 6, it is characterized in that: in the described step (3), the immersion water is a deionized water.
7. according to the described method of extracting anise tree volatile oil and shikimic acid crude extract of uniting of claim 1, it is characterized in that: in the described step (3), the water logging bubble is intermittence, continuous or adverse current immersion.
8. according to the described method of extracting anise tree volatile oil and shikimic acid crude extract of uniting of claim 1, it is characterized in that: in the described step (3), adopt ultrasonic coupling in the water logging bubble process.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008101985927A CN101371700A (en) | 2008-09-17 | 2008-09-17 | Method for unitedly extracting anise tree volatile oil and shikimic acid crude extract |
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| CNA2008101985927A CN101371700A (en) | 2008-09-17 | 2008-09-17 | Method for unitedly extracting anise tree volatile oil and shikimic acid crude extract |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101851552A (en) * | 2010-06-11 | 2010-10-06 | 淮海工学院 | Extracting method of blackberry seed oil |
| CN101560150B (en) * | 2009-05-22 | 2013-01-09 | 中国科学院广州化学研究所 | Method for extracting shikimic acid from aniseed |
| CN106278873A (en) * | 2016-08-19 | 2017-01-04 | 广西甙元植物制品有限公司 | A kind of production technology extracting separation shikimic acid from anise |
-
2008
- 2008-09-17 CN CNA2008101985927A patent/CN101371700A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101560150B (en) * | 2009-05-22 | 2013-01-09 | 中国科学院广州化学研究所 | Method for extracting shikimic acid from aniseed |
| CN101851552A (en) * | 2010-06-11 | 2010-10-06 | 淮海工学院 | Extracting method of blackberry seed oil |
| CN106278873A (en) * | 2016-08-19 | 2017-01-04 | 广西甙元植物制品有限公司 | A kind of production technology extracting separation shikimic acid from anise |
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Application publication date: 20090225 |