CN101781602A - Method for extracting allium mongolicum regel seed oil by using supercritical carbon dioxide - Google Patents
Method for extracting allium mongolicum regel seed oil by using supercritical carbon dioxide Download PDFInfo
- Publication number
- CN101781602A CN101781602A CN 201010121714 CN201010121714A CN101781602A CN 101781602 A CN101781602 A CN 101781602A CN 201010121714 CN201010121714 CN 201010121714 CN 201010121714 A CN201010121714 A CN 201010121714A CN 101781602 A CN101781602 A CN 101781602A
- Authority
- CN
- China
- Prior art keywords
- extraction
- carbon dioxide
- allium mongolicum
- mongolicum regel
- supercritical carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Extraction Or Liquid Replacement (AREA)
- Edible Oils And Fats (AREA)
Abstract
The invention relates to a method for extracting allium mongolicum regel seed oil by using supercritical carbon dioxide, belonging to the field of food processing and specially used for comprehensive development and deep processing of allium mongolicum regel seeds. The allium mongolicum regel (Allium Mongolicum Regel) seeds are dried (the water content is smaller than 6 percent) and crushed into 20-40 meshes, the allium mongolicum regel seed oil is extracted by adopting an supercritical carbon dioxide extraction technology, and the optimal process parameters are set as follows: the extraction pressure is 31.50MPa, the extraction temperature is 46.00 DEG C and the extraction time is 101.60min. Under the conditions, yellow decant oily substances are obtained with the purity of above 99 percent and the maximum extraction yield of 15.067 percent. The process for extracting the allium mongolicum regel seed oil by using the supercritical carbon dioxide provides a new method for deep processing of the allium mongolicum regel seeds and has the advantages of strong operability, higher yield, high extraction efficiency, high product purity, little damage of active components, favorable safety, favorable repeatability and the like.
Description
One, technical field
The present invention relates to the method for extracting allium mongolicum regel seed oil by using supercritical carbon dioxide, belong to the food-processing field, be exclusively used in the extraction allium mongolicum regel seed oil.
Two, background technology
Husky green onion is Liliaceae (LiLiaceae) allium (Allium) plant, and formal name used at school Mongolia fragrant-flowered garlic (AlliumMongolicum Regel) is called Mongolian green onion, mountain green onion, is a kind of perennial bulb herbaceous plant.Be distributed in the ground such as the Inner Mongol, Gansu, Xinjiang of Mongolia south, Russia and Kazakhstan and NORTHWEST CHINA.Compendium of Material Medica is put down in writing the medicinal efficacy of husky green onion: the same green onion of distinguishing the flavor of, and suffering, tepor, nontoxic.Cure mainly: the contact dermatitis poison, chigger in the mountain stream, penetrate poison such as worker, to remove miasma vicious; Liquor soaks, or smashes and tie up, the big effect.Double rocambole, flourish cornel, not private, cure mainly and let out essence.Eat strong will benefit courage for a long time.Husky green onion over-ground part is gone into anaesthetic, can whet the appetite, helps digestion, desinsection, and the laudatory title of " glossy ganoderma in the dish " is arranged, food can control dysentery with red and white feces, enteritis, diarrhoea, all diseases of the obstruction of qi in the chest.Often eat and can strengthen children's intelligence, improve immunologic function, can effectively prevent the generation of senile dementia, can also suppress the abnormality proliferation with inverse cancer cell, longevity makes for good health.According to the Shennong's Herbal record, husky green onion seed medicinal efficacy is close with the shallot seed, and it distinguishes the flavor of hot, and temperature is returned lung, liver, stomach warp, classifies middle product as, and it is smart to have the bowl spares benefit, the effect of eyesight improvement powder medicine wind, and it is dizzy to be used to suffer from a deficiency of the kidney, common cold caused by wind-cold.Contain beneficial fatty acids such as oleic acid, linolic acid, eicosanoic acid, palmitinic acid and linolenic acid in the husky green onion seed, and vitamins C and β-Gu Zaichun isoreactivity composition.
In recent years, mainly concentrate on extraction, separation and the analysis aspect of volatile oil for the research of husky green onion active constituents of medicine, less to the research of seed.At present, from plant seed, extract greasy method solvent refluxing extraction method, cold-maceration, hot moulding method, supercritical carbon dioxide extraction method, ultrasonic extraction method, microwave extraction method etc. are arranged.But take all factors into consideration from extraction efficiency, product purity, dissolvent residual problem equal angles, that the supercritical carbon dioxide extraction technology has is easy to operate, energy consumption is low, extraction efficiency is high, the product purity advantages of higher, as a kind of more satisfactory extracting method, has very vast potential for future development.(Response Surface Method (RSM, Response surface methodology) sees reference document: Siti Machmudah, Yukari Kawahito, Mitsuru Sasaki, Motonobu Goto.Supercritical CO
2Extraction of rosehip seedoil:Fatty acids composition and process optimization.J.of Supercritical Fluids.41:2007,421-428.) be the synthetic of Statistic Design experimental technique, it comprise experimental design, modeling, testing model well-formedness, factorial effect assessment, investigate and seek factor optimum operation condition, the response surface method successfully is applied to many aspects of biotechnology in recent years.
Three, summary of the invention
Problems such as technical problem the present invention aims to provide a kind of method of extracting allium mongolicum regel seed oil by using supercritical carbon dioxide, and organic solvent residual, the product purity that exists with solution traditional method for extracting Vegetable oil lipoprotein is low, the aesthetic quality is poor, the extraction yield is low.
Technical scheme embodiment of the present invention are as follows:
1. the method for extracting allium mongolicum regel seed oil by using supercritical carbon dioxide comprises:
(1) raw material: sophisticated wild husky green onion seed, cross scalping and remove dust and impurity, clear water rinsing, material cleanliness 〉=99%;
(2) drying: husky green onion seed is dried naturally or place 40 ℃ of oven dry of electric heating constant temperature air dry oven, water content gets final product less than 6%;
(3) pulverize: the husky green onion seed that will dry is pulverized and sieving for standby, and granularity is 20～40 orders;
(4) supercritical carbon dioxide extraction: the husky green onion seed after the above-mentioned pulverizing is placed the supercritical carbon dioxide extraction still, regulate extracting pressure 25～35Mpa, 40～50 ℃ of extraction temperature, extraction time 40～120min, carbon dioxide flow 40Kg/h separates I pressure 8～10MPa, 45 ℃ of temperature, separate II pressure 5～7MPa, 35 ℃ of temperature.Collect purified allium mongolicum regel seed oil with triangular flask in the separating still exit.Allium mongolicum regel seed oil extraction yield (%)=oil extraction amount (g)/charge amount (g) * 100%.
Utilize Design Expert (Static Made Easy, Minneapolis, MN, USA.version 7.1.1,2006) software carries out regression analysis to the extracting method experimental data of allium mongolicum regel seed oil, the secondary multivariate regression model that draws: Y=14.645+0.55324x
1+ 0.39503x
2+ 0.71336x
3+ 0.19320x
1x
2-0.30193x
1x
3+ 0.3589x
2x
3-0.62431x
1 2-0.77284x
2 2-0.42996x
3 2X in the model
1: be encoded radio, the x of pressure independent variable(s)
2: be encoded radio, the x of temperature independent variable(s)
3: be the encoded radio (x of time independent variable(s)
i=(X
i-X
0)/Δ X encodes to independent variable(s), wherein x
iBe the encoded radio of independent variable(s), X
iBe the actual value of independent variable(s), X
0Be the actual value of experimental center point place independent variable(s), Δ X is the change step of independent variable(s)), Y is the allium mongolicum regel seed oil yield.This model can dope the extracting allium mongolicum regel seed oil by using supercritical carbon dioxide yield, and extracts the technology of allium mongolicum regel seed oil by this secondary multivariate regression model optimization.Optimum parameter is optimized for extracting pressure 31.50MPa in its supercritical carbon dioxide extraction process, 46.00 ℃ of extraction temperature, extraction time 101.60min.
Beneficial effect the present invention utilizes supercritical carbon dioxide extraction method to extract husky green onion seed vegetables oil, and the Response Surface Method of using in the DesignExpert software (RSM) is carried out process optimization, set up the process modeling of extracting allium mongolicum regel seed oil by using supercritical carbon dioxide, for the industrial application of this technology provides call parameter.Compare with general grease extracting method, this invention has following advantage:
1. the inventive method is simple, and is workable, and processing parameter main in the extraction process is optimized, and shortened extraction time to a certain extent, improved extraction efficiency and grease yield, and the maximum extraction yield is 15.096%.
2. the present invention utilizes supercritical carbon dioxide extraction method to extract allium mongolicum regel seed oil, has solved organic solvent residual, extraction selectivity is poor, product purity is low and problem such as environmental pollution, and products obtained therefrom is yellow clarification oily matter, has the special local flavor of allium mongolicum regel seed oil; Purity is more than 99%.
3. the optimum process condition that obtains of present method optimization is comparatively gentle, easy handling, and repeatability is strong, when realizing allium mongolicum regel seed oil maximum extraction yield, has also guaranteed the stable of activeconstituents in the product.
4. allium mongolicum regel seed oil supercritical carbon dioxide method for extracting provided by the invention, the industry that can directly apply to husky green onion seed is extracted, and is its further development and use in fields such as food chemical industry condition that facilitates.
Four, description of drawings
Allium mongolicum regel seed oil extraction yield (%)=oil extraction amount (g)/charge amount (g) * 100%.A: pressure; B: temperature; C: time.
Fig. 1 is response surface 3D and the corresponding isogram that pressure and temperature influence allium mongolicum regel seed oil extraction yield.
Time value is fixed as C:80min, A: pressure, B: temperature.
Fig. 2 is response surface 3D and the corresponding isogram that pressure and time allium mongolicum regel seed oil extraction yield is influenced.
Temperature value is fixed as B:45 ℃, A: pressure, C: time.
Fig. 3 is response surface 3D and the corresponding isogram of temperature and time to the influence of allium mongolicum regel seed oil extraction yield.
Force value is fixed as A:30MPa, B: temperature, C: time.
Five, embodiment
(Response Surface Method (RSM) Box-Behnken model among the employing Design Expert of statistical software sees reference document: Box GEP.Multifactor designs of first order.Biometrika 1952; 39:49-57. with Box GEP, Behnken DW.Some new three level design for the study of quantitative variables.Technometrics 1960; 2:455-75.) design and data analysis experimentize.Selective pressure, temperature, time is the independent variable(s) of face experiment in response, and allium mongolicum regel seed oil extraction yield is as dependent variable.Each independent variable(s) is set three parameter levels respectively: pressure 25MPa, 30MPa, 35MPa, and 40 ℃, 45 ℃, 50 ℃ of temperature, the time is 40min, 80min, 120min, and three levels are represented with code-1,0,1 respectively.
According to the experimental group number of Box-Behnken pattern layout, carry out 17 groups of response surface random experiments.Experimental result is carried out secondary multiple regression match, obtain coding dependent variable (allium mongolicum regel seed oil yield Y) coding independent variable(s) (extracting pressure x
1, temperature x
2, time x
3) the multinomial regression equation of secondary:
Y＝14.645+0.55324x
1+0.39503x
2+0.71336x
3+0.19320x
1x
2-0.30193x
1x
3+0.35890x
2x
3-0.62431x
1 2-0.77284x
2 2-0.42996x
3 2
Above-mentioned regression model is carried out variance analysis, and the result shows that this model has utmost point significance (P＜0.001), and coefficient (Adj R-Squared) Adj R is determined in the adjustment of model
2=0.9744, illustrate that this model can explain that 97.44% response value changes.Therefore, this model-fitting degree is good, and testing error is little, and this model is suitable, can analyze the extracting allium mongolicum regel seed oil by using supercritical carbon dioxide yield and predicts with this model.Model is carried out the test of significance of regression equation coefficient, obtain an once x of model
1, x
3With quadratic term x
1 2, x
2 2(p＜0.0001) is extremely remarkable, once an x
2, mutual x
1x
2, x
1x
3, x
2x
3With quadratic term x
3 2Significant difference shows pressure, temperature, time factor, and the interaction of pressure and temperature, pressure and time, temperature and time has remarkably influenced to yield, as Fig. 1, shown in 2,3.By regression model optimization, obtaining best extraction process parameter is extracting pressure 31.50MPa, 46.00 ℃ of extraction temperature, and extraction time 101.60min, the maximum yield of prediction allium mongolicum regel seed oil is 15.067%.
Embodiment
The extracting allium mongolicum regel seed oil by using supercritical carbon dioxide method is as follows:
(1) raw material: sophisticated wild husky green onion seed, material cleanliness 〉=99%;
(2) drying: husky green onion seed dried naturally or place 40 ℃ of oven dry down of electric heating constant temperature air dry oven, water content is less than 6%;
(3) pulverize: the husky green onion seed that will dry is pulverized and sieving for standby, and granularity is 20～40 orders;
(4) supercritical carbon dioxide extraction: the husky green onion seed after the above-mentioned pulverizing is placed supercritical carbon dioxide extraction apparatus (HA121-50-01 type supercritical extraction unit, the production of Huaan, Nantong supercritical extraction company limited) in the extraction kettle, set optimal processing parameter: extracting pressure 31.50MPa, 46.00 ℃ of extraction temperature, extraction time 101.60min, CO
2Flow 40Kg/h separates I pressure 8～10MPa, and 45 ℃ of temperature are separated II pressure 5～7MPa, 35 ℃ of temperature.Collect purified allium mongolicum regel seed oil with triangular flask in the separating still exit.
The gained allium mongolicum regel seed oil is yellow, clarifying oily matter, and purity is more than 99%; Maximum extraction yield predictor is 15.067%, and measured value is 14.93%～15.12%, conforms to predictor.
In the method for the described extracting allium mongolicum regel seed oil by using supercritical carbon dioxide of above-mentioned example, can effectively carry out extracting allium mongolicum regel seed oil by using supercritical carbon dioxide by the parameters that Response Surface Method (RSM) the Box-Behnken model among the Design Expert of statistical software obtains, improve extraction efficiency greatly, can be used for extraction in the production allium mongolicum regel seed oil.Equipment and technology that pre-treatment of the present invention requires are also fairly simple, have good market outlook.
Claims (3)
1. the method for extracting allium mongolicum regel seed oil by using supercritical carbon dioxide
(1) raw material: sophisticated wild husky green onion seed, to cross scalping and remove dust and impurity, the clear water rinsing reaches more than 99% the material cleanliness;
(2) drying: husky green onion seed dried naturally or place 40 ℃ of oven dry down of electric heating constant temperature air dry oven, water content is less than 6%;
(3) pulverize: the husky green onion seed that will dry is pulverized and sieving for standby, and granularity is 20～40 orders;
(4) supercritical carbon dioxide extraction: the husky green onion seed after the above-mentioned pulverizing is placed the supercritical carbon dioxide extraction still, regulate extracting pressure 25～35Mpa, 40～50 ℃ of extraction temperature, extraction time 40～120min, CO
2Flow 40Kg/h separates I pressure 8～10MPa, and 45 ℃ of temperature are separated II pressure 5～7MPa, 35 ℃ of temperature; Collect purified allium mongolicum regel seed oil in the separating still exit.
2. allium mongolicum regel seed oil supercritical carbon dioxide method for extracting according to claim 1, its extraction process parameter is: extracting pressure 31.50MPa, 46.00 ℃ of extraction temperature, extraction time 101.60min.
3. the product that method obtained of claim 1 or 2 described extracting allium mongolicum regel seed oil by using supercritical carbon dioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010121714 CN101781602A (en) | 2010-03-11 | 2010-03-11 | Method for extracting allium mongolicum regel seed oil by using supercritical carbon dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010121714 CN101781602A (en) | 2010-03-11 | 2010-03-11 | Method for extracting allium mongolicum regel seed oil by using supercritical carbon dioxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101781602A true CN101781602A (en) | 2010-07-21 |
Family
ID=42521756
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010121714 Pending CN101781602A (en) | 2010-03-11 | 2010-03-11 | Method for extracting allium mongolicum regel seed oil by using supercritical carbon dioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101781602A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106106842A (en) * | 2016-06-24 | 2016-11-16 | 山东天博食品配料有限公司 | A kind of goldball onion quintessence oil and preparation method thereof |
| CN107723094A (en) * | 2017-11-08 | 2018-02-23 | 海南师范大学 | A kind of supercritical CO2The method for extracting miracle fruit seed essential oil |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321735A (en) * | 2001-05-24 | 2001-11-14 | 南京农业大学 | Method for extracting onion oil |
| CN101508937A (en) * | 2009-03-12 | 2009-08-19 | 中山大学 | Supercritical method for extracting nutmeg essential oil with carbonic anhydride |
| CN101560438A (en) * | 2009-05-13 | 2009-10-21 | 南京农业大学 | Supercritical carbon dioxide extraction method of fistular onion seed oil |
-
2010
- 2010-03-11 CN CN 201010121714 patent/CN101781602A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321735A (en) * | 2001-05-24 | 2001-11-14 | 南京农业大学 | Method for extracting onion oil |
| CN101508937A (en) * | 2009-03-12 | 2009-08-19 | 中山大学 | Supercritical method for extracting nutmeg essential oil with carbonic anhydride |
| CN101560438A (en) * | 2009-05-13 | 2009-10-21 | 南京农业大学 | Supercritical carbon dioxide extraction method of fistular onion seed oil |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106106842A (en) * | 2016-06-24 | 2016-11-16 | 山东天博食品配料有限公司 | A kind of goldball onion quintessence oil and preparation method thereof |
| CN107723094A (en) * | 2017-11-08 | 2018-02-23 | 海南师范大学 | A kind of supercritical CO2The method for extracting miracle fruit seed essential oil |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Ballesteros et al. | Optimization of autohydrolysis conditions to extract antioxidant phenolic compounds from spent coffee grounds | |
| CN103555412B (en) | Method for extracting tea-seed oil | |
| US20210275940A1 (en) | System and Method For Continuous Stirred Tank Solvent Extraction Using Feedstock | |
| CN101732359B (en) | Integrated method for poly-generation of Chinese medicinal extracts | |
| CN106036928B (en) | A kind of pure natural wild walnut is crushed and Kernel-hull separation method | |
| CN101775333A (en) | Supercritical CO2 method for extracting barbadosnut seed oil and product thereof | |
| CN101690525B (en) | Method for extracting myrica seed oil | |
| CN103374456A (en) | Method for extracting vegetable oil through microbiological fermentation | |
| CN105602719A (en) | Supercritical extraction method of tea oil | |
| CN101781602A (en) | Method for extracting allium mongolicum regel seed oil by using supercritical carbon dioxide | |
| CN101451089A (en) | Method for extracting Chinese chive seed oil by supercritical carbon dioxide | |
| Guemghar et al. | Phenolic compounds from artichoke (Cynara scolymus L.) byproducts: optimization of microwave assisted extraction and enrichment of table oil | |
| CN101555434A (en) | Process for extracting herpetospermum pedunculosum seed oil by supercritical CO* | |
| CN103937610A (en) | Extraction technology for essential oil | |
| CN101560438A (en) | Supercritical carbon dioxide extraction method of fistular onion seed oil | |
| CN102051261A (en) | Method for continuously extracting lacquer wax and lacquer by supercritical CO2 fluid | |
| CN101781603A (en) | Method for extracting brassica rapa l. seed oil by using supercritical carbon dioxide | |
| CN103829242A (en) | Health-care food containing fruit of nitraria red pigment | |
| CN101006823B (en) | Preparation method of apple seeds protein | |
| CN101390975A (en) | Extraction method of citrus active ingredient | |
| CN109536273A (en) | The technique of fatty acid substance in a kind of supercritical fluid extraction sesame | |
| CN110373262A (en) | A kind of Lai wood fruit oil refinement method of low-cost and high-quality | |
| CN115119931A (en) | Production method for producing four pepper products | |
| CN103571614A (en) | Preparation method of castor oil and castor oil prepared through same | |
| CN103432205A (en) | Novel method for extracting high-purity lotus leaf flavone |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20100721 |