CN101451089A - Method for extracting Chinese chive seed oil by supercritical carbon dioxide - Google Patents
Method for extracting Chinese chive seed oil by supercritical carbon dioxide Download PDFInfo
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- CN101451089A CN101451089A CNA2008101237682A CN200810123768A CN101451089A CN 101451089 A CN101451089 A CN 101451089A CN A2008101237682 A CNA2008101237682 A CN A2008101237682A CN 200810123768 A CN200810123768 A CN 200810123768A CN 101451089 A CN101451089 A CN 101451089A
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- leek
- chinese chive
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Abstract
The invention relates to a method for extracting leek rapeseed oil through supercritical carbon dioxide, which belongs to the field of food processing and is specially used for deep processing of leek rapeseeds. The raw materials and the technology comprise the following: the leek rapeseeds are dried and crushed and subjected to supercritical CO2 extraction; the extraction temperature is 40.40 DEG C, the extraction time is 86.70 minutes, and the extraction pressure is 22.25 MPa; the leek rapeseed oil is extracted; and the purity of the leek rapeseed oil is more than 99 percent, and the yield of the leek rapeseed oil is between 17.23 and 17.52 percent. The invention provides a novel method for deeply processing the leek rapeseeds. The method has the advantages of strong maneuverability, good safety, higher yield and good repeatability.
Description
One, technical field
The present invention relates to supercritical CO
2Extract the method for Chinese chive seed oil, belong to the food-processing field, be exclusively used in the extraction of Chinese chive seed oil.
Two, background technology
Leek (Allium tuberosum Rottl.) is the perennial perennial root herbaceous plant of Liliaceae allium, originates in China.Having another name called fragrant-flowered garlic, Folium Allii tuberosi, is the long a kind of ancient vegetables of cultivation history.The leek seed is the dry mature seed of liliaceous plant leek.The leek seed is warm in nature, and flavor is hot, sweet.Has warm invigorating the liver and kidney, supporing yang controlling nocturnal emission with astringent drugs.Be used for impotence and seminal emission, soreness of waist and knee joint, enuresis frequent micturition, leukorrhea turbid down (document sees reference: " Chinese pharmacopoeia 2005 editions).The Chinese chive seed oil fatty acid component is: palmitinic acid, linolic acid, oleic acid, stearic acid, eicosanoic acid, arachidonic acid etc., contain sulfocompound, flavonoid glycoside, alkaloid, vitamins C isoreactivity composition in addition.
Organic solvent extraction method and water at atmospheric pressure vapor distillation extraction method are adopted in the extraction of Chinese chive seed oil at present.The atmospheric steam distillation and extraction method need be at 100 ℃, and the normal atmosphere about 101kpa is distillation down, and often owing to the distillation temperature height, active compound is destroyed by high temperature and decomposes, and extraction time is long, and (12～24h), energy consumption is big.The organic solvent extraction method inevitably produces organic solvent residue, brings certain difficulty for separation purification and application.
Supercritical carbon dioxide fluid (SC-CO
2), have critical temperature (TC) and emergent pressure (PC) low, nontoxic, colourless, do not fire, advantage such as inexpensive, unreactiveness.(Response Surface Method (RSM) sees reference document: SitiMachmudah, Yukari Kawahito, Mitsuru Sasaki, Motonobu Goto.Supercritical CO2extraction of rosehip seed oil:Fatty acids composition and process optimization.J.ofSupercritical Fluids.41:2007,421-428.) be the synthetic of Statistic Design experimental technique, it comprises experimental design, modeling, the testing model well-formedness, the assessment of factorial effect, 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
Technical problem the object of the present invention is to provide a kind of supercritical CO
2Extract the method for Chinese chive seed oil, solve and utilize the active substance destruction of prior art extraction Chinese chive seed oil existence many, the inferior shortcoming of Chinese chive seed oil.
Technical scheme: embodiment of the present invention are as follows:
1. the method for extracting Chinese chive seed oil by supercritical carbon dioxide comprises:
(1) raw material: leek seed, material cleaning, cleanliness 〉=99%;
(2) drying: with the seasoning of leek seed or in constant temperature oven≤50 ℃ drying 10～20h, water content is about 6.5% and gets final product;
(3) pulverize: with high speed disintegrator the leek seed is pulverized, sieve (20 order) is standby;
(4) supercritical CO
2Extract: the leek seed after the above-mentioned pulverizing is dropped into supercritical CO
2In the extraction plant, regulate 35～45 ℃ of extraction temperature, extracting pressure 15～25Mpa, the extraction time is 30～90min, CO
2Flow is fixed as 20L/h, and the extraction certain hour is directly collected Chinese chive seed oil in the extraction kettle outlet with triangular flask;
2. according to the extracting method of Chinese chive seed oil, utilize Design Expert (Static Made Easy, Minneapolis, MN, USA.version 7.1.1,2006) software carries out regression analysis to experimental data, the secondary multivariate regression model that draws: Y=16.1066+1.862x
1+ 0.318625x
2+ 2.444375x
3-0.03325x
1x
2-1.39375x
1x
3-0.1675x
2x
3-1.36105x
1 2-1.5893x
2 2-1.1383x
3 2(x
1: be encoded radio, the x of pressure independent variable(s)
2: be encoded radio, the x of temperature independent variable(s)
3: being the encoded radio of time independent variable(s)) this model can dope the extracting Chinese chive seed oil by supercritical carbon dioxide yield, and extract the technology of Chinese chive seed oil by this secondary multivariate regression model optimization.Its supercritical CO
2Optimum parameter is optimized for and extracts 40.40 ℃ of temperature in the leaching process, extracts pressure 22.25Mpa, and extraction time is 86.70min.
Beneficial effect: the present invention selects supercritical carbon dioxide extraction and Response Surface Method (RSM) Statistic Design for use, by Design Expert software testing data is carried out regression analysis, carry out extracting Chinese chive seed oil by supercritical carbon dioxide method and determination of main parameters and extracting method is optimized.Compare with traditional extraction technology, its advantage is:
(1) significant parameter that filters out by the present invention can be realized extracting Chinese chive seed oil and have and extract oil yield height (yield improves 5%), extraction efficiency height, extraction time short (than the organic solvent extraction 10-20h that saves time), and technology is simple, easy to operate.
(2) extracting Chinese chive seed oil by supercritical carbon dioxide have that energy consumption is low, product purity is high, extract Chinese chive seed oil no solvent residue and environmentally safe etc. advantage.Supercritical CO of the present invention
2The extraction Chinese chive seed oil has advantages such as noresidue, selectivity be strong, has good DEVELOPMENT PROSPECT.Utilize Chinese chive seed oil that technology of the present invention extracts for yellow, clarifying oily matter, have the special local flavor of Chinese chive seed oil; Purity is more than 99%; Yield is 17.23～17.42%.
(3) selected suitable extraction conditions promptly to extract 40.40 ℃ of temperature, extracted pressure 22.25Mpa, extraction time is 86.70min, and suitable material moisture content 6.5% and raw meal particle size 20 orders.By model to supercritical CO
2Extract the maximum yield of Chinese chive seed oil and predict that the extraction pressure range is: 18.70～24.30MPa; The extraction temperature range is: 38.35～42.30 ℃; Extraction time, scope was: 66.60～87.60min, regulate the extraction conditions supercritical CO in this parameter area
2Extracting Chinese chive seed oil extraction yield is 16.96～17.39%.Reconciling the extraction parameter is 40.40 ℃ extracting temperature, and extraction time is 86.70min, and under the condition of pressure 22.25MPa, the theoretical yield of Chinese chive seed oil maximum extracted is 17.42%, and the actual extracting yield is 17.37～17.52%, conforms to predictor.
(4) extracting Chinese chive seed oil by supercritical carbon dioxide method provided by the invention can be used for the extraction to Chinese chive seed oil in the production.
Four, description of drawings
Fig. 1 is that pressure and temperature are extracted the response surface 3D and the isogram of yield influence to Chinese chive seed oil,
Extraction time is fixed as 60min (x
3=0).
Fig. 2 is that time and temperature are extracted the response surface 3D and the isogram of yield influence to Chinese chive seed oil,
Extracting pressure fixing is 20MPa (x
1=0).
Fig. 3 extracts the response surface 3D and the isogram of yield influence to Chinese chive seed oil at pressure and time,
Extract temperature and be fixed as 40 ℃ of (x
2=0).
x
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 of time independent variable(s), x
i=(X
i-X
0)/Δ X encodes to independent variable(s), wherein, and 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).The strong and weak size of isocontour shape reflection interaction, oval expression two factor significant interaction.
Five, embodiment
(document sees reference: Box GEP.Multifactor designs of first order.Biometrika 1952 by Response Surface Method (RSM) Box-Behnken model in conjunction with pertinent literature in the present invention; 39:49-57. with Box GEP, Behnken DW.Some new three level design for the study of quantitative variables.Technometrics 1960; 2:455-75.) designed 35 ℃, 40 ℃, 45 ℃ three Temperature Treatment, 15MPa, 20MPa, three pressure treatment of 25Mpa, 30min, 60min, three CO of 90min
2The extraction time handles, and suitable water content 6.5% is that index screening goes out best extraction conditions with the yield.Data are carried out regression analysis by experiment, get secondary multivariate regression model: Y=16.1066+1.862x
1+ 0.318625x
2+ 2.444375x
3-0.03325x
1x
2-1.39375x
1x
3-0.1675x
2x
3-1.36105x
1 2-1.5893x
2 2-1.1383x
3 2, this model is carried out variance analysis (ANOVA): F
Return=50.9459〉F
0.01(9,4)=14.66, p＜0.0001 model (1) highly significant, coefficient (Adj R-Squared) Adj R is determined in the adjustment of model
2=0.9656, the model-fitting degree is good, and experimental error is little, can analyze the extracting Chinese chive seed oil by supercritical carbon dioxide yield and predicts with this model.Model is an x once
1, x
3(p＜0.0001), quadratic term x
1 2, x
2 2, x
3 2(p＜0.0001) is extremely remarkable; A mutual x
1x
3Significant difference.x
1Pressure, x
2Temperature, x
3Time and interaction thereof are to influence such as Fig. 1 of response value, shown in 2,3.The strong and weak size of isocontour shape reflection interaction, oval expression two factor significant interaction.For extracting 40.40 ℃ of temperature, extract pressure 22.25Mpa by the model optimization extracting parameter, extraction time is 86.70min, can extract the grease in the leek seed to greatest extent.
Embodiment 1:
Supercritical CO
2Extract " 791 snow fragrant-flowered garlic " Chinese chive seed oil:
(1) raw material: leek seed " 791 snow fragrant-flowered garlic " Nanjing starlight kind industry company limited, cleanliness 〉=99%;
(2) drying: with the seasoning of leek seed or in constant temperature oven≤50 ℃ drying 10～20h, water content is about 6.5% and gets final product;
(3) pulverize: with high speed disintegrator the leek seed is pulverized, sieve (20 order) is standby;
(4) supercritical CO
2Extract: the leek seed after the above-mentioned pulverizing is dropped into supercritical CO
2(HA121-50-01 type supercritical extraction unit, Huaan, Nantong supercritical extraction company limited produces) regulated and extracted 40.40 ℃ of temperature in the extraction plant, extracts pressure 22.25Mpa, and extraction time is 86.70min, CO
2Flow 20L/h, separating still separating pressure 4～8MPa, 30 ℃ of separation temperatures, extraction finishes directly to collect purified Chinese chive seed oil in the extraction kettle outlet with triangular flask.
The Chinese chive seed oil that is extracted has the special local flavor of Chinese chive seed oil for yellow, clarifying oily matter; Purity is more than 99%; Yield is 17.23～17.42%.
Model is to supercritical CO
2Extract the maximum yield of Chinese chive seed oil and predict that the extraction pressure range is: 18.70～24.30MPa; The extraction temperature range is: 38.35～42.30 ℃; Extraction time, scope was: 66.60～87.60min, regulate the extraction conditions supercritical CO in this parameter area
2Extracting Chinese chive seed oil extraction yield is 16.96～17.39%.Reconciling the extraction parameter is 40.40 ℃ extracting temperature, and extraction time is 86.70min, and under the condition of pressure 22.25MPa, the theoretical yield of Chinese chive seed oil maximum extracted is 17.42%, and the actual extracting yield is 17.37～17.52%, conforms to predictor.
Equipment and technology that pre-treatment of the present invention requires are fairly simple, select for use the leek seed of other kinds also to obtain same effect, by the supercritical CO of optimizing
2Extract the Chinese chive seed oil parameters, can effectively carry out supercritical CO
2The extraction of Chinese chive seed oil improves extraction efficiency greatly, can be used for the extraction to Chinese chive seed oil in the production, has good market outlook.
Claims (3)
1. the method for extracting Chinese chive seed oil by supercritical carbon dioxide comprises:
(1) raw material: leek seed;
(2) drying: dry below 60 ℃ with the seasoning of leek seed or at constant temperature oven, water content is about 6.5% and gets final product;
(3) pulverize: with high speed disintegrator the leek seed is pulverized, it is standby to cross 20 mesh sieves;
(4) supercritical CO
2Extract: the leek seed after the above-mentioned pulverizing is dropped into supercritical CO
2In the extraction plant, regulate 35～45 ℃ of extraction temperature, extracting pressure 15～25Mpa, the time is 30～90min, CO
2Flow 20L/h directly collects purified Chinese chive seed oil in the extraction kettle outlet with triangular flask.
2. according to the method for the described extracting Chinese chive seed oil by supercritical carbon dioxide of claim 1, its supercritical CO
2Parameter regulation is 40.40 ℃ of extraction temperature in the leaching process, extracting pressure 22.25Mpa, and extraction time is 86.70min.
3. the Chinese chive seed oil product that obtained of claim 1 or 2 described methods.
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|---|---|---|---|
| CNA2008101237682A CN101451089A (en) | 2008-06-04 | 2008-06-04 | Method for extracting Chinese chive seed oil by supercritical carbon dioxide |
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|---|---|---|---|
| CNA2008101237682A CN101451089A (en) | 2008-06-04 | 2008-06-04 | Method for extracting Chinese chive seed oil by supercritical carbon dioxide |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105154217A (en) * | 2015-09-24 | 2015-12-16 | 全椒县尹氏油脂有限公司 | Chinese chive seed oil extracting method |
| CN105343465A (en) * | 2015-11-16 | 2016-02-24 | 无锡瑞盈生命科学有限公司 | A compound tuber onion seed oil health-care spray and a preparing method |
| CN106280684A (en) * | 2016-08-17 | 2017-01-04 | 张静 | A kind of preparation method of environmental-friendly plant oil-based ink binder |
| CN107441306A (en) * | 2017-08-10 | 2017-12-08 | 平顶山市平丰种业有限责任公司 | A kind of extraction and its application of leek seed active component |
| 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 |
| CN108659950A (en) * | 2018-05-08 | 2018-10-16 | 广西大学 | A kind of preparation method of Chinese chive seed oil and polypeptide |
-
2008
- 2008-06-04 CN CNA2008101237682A patent/CN101451089A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105154217A (en) * | 2015-09-24 | 2015-12-16 | 全椒县尹氏油脂有限公司 | Chinese chive seed oil extracting method |
| CN105343465A (en) * | 2015-11-16 | 2016-02-24 | 无锡瑞盈生命科学有限公司 | A compound tuber onion seed oil health-care spray and a preparing method |
| CN106280684A (en) * | 2016-08-17 | 2017-01-04 | 张静 | A kind of preparation method of environmental-friendly plant oil-based ink binder |
| CN107441306A (en) * | 2017-08-10 | 2017-12-08 | 平顶山市平丰种业有限责任公司 | A kind of extraction and its application of leek seed active component |
| 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 |
| CN108659950A (en) * | 2018-05-08 | 2018-10-16 | 广西大学 | A kind of preparation method of Chinese chive seed oil and polypeptide |
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Open date: 20090610 |