CN101781604A - Method for extracting semen nigellae oil by using supercritical carbon dioxide - Google Patents
Method for extracting semen nigellae oil by using supercritical carbon dioxide Download PDFInfo
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- CN101781604A CN101781604A CN 201010121719 CN201010121719A CN101781604A CN 101781604 A CN101781604 A CN 101781604A CN 201010121719 CN201010121719 CN 201010121719 CN 201010121719 A CN201010121719 A CN 201010121719A CN 101781604 A CN101781604 A CN 101781604A
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Abstract
The invention relates to a method for extracting semen nigellae oil by using supercritical CO2, belonging to the field of food processing and specially used for comprehensive development and deep processing of semen nigellae. Taking semen nigellae (Semen Nigellae) as a raw material, the method comprises the following process steps: semen nigellae (Semen Nigellae) is dried and crushed and is extracted by supercritical CO2, and the optimal process parameters areas follows: the extraction pressure is 29.20 MPa, the extraction temperature is 40.15 DEG C and a CO2 flow is 21.92 L/h. The semen nigellae oil extracted under the conditions has the purity of above 99 percent and the maximum extraction yield of 37.897 percent. The process for extracting the semen nigellae oil by using the supercritical CO2 provides a new method for deep processing of the semen nigellae and can efficiently carry out research on extracting the semen nigellae oil by the supercritical CO2. The invention has the advantages of strong operability, favorable safety, higher yield, favorable repeatability, high extraction efficiency, simple process, high product purity, non pollution and the like and can be used for extracting the semen nigellae oil in production.
Description
One, technical field
The present invention relates to supercritical CO
2The method of extracting semen nigellae oil belongs to the food-processing field, is exclusively used in the extraction of Oleum Nigellae.
Two, background technology
Nigella damascena L. is that Ranunculaceae (Ranunculaceae) Nigella damascena L. belongs to (Nigella) plant, and general medicinal part is a seed.As medicinal three kinds that have, be respectively fruit Nigella damascena L. (Nigella sative Linn.) at present, have another name called tame Nigella damascena L.; Nigella glandulifera Freyn (Nigella glandulifera Preyn et Sint.) has another name called Semen Nigellae; And Nigella damascena L. (Nigelladamascena L.).Nigella glandulifera Freyn (Nigella glandulifera Preyn et Sint) is the annual herb plant, mainly is distributed in ground such as Turfan, Xinjiang, Hami, Shanshan, and also there are plantation in the Soviet Union, Iran, Afghanistan, Pakistan, Egypt etc.The nigella glandulifera Freyn herb all can be used as medicine, but is main medicinal materials with seed, and its seed almost completely is used for edible and medical aspect.Nigella glandulifera Freyn is repeatedly taken in the Pharmacopoeia of the People's Republic of China (contained Semen Nigellae Semen Nigellae by name) and " Chinese ethnic drug will " as the dimension medicinal material.Its nature and flavor are sweet, hot, warm.Effect is diuresis, tonifying the brain and kidney, invigorate blood circulation, detoxifcation, lactogenesis, stimulate the menstrual flow, cough-relieving, crow are sent out, anti-ageing.Be usually used in diseases such as shortness of breath uncomfortable in chest, edema, tinnitus, milk minimizing, hot pouring, urolithiasis, amenorrhoea, take for a long time and can make white hair change crow; Mix vinegar in addition and eat and to get rid of intestinal parasites by means of drugs, mix sweet eating and to control asthma.Contain the lipid acid to the human body beneficial such as oleic acid, linolic acid, palmitinic acid, eicosanoic acid in the Semen Nigellae, also contain Ranunculin, saponin(e, alkaloids isoreactivity composition in addition.
Cold press extraction method and organic solvent extraction method are adopted in the extraction of Oleum Nigellae at present.The cold press extraction method inevitably bring impurity into and extract insufficient, to extract yield lower.There is organic solvent residue in the organic solvent extraction method, brings certain difficulty for separation purification and application; In addition, the organic solvent extraction method is difficult to extract to some activeconstituents or is difficult to extract complete.
Supercritical CO
2Fluid, have critical temperature and emergent pressure low, nontoxic, colourless, do not fire, advantage such as inexpensive, unreactiveness, with traditional extraction technology relatively, it has, and extractability is strong, extraction efficiency is high, with short production cycle, technology is simple, easy to operate, energy consumption is low, the product loss is little and the product purity advantages of higher.(Response surface methodology, RSM) (Response Surface Method sees reference document: Siti Machmudah, Yukari Kawahito, Mitsuru Sasaki, Motonobu Goto.Supercritical CO
2Extraction of rosehip seed oil:Fattyacids 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
Technical problem the object of the present invention is to provide a kind of supercritical CO
2The method of extracting semen nigellae oil solves and utilizes the active substance destruction of prior art extraction Oleum Nigellae existence many, the inferior shortcoming of Oleum Nigellae.
Technical scheme: embodiment of the present invention are as follows:
1. supercritical CO
2The method of extracting semen nigellae oil comprises:
(1) raw material: Semen Nigellae, remove hybrid and various impurity, make raw material cleanliness 〉=99%;
(2) drying: dry down for 40 ℃ with the Semen Nigellae seasoning or at the electric heating constant temperature air dry oven, water content gets final product less than 6%;
(3) pulverize: with high speed disintegrator Semen Nigellae is pulverized, sieve (40 order) is standby;
(4) supercritical CO
2Extraction: the Semen Nigellae sample after the above-mentioned pulverizing is dropped into supercritical CO
2In the extraction plant, regulate extracting pressure 25～35Mpa, 35～45 ℃ of extraction temperature, CO
2Flow 18～22L/h, the extraction time is fixed as 100min, separates I pressure 7～8MPa, and 45 ℃ of temperature are separated II pressure 4～6MPa, 35 ℃ of temperature.Directly collect Oleum Nigellae with triangular flask in the separating still exit.
Utilize Design Expert (Static Made Easy, Minneapolis, MN, USA.version 7.1.1,2006) software the extracting method experimental data of Oleum Nigellae to be carried out regression analysis, the secondary multivariate regression model that draws: Y=36.81+0.78x
1-0.014x
2+ 1.27x
3+ 0.41x
1x
2-0.099x
1x
3+ 0.32x
2x
3-2.16x
1 2-1.64x
2 2+ 0.031x
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 CO
2Encoded radio (the x of flow 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 Oleum Nigellae yield.This model can dope supercritical CO
2The extracting semen nigellae oil yield, and pass through the technology that Oleum Nigellae is extracted in this secondary multivariate regression model optimization.Its supercritical CO
2Optimum parameter is optimized for 40.15 ℃ of extraction temperature, extracting pressure 29.20Mpa, CO in the extraction process
2Flow 21.92L/h.
Beneficial effect: the present invention selects supercritical CO for use
2Extraction and Response Surface Method (RSM) Statistic Design are carried out regression analysis by Design Expert software to testing data, carry out supercritical CO
2Extracting semen nigellae oil method and determination of main parameters also are optimized extracting method, set up supercritical CO
2The process modeling of extracting semen nigellae oil is for the industrial application of this technology provides call parameter.Compare with traditional extraction technology, its advantage is:
(1) significant parameter that filters out by the present invention can be realized extracting Oleum Nigellae and have and extract the oil yield height, the extraction efficiency height, extraction time is short, technology is simple, easy to operate.
(2) the present invention utilizes supercritical CO
2Abstraction technique extracts the Semen Nigellae vegetables oil and has advantages such as energy consumption is low, product purity is high, extract Oleum Nigellae no solvent residue and environmentally safe, has good DEVELOPMENT PROSPECT.The Oleum Nigellae that utilizes technology of the present invention to extract is the clarifying oily matter of light brown, has the special local flavor of Oleum Nigellae; Purity is more than 99%.
(3) optimum process condition that obtains of present method optimization is comparatively gentle, i.e. extracting pressure 29.20Mpa, 40.15 ℃ of extraction temperature, CO
2Flow 21.92L/h and suitable material moisture content 6% and raw meal particle size 40 orders.This processing condition easy handling, repeatability is strong, when realizing Oleum Nigellae maximum extraction yield, has also guaranteed the stable of activeconstituents in the product.
(4) Oleum Nigellae supercritical CO provided by the invention
2Extracting process, the industry that can directly apply to Semen Nigellae is extracted, and is its further development and use in fields such as food chemical industry condition that facilitates.
Four, description of drawings
Fig. 1 is that pressure and temperature are extracted the response surface 3D and the isogram of yield influence to Oleum Nigellae,
CO
2Flow is fixed as C:20L/h (x
3=0), A: pressure, B: temperature.
Fig. 2 is pressure and CO
2Flow extracts the response surface 3D and the isogram of yield influence to Oleum Nigellae,
Extract temperature and be fixed as B:40 ℃ of (x
2=0), A: pressure, C:CO
2Flow.
Fig. 3 is temperature and CO
2Flow extracts the response surface 3D and the isogram of yield influence to Oleum Nigellae,
Extracting pressure fixing is A:30MPa (x
1=0), B: temperature, C:CO
2Flow.
Oleum Nigellae yield=(extracting semen nigellae oil weight/adding sample size) * 100%.
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; 25MPa, 30MPa, three pressure treatment of 35Mpa; 18L/h, 20L/h, three CO of 22L/h
2Flow is handled, and 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=36.81+0.78x
1-0.014x
2+ 1.27x
3+ 0.41x
1x
2-0.099x
1x
3+ 0.32x
2x
3-2.16x
1 2-1.64x
2 2+ 0.031x
3 2, this model is carried out variance analysis (ANOVA), the result shows that this model has utmost point significance (P＜0.001), coefficient (Adj R-Squared) AdjR is determined in the adjustment of model
2=0.9781, illustrate that this model can explain the variation of 97.81% response value.Therefore, this model-fitting degree is good, and experimental error is little, can be with this model to supercritical CO
2The extracting semen nigellae oil yield is analyzed and is predicted.Model is carried out the test of significance of regression equation coefficient, obtain an once x of model
1, x
3(p＜0.0001), quadratic term x
1 2, x
2 2(p＜0.0001) is extremely remarkable; A mutual x
1x
2, x
2x
3Significant difference.x
1Pressure, x
2Temperature, x
3CO
2Flow 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.By regression model optimization, obtaining best extraction process parameter is 40.15 ℃ of extraction temperature, extracting pressure 29.20Mpa, CO
2Flow 21.92L/h, the maximum yield of prediction Oleum Nigellae is 37.897%, experiment actual value and predictor are coincide.
Embodiment:
Supercritical CO
2Extraction " nigella glandulifera Freyn " Oleum Nigellae method is as follows:
(1) raw material: sophisticated nigella glandulifera Freyn seed, cleanliness 〉=99%;
(2) drying: dry down for 40 ℃ with the Semen Nigellae seasoning or at the electric heating constant temperature air dry oven, water content is about 6% and gets final product;
(3) pulverize: with high speed disintegrator Semen Nigellae is pulverized, sieve (40 order) is standby;
(4) supercritical CO
2Extraction: the Semen Nigellae sample after the above-mentioned pulverizing is dropped into supercritical CO
2In the extraction kettle of extraction plant (HA121-50-01 type supercritical extraction unit, Huaan, Nantong supercritical extraction company limited produces), regulate 40.15 ℃ of extraction temperature, extracting pressure 29.20Mpa, CO
2Flow 21.92L/h, the extraction time is 100min, separates I pressure 7～8MPa, 45 ℃ of temperature are separated II pressure 4～6MPa, 35 ℃ of temperature.Extraction finishes directly to collect purified Oleum Nigellae in the separating still exit with triangular flask.The Oleum Nigellae that is extracted is light brown, clarifying oily matter, has the special local flavor of Oleum Nigellae, and purity is more than 99%; Maximum extraction yield predictor is 37.897%, and measured value is 37.67%～37.93%, conforms to predictor.
The supercritical CO that obtains by this model
2The extracting semen nigellae oil parameters can effectively be carried out supercritical CO
2The extraction of extracting semen nigellae oil improves extraction efficiency greatly, can be used for the extraction to Oleum Nigellae in the production.Equipment and technology that pre-treatment of the present invention requires are also fairly simple, select for use the Nigella damascena L. seed of other kinds also can obtain same effect.The Oleum Nigellae of this technology extraction gained all is better than the Oleum Nigellae of cold press extraction and organic solvent extraction gained on organoleptic quality and purity, have good market outlook.
Claims (3)
1. supercritical CO
2The method of extracting semen nigellae oil comprises:
(1) raw material: Semen Nigellae, cleanliness 〉=99%;
(2) drying: dry down for 40 ℃ with the Semen Nigellae seasoning or at the electric heating constant temperature air dry oven, water content is less than 6%;
(3) pulverize: with high speed disintegrator Semen Nigellae is pulverized, it is standby to cross 40 mesh sieves;
(4) supercritical CO
2Extraction: the Semen Nigellae sample after the above-mentioned pulverizing is dropped into supercritical CO
2In the extraction plant, regulate 35～45 ℃ of extraction temperature, extracting pressure 25～35Mpa, CO
2Flow 18～22L/h, extraction time 100min separates I pressure 7～8MPa, and 45 ℃ of temperature are separated II pressure 4～6MPa, 35 ℃ of temperature; Directly collect purified Oleum Nigellae with triangular flask in the separating still exit.
2. according to the described supercritical CO of claim 1
2The method of extracting semen nigellae oil, its supercritical CO
2Parameter regulation is 40.15 ℃ of extraction temperature in the extraction process, extracting pressure 29.20Mpa, CO
2Flow 21.92L/h.
3. the product that method obtained of claim 1 or 2 described extracting semen nigellae oil by using supercritical carbon dioxide.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103961282A (en) * | 2014-05-14 | 2014-08-06 | 江南大学 | Method for extracting antioxidant ingredient from nigella plant seeds based on cloud point extraction and application of antioxidant ingredient |
| CN111542313A (en) * | 2017-12-27 | 2020-08-14 | 萨米莱布斯有限公司 | Compositions containing thymoquinol and methods of making same |
| CN111763560A (en) * | 2019-04-02 | 2020-10-13 | 深圳市金枫生物医药科技有限公司 | Acer truncatum oil extraction method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1237618A (en) * | 1999-05-13 | 1999-12-08 | 潘泰安 | Fruit seed oil obtained by supercritical CO2 extraction and its product |
| 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 201010121719 patent/CN101781604A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1237618A (en) * | 1999-05-13 | 1999-12-08 | 潘泰安 | Fruit seed oil obtained by supercritical CO2 extraction and its product |
| CN101560438A (en) * | 2009-05-13 | 2009-10-21 | 南京农业大学 | Supercritical carbon dioxide extraction method of fistular onion seed oil |
Non-Patent Citations (2)
| Title |
|---|
| 《农产品加工（创新版）》 20090430 张谦等 新疆黑种草籽实与油脂品质特性及其SFE萃取工艺的初步研究 第39页 1-3 , 第4期 2 * |
| 《粮油加工与食品机械》 20051030 刘彩丽等 超临界CO2 流体萃取技术提取特种油脂的研究进展 47-50 1-3 , 第10期 2 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103961282A (en) * | 2014-05-14 | 2014-08-06 | 江南大学 | Method for extracting antioxidant ingredient from nigella plant seeds based on cloud point extraction and application of antioxidant ingredient |
| CN103961282B (en) * | 2014-05-14 | 2016-09-14 | 江南大学 | A kind of method and application extracting antioxidant content in Nigella damascena L. platymiscium seed based on cloud point extraction method |
| CN111542313A (en) * | 2017-12-27 | 2020-08-14 | 萨米莱布斯有限公司 | Compositions containing thymoquinol and methods of making same |
| CN111542313B (en) * | 2017-12-27 | 2023-11-21 | 萨米莱布斯有限公司 | Composition containing baili hydroquinone and preparation method thereof |
| CN111763560A (en) * | 2019-04-02 | 2020-10-13 | 深圳市金枫生物医药科技有限公司 | Acer truncatum oil extraction method |
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Application publication date: 20100721 |