CN1683481A - Process for extracting anise oil and anisoxide - Google Patents
Process for extracting anise oil and anisoxide Download PDFInfo
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- CN1683481A CN1683481A CNA2004100305824A CN200410030582A CN1683481A CN 1683481 A CN1683481 A CN 1683481A CN A2004100305824 A CNA2004100305824 A CN A2004100305824A CN 200410030582 A CN200410030582 A CN 200410030582A CN 1683481 A CN1683481 A CN 1683481A
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- essence
- fructus foeniculi
- extracting method
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- aniseed oil
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Abstract
Fresh anise fruit as material is processed through crushing, 95 % concentration alcohol soaking, grinding, centrifugal solid-liquid separation, decompression distillation, concentration to recover alcohol, extraction of the concentrate with ethyl acetate to obtain anise oil. Through further cold precipitation, anisoxide is separated. The extraction is not heated and has less damage of the heat sensitive matter in anise, and the natural scent and bioactivity of anise maintained.
Description
Technical field
The present invention relates to natural product extraction, particularly the method for star aniseed oil extraction.
Technical background
Star anise
Nature and flavor with return through Xin Wen.Return liver, kidney, spleen, stomach warp.Function and notes are controlled: warming YANG to expel cold, regulating QI to relieve pain.Be used for cold hernia stomachache, lumbago due to renal deficiency, gastrofrigid vomiting, coldness and pain in the epigastrium [Zheng Zhanhu etc., Chinese medicine modern study and application, Xueyuan Press, 1997, Beijing].
Main component: in the volatile oil based on trans phenylmethylether (trans-anethole) [Ceng Guanxiong etc., herbal medicine, 1983; 14 (9) 19], also contain fenchone (anisgl acetone) and α-Pai Xi (α-pinene) amphene (camphene) borneol [Chen Yaozu etc., analytical chemistry, 1986 such as (bomeol); 14 (11); 853] 3-rutinose, 3-glucose and galactoside (3-rutinosides, 3-glucosidesand3-galactosidesof kaempferol and querctin) [CA, 1981 of, also containing flavonoid such as kaempferol and Quercetin in addition; 95; 217683w] sesquiterpene lactones class [Okuyama Emi et al.Chem pharm Bull, 1993; 41 (9) 1670], β-Gu Zaichun ([CA, 1987 such as vitamin-E of β-sitosterol); 107; 57610f].
The volatile oil that adopts sherwood oil refluxing extraction and steam distillation to extract the star anise base of leaf again can obtain 1.9% yield [Huang Xiangzhong, Funing, Yunnan star anise warp and leaf volatile oil chemical constitution study, Yunnan chemical, 2002,29 (6)].
Pharmacological research shows that Fructus Anisi Stellati extract has antihistaminic effect [Yao Zhicheng, herbal medicine, 1985; 16 (2); 22], the phenylmethylether that star anise is extracted has function of increasing leukocyte [Song Shuyuan, pharmacy circular, 1980,15 (3); 46], have antioxygenation [family Tian Jingnan, foreign medical science, traditional Chinese medicine fascicle, 1993,1 (15); 37], have anti-microbial effect, the Gram-positive negative bacteria is all had restraining effect [the new medical college in Jiangsu.Chinese medicine voluminous dictionary (first volume) Shanghai; Shanghai science tech publishing house, 1986; 27], olium anisi has antimycotic effect [Li Jian, the experimental observation of three kinds of traditional medicine volatile oil antifungic actions, Chinese ecological magazine, 1,997 9 (3); 31], generate aubepine [the easy Feng Ping etc. of high value after the star aniseed oil ozonize, ozonization method is produced the research of phenyl aldehyde and aubepine, Guangxi University's journal (natural science edition) 1998,23 (3)], the cough syrup that adopts the star aniseed oil preparation is the good medicine [Xue Daquan of treatment cough clinically, cyclodextrin inclusion technique improves the research of cough syrup quality, Chinese patent medicine, 2001,23 (12)].
Experiment shows that the extraction temperature effect of volatile oil material is fairly obvious, adopting its poor yields of different process for extracting is the 8.8 times of [Li Xiuqin of distillation extraction of seething with excitement apart from very outstanding as Radix Bupleuri volatile oil at 65 ℃ supercritical extraction yield, Sun Xiuyan, He Chonggui, the research of Radix Bupleuri volatile oil extracting method, Chinese Pharmaceutical Journal, 39 (2) 103], Rhizoma Curcumae volatile oil extracts and studies show that: adopt the supercritical extraction Rhizoma Curcumae volatile oil, contain the fragrant alkene of β-pull in the Rhizoma Curcumae volatile oil, Curcumenol, isocurcumenol, curdione, wherein curdione is higher and adopt the Rhizoma Curcumae volatile oil of aqueous vapor distillation extraction to contain curdione seldom, the Rhizoma Curcumae volatile oil fragrance of supercritical extraction is pure, natural flavor, and the Rhizoma Curcumae volatile oil fragrance of aqueous vapor distillation extraction Rhizoma Curcumae volatile oil and supercritical extraction has significant difference, this has illustrated because the supercritical extraction temperature is not destroyed than the material that hangs down a large amount of easy oxidations of thermo-sensitivity, and the aqueous vapor distillation extraction is owing to make heat-sensitive materials produce heated denaturalization in heating condition for a long time.The volatile oil of star anise belongs to fragrant class material together and obviously adopts the aqueous vapor distillating method to extract its composition and the fragrance local flavor all can be affected, but the technology great majority of existing production star anise volatile oil adopt the aqueous vapor distillating method to extract, disclosed 96118216.4 " from the fennel calamus plant, the extracting the processing method of essential oil " of patent gazette, " 90107883.2 with the method for preparing edible perfume with wild star-anise ", " 90109568.0 anistree essence and production method thereof " all is to adopt the aqueous vapor distillating method, because the restriction of extractive technique fails to make this natural product of star anise to realize due economic worth and social benefit.
Summary of the invention
The present invention will provide a kind of can keep the effective constituent of star anise natural product and keep the star anise natural flavor, and the pure star aniseed oil of fragrance also extracts the star anise essence simultaneously and exempts to heat process for extracting to improve star anise natural product utility value.
The present invention is achieved in that the aquatic foods product star anise fruit that will gather shreds as in the container with clipper, add 95% alcohol immersion, the broken end of aquatic foods product star anise fruit and 95% alcohol mixed solution are placed in the sealing ball mill container in the machine, ball milling in ball mill, the bump repeatedly at mechanical milling process abrading-ball and the broken end of star anise fruit, make star anise fruit tissue cell in the environment that organic solvent soaks, be subjected to the function cells fragmentation of pressure, intracellular composition is dissolved in 95% ethanolic soln after the cytoclasis, star anise fruit tissue cell is subjected to the effect of pressure to make cytomorphosis even without broken owing to clashing into repeatedly in the environment that organic solvent soaks, cell compressive deformation smaller volume, it is big that smaller volume ICP power becomes, volume became big when decompression was strong after the bump, little alternation when big during cell volume, its internal volume of cell volume alternation changes thereupon, volume pressure increased when its internal volume diminished, volume pressure diminished when its internal volume became big, ICP power changes the cell walls permeability and increases, the increase of cell permeability helps solvent convection current inside and outside cell, back and forth the solvent of cell walls both sides convection current will be dissolved in the solvent with intercellular solvable composition in the cell, fully will contain star anise fruit activeconstituents and star anise fruit fibre solidity thing mixing solutions whizzer centrifugation solidity thing after the ball milling, fiber solidity thing is discarded, extracting centrifugal liquid, centrifugate is put negative pressure evaporation to be reclaimed 95% ethanol mixing solutions is concentrated, negative pressure is controlled at≤5pa, make moisture in the fresh fruit and 95% ethanol≤35 ℃ of evaporations, be concentrated into and 1/4 of bright product star anise fruit weight, the ethyl acetate that adds 2 times of volumes then, stir after adding ethyl acetate, stirring is placed on after finishing in 5 ℃ of environment and made the species precipitate that is not dissolved in ethyl acetate solvent in cold heavy 24 hours, get supernatant liquor then, supernatant liquor is put the negative pressure system evaporation, negative pressure is controlled at≤5pa, moisture and ethyl acetate evaporation are waved≤35 ℃ of temperature controls and get star anise olium anisi to the greatest extent afterwards, the whole process temperature of extracting all under≤35 ℃ condition, makes the temperature-sensitive class material in the star aniseed oil not be subjected to heat collapse.
Cold heavy throw out is put negative pressure system evaporate, negative pressure is controlled at≤5pa, moisture and ethyl acetate evaporation are waved≤35 ℃ of temperature controls and get the star anise essence to the greatest extent afterwards.
Embodiment 1 star aniseed oil and Fructus Foeniculi essence extracting method:
The first step: get 10 kilograms of bright star anise fruits.
Second step: bright star anise fruit is shredded.
The 3rd step: will shred bright star anise fruit and be soaked in 100 liter of 95% ethanolic soln, soaked 10 hours.
The 4th mends: shredder grinding 10 hours is put at the broken end of star anise fruit that will be soaked in ethyl acetate solution.
The 5th step: the star anise fruit mixing solutions that will grind 10 hours adopts whizzer centrifugation solidity thing, gets fluidity thing (the solidity thing discards).
The 6th step: the centrifugate underpressure distillation is concentrated, is decompressed to≤5Pa, temperature control≤35 ℃, distillation is reclaimed ethanol, is distilled to 2.5 liters of concentrated solutions.
The 7th step: in 2.5 liters of concentrated solutions, add 5 liters of ethyl acetate, add afterwards and fully stir.
The 8th step: place 5 ℃ of freezers cold heavy after stirring.
The 9th step: cold heavy afterwards supernatant liquor the separation with throw out.
The tenth step: the supernatant liquor underpressure distillation is concentrated, is decompressed to≤5Pa, temperature control≤35 ℃, ethyl acetate is reclaimed in distillation, evaporating water gets star aniseed oil.
The 11 step: the throw out underpressure distillation is concentrated, is decompressed to≤5Pa, temperature control≤35 ℃, ethyl acetate is reclaimed in distillation, evaporating water gets the star anise essence.
Claims (6)
1, the extracting method of a kind of star aniseed oil and Fructus Foeniculi essence is characterized in that: (1) chooses that bright star anise fruit, (2) shred, (3) immersion, (4) ball milling, (5) centrifugal solid-liquid separate, (6) underpressure distillation is reclaimed ethanol and concentrated that cold heavy (9) supernatant liquor separates (10) supernatant liquor underpressure distillation (11) throw out underpressure distillation evaporating water in (8) 5 ℃ of freezers of (7) ethyl acetate extraction with throw out.
2, it is characterized in that by the extracting method of described star aniseed oil of claim 1 and Fructus Foeniculi essence star anise chooses bright product fruit.
3, the extracting method by described star aniseed oil of claim 1 and Fructus Foeniculi essence is characterized in that star anise ball milling in 95% ethanolic soln.
4, by the extracting method of described star aniseed oil of claim 1 and Fructus Foeniculi essence it is characterized in that underpressure distillation concentrates, pressure≤5Pa, temperature control≤35 ℃.
5, the extracting method by described star aniseed oil of claim 1 and Fructus Foeniculi essence is characterized in that separating in the concentrated solution olium anisi ethyl acetate extraction.
6, the extracting method by described star aniseed oil of claim 1 and Fructus Foeniculi essence is characterized in that separating out cold sinking in 5 ℃ of freezers of Fructus Foeniculi essence.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2004100305824A CN1683481A (en) | 2004-04-12 | 2004-04-12 | Process for extracting anise oil and anisoxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2004100305824A CN1683481A (en) | 2004-04-12 | 2004-04-12 | Process for extracting anise oil and anisoxide |
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| CN1683481A true CN1683481A (en) | 2005-10-19 |
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| CNA2004100305824A Pending CN1683481A (en) | 2004-04-12 | 2004-04-12 | Process for extracting anise oil and anisoxide |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102651978A (en) * | 2009-12-16 | 2012-08-29 | 株式会社钟化 | Method for producing flavoring agent, and flavoring agent |
| CN102872185A (en) * | 2012-09-21 | 2013-01-16 | 大连民族学院 | Method for ultrasonically extracting coumarin from alfalfa |
| CN104974853A (en) * | 2015-07-17 | 2015-10-14 | 王再青 | Method for extracting peppermint essential oil |
| CN105062686A (en) * | 2015-07-17 | 2015-11-18 | 王再青 | Method for extracting lavender essential oil |
| CN109497493A (en) * | 2018-12-11 | 2019-03-22 | 唐国文 | A kind of cooking wine and preparation method thereof containing star anise extract |
-
2004
- 2004-04-12 CN CNA2004100305824A patent/CN1683481A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102651978A (en) * | 2009-12-16 | 2012-08-29 | 株式会社钟化 | Method for producing flavoring agent, and flavoring agent |
| CN103783626A (en) * | 2009-12-16 | 2014-05-14 | 株式会社钟化 | Method for producing flavoring agent, and flavoring agent |
| CN102872185A (en) * | 2012-09-21 | 2013-01-16 | 大连民族学院 | Method for ultrasonically extracting coumarin from alfalfa |
| CN102872185B (en) * | 2012-09-21 | 2014-05-07 | 大连民族学院 | Method for ultrasonically extracting coumarin from alfalfa |
| CN104974853A (en) * | 2015-07-17 | 2015-10-14 | 王再青 | Method for extracting peppermint essential oil |
| CN105062686A (en) * | 2015-07-17 | 2015-11-18 | 王再青 | Method for extracting lavender essential oil |
| CN109497493A (en) * | 2018-12-11 | 2019-03-22 | 唐国文 | A kind of cooking wine and preparation method thereof containing star anise extract |
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