CN100343218C - Method for extracting omega 6 polyunsaturated fatty acid from plant seeds - Google Patents
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- CN100343218C CN100343218C CNB200510017294XA CN200510017294A CN100343218C CN 100343218 C CN100343218 C CN 100343218C CN B200510017294X A CNB200510017294X A CN B200510017294XA CN 200510017294 A CN200510017294 A CN 200510017294A CN 100343218 C CN100343218 C CN 100343218C
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Abstract
The present invention relates to a method for extracting omega-6 polyunsaturated fatty acids from vegetable seeds, which belongs to a method for extracting omega-6 polyunsaturated fatty acids. Impurities are removed from the vegetable seeds, and the vegetable seeds are properly pretreated, coarsely crushed, fast dried in the mode of microwave oscillation of broken walls and fine pulverized to be made into powder with certain granularity; the obtained powder is extracted in supercritical CO2 fluid, proper extraction conditions are adopted for selective extraction, separation and purification of the omega-6 polyunsaturated fatty acids in raw materials. The present invention has the advantages of sufficient utilization of the raw materials in the manufacture process, no generation of waste slag and waste steam, no environmental pollution, high physiological activity of products and excellent mouth feelings.
Description
Technical field
The invention belongs to the extracting method of omega 6 polyunsaturated fatty acid, refer in particular to from plant seed and extract.
Background technology
In the molecule of cis polyunsaturated fatty acid, apart from carboxyl two keys farthest are the omega 6 polyunsaturated fatty acids that are called on the 6th carbon atom reciprocal, linolic acid wherein, gamma-linolenic acid, arachidonic acid be not because of synthesizing voluntarily and must absorb from food in the body, be called as indispensable fatty acid, especially linolic acid is that human body can not lack, in human body, can not transform acquisition, and gamma-linolenic acid and arachidonic acid can transform acquisition by linolic acid in human body by other lipid acid.The human body cell film is being controlled electron transport, regulate nutritive substance and enter in the cell and the discharge of refuse in the cell, and the effect that lipid acid cell membrane phosphatide is brought into play has decisive influence.Keep the mobile relatively of film, lipid acid must have suitable nonsaturation, otherwise the cells physiological function will be lost.Discover that the unsaturated fatty acids of not all kind all has significant nourishing function, have only above-mentioned indispensable fatty acid just to have stronger physiological function.Studies show that the cytolemma that lacks indispensable fatty acid presents a kind of the expansion and becomes big ill shape.When lacking linolic acid and gamma-linolenic acid, cholesterol will be gathered in arterial blood by more saturated fatty acid esterification, and the extent of metabolism of cholesterol is reduced, and causes atherosclerosis.Linolic acid and gamma-linolenic acid can make cholesteryl esterization, thereby reduce the cholesterol levels of interior serum of body and liver.Linolic acid also has the formation that reduces blood cholesterol levels, prevent blood plate thrombus, suppress effect such as artery thrombosis, in addition diabetes also had certain prophylactic effect.
Contain a large amount of Vegetable oil lipoprotein in the plant seed, milling process or organic solvent method are adopted in the greasy extraction of traditional plant seed more, the products obtained therefrom complicated component, process for refining is loaded down with trivial details, and organic solvent residual also brings chemical pollution to product, therefore can only there be special nourishing function as common oil for cooking or industrial chemicals.Especially be rich in the grease of polyunsaturated fatty acid,, extract in addition that serious sex change and chemical pollution take place the remaining grouts in fat back and recycle value is extremely low even do not have recycle value because easy oxidative rancidity reduces the grease package stability greatly.
Pertinent data is looked into new result and is shown, be that raw material extracts grease at present both at home and abroad with the plant seed, the mixtures that adopt milling process or organic solvent method to extract glycerol fatty acid ester and lipid acid more, carry out fractionation then and obtain lipid acid, omega 6 polyunsaturated fatty acid purity is low in the products obtained therefrom, has organic solvent residual, can not reach the health-care effect of expection, and yield is lower, and also there is environmental issue in complex operation.
Summary of the invention
The invention provides the extracting method of omega 6 polyunsaturated fatty acid in a kind of plant seed, big and defective such as environmental problem arranged to solve the operational danger that omega 6 polyunsaturated fatty acid purity is low and degree of oxidation is high and organic solvent method exists that traditional milling process exists.The technical scheme that the present invention takes is:
Comprise the steps:
A. the pre-treatment of plant seed, select edible plant seed, remove oil-containing is low in the seed part or unedible part, keep part edible, that contain innage, adopt then clean, washing and processed, removal is mixed in impurity wherein, carries out coarse reduction again, and making its granularity is 1mm～5mm;
B. microwave broken wall, drying, pulverizing stops 1min～5min behind microwave oscillation 1min～5min, detects material moisture, so carry out microwave oscillation, the embrittlement of material cell walls is broken, remove most of moisture simultaneously, detect material moisture 6%～8%, stop microwave oscillation; With the further smart pulverizing of the feed particulate material of dehydration broken wall, making its granularity is 0.5mm～2mm;
C. supercritical CO
2Abstraction purification obtains raw material to above-mentioned steps and carries out the selective extraction separation, extracting pressure 15MPa～45MPa, 35 ℃～55 ℃ of extraction temperature, extraction time 1h～3h, CO
2Flow 15L/h～40L/h.
The used plant seed of the present invention comprises all grass seeds, seeds of leguminous plant and trees seed.
Indication raw material of the present invention comprises plant seed, kind of benevolence or embryo shell.
The present invention is raw material with the plant seed, adopts repeatedly microwave concussion broken wall rapid dry process of intermittent type, when removing part moisture, makes the cell walls embrittlement and breaks, and improves the solubility rate of thing in the born of the same parents, utilizes supercritical CO then
2Fluid extraction technology is realized extracting purifying one and is gone on foot the omega 6 polyunsaturated fatty acid that the advanced technologies of finishing obtains higher degree.The present invention does not use acid, alkali and organic solvent aborning, does not have operational danger and environmental issue and can make production serialization, automatization, compares with traditional method, can enhance productivity more than 2 times.Product of the present invention shows to have tangible reducing blood-fat, reducing cholesterol, prevent thrombotic function through the function test result, have high economic benefit and good social benefit.
The intermittent type that the present invention adopts repeatedly microwave shakes broken wall rapid dry process vibration, penetration owing to microwave when removing moisture, polar molecule in the material rotates, vibrates and rubs, make the cell walls embrittlement and break, microwave heating effect produces the excessive diffusing of a large amount of steam and also makes cell walls tendering of fiber and fracture in addition, thereby has improved the mass transfer diffusion and the stripping capacity of intracellular organic matter; Supercritical CO
2Fluid extraction technology has easy to operate, and selectivity is good, the degreasing rate height, and have advantages such as efficient, low consumption, nontoxic, pollution-free, noresidue.Supercritical CO
2Fluid extraction technology optionally extracts certain composition of raw material, integrates extraction, separation, purifying, has simplified the extraction and purification process of object.Studies show that intermittent type repeatedly microwave concussion broken wall rapid drying and supercritical CO
2The fluid extraction operation all can keep the biologically active substance in the raw material to greatest extent, handles back extract and residuum and does not all have the generation of sex change phenomenon, and the comprehensive Utilization Ways of raw material is extensive, has improved utilization ratio of raw materials.
Advantage of the present invention is the raw material availability height, and no waste residue produces in the production process, does not use acid, alkali or organic solvent, and environment is not caused any pollution, product physiologically active height, and mouthfeel is good.
The yield of omega 6 polyunsaturated fatty acid of the present invention can reach more than 96%, and extract composition purity is higher, and omega 6 polyunsaturated fatty acid content reaches more than 95%.Extract and extract remainder all do not have chemical pollution in addition, and extract remainder can be used as the raw materials for production of edible cooking with oil or other extracts active ingredients and product.
The omega 6 polyunsaturated fatty acid that the present invention produced can further be made emulsion, powdery oil or microcapsule-type protective foods raw materials for production, and it is directly edible also can be processed into soft capsule type product.
Embodiment
The extracting and purifying method of grass corn omega 6 polyunsaturated fatty acid.
Corn is one of China staple crops, the a large amount of by product maize of the annual output of corn processed enterprises such as W-Gum factory or corn distillery, most organic solvent extraction Semen Maydis oils of directly using, because it contains a large amount of unsaturated fatty acidss, the not anti-storage of Semen Maydis oil, easy oxidative rancidity, the complete sex change of gained corn chop protein, recycle value is extremely low, even does not have recycle value, so raw material is underutilized, added value is very low, cause major product cost height, the market competitiveness is poor, and economic benefit is low.If maize high added value comprehensive utilization can be improved the corn processed economic benefit of enterprises greatly, also be simultaneously to obtain one of the corn omega 6 polyunsaturated fatty acid effective way.Maize accounts for 7%～14% of corn kernel, and maize lipid content 36%～47% wherein is unsaturated fatty acids more than 80%, and omega 6 polyunsaturated fatty acid accounts for about 25% of unsaturated fatty acids.Adopt the technology of the present invention, unsettled omega 6 polyunsaturated fatty acid in the maize fat can be extracted major part.Omega 6 polyunsaturated fatty acid is made protective foods, can realize the high value added utilization of corn, and its package stability of remaining maize fat strengthens greatly, and then can increase substantially the greasy commercial value of corn.
Raw material: remove oil-containing is low in the corn seed part or unedible part, keep part edible, that contain innage, concrete grammar is that the broken lobe of corn kernel decortication is obtained maize; Maize also can be from W-Gum factory, corn distillery or grain processing plant, and corn can be any kind of planting in the world.
Laboratory apparatus:
Supercritical CO
2The fluid extraction device: Huaan, Nantong supercritical extraction company limited produces the HA221-50-06 type.
The microwave oscillation drying installation: Sanle Microwave Technology Development Co., Ltd, Nanjing produces the WZ25-2 type.
Whizzer: sky, PVG this centrifugal machine company limited produces the SS300 type.
Pulverizer: Hua Tong machine works in Zhengzhou produces 300 types.
Moisture detector: Switzerland Mettler Toledo Inc. produces the HG53 type.
Embodiment 1
A. pre-treatment, the pre-treatment when being raw material with the by product maize of W-Gum factory or corn distillery.
Soak, wash: derive from the maize of W-Gum factory or corn distillery, stronger irritating smell is arranged, color is dark yellow, can not directly use.The tap water immersion 1h～2h of maize with 20 ℃ with flowing water rinsing gently, should be removed compositions such as remaining starch, small-particle endosperm and fiber then.Gained wet corn embryo is to carry out centrifugal dewatering under the condition of 2800r/min. at rotating speed, makes its water content 25～30%, carries out coarse reduction then, and making its granularity is 1mm～5mm.
B. microwave broken wall, drying, pulverizing
To stop 1min behind the maize microwave oscillation 2min after the pre-treatment, detect the maize water content, if water content is higher than 8%, then so carry out microwave oscillation 1 time again, detect the water content of this maize again, when recording its water content less than 8% the time, stop this microwave oscillation and drying, maize after this oven dry is carried out smart pulverization process, and making its granularity is 0.5mm～2mm, places shady and cool dry place to store standby.
C. supercritical CO
2Fluid extraction extracts purifying
Extracting pressure is 20Mpa, 50 ℃ of temperature, time 120min, CO
2Flow 35L/h.Gained extract corn omega 6 polyunsaturated fatty acid content is greater than 95%, and is faint yellow, is as good as assorted flavor.
Embodiment 2
A. pre-treatment, the by product maize that breaks lobe gained maize or grain processing plant with the corn kernel decortication is the pre-treatment of raw material.
Clean, this kind raw material maize contains more impurity, starch, crack rice etc., so will sieve, removes sandstone, metal, cracks rice and small-particle impurity, and the method with selection by winnowing obtains maize again.
Soaking and water washing is put into maize 18 ℃ tap water immersion and is stirred soak time 30min～40min.Impurity such as starch attached to it, dust are removed in rinsing gently under flowing water, carry out centrifugal dewatering then under rotating speed is the condition of 2800r/min, make its water content 25～30%, carry out coarse reduction, and making its granularity is 1mm～5mm.
B. microwave broken wall, drying, pulverizing
To stop 3min behind the maize microwave oscillation 3min after the pre-treatment, detect the maize water content, if water content is higher than 7%, then so carry out microwave oscillation 1 time again, detect the water content of this maize again, when recording its water content less than 7% the time, stop this microwave oscillation and drying, maize after this oven dry is carried out smart pulverization process, and making its granularity is 0.5mm～2mm, places shady and cool dry place to store standby.
C. supercritical CO
2Fluid extraction extracts purifying
Extracting pressure is 28Mpa, 42 ℃ of temperature, time 100min, CO
2Flow 33L/h.Gained extract corn omega 6 polyunsaturated fatty acid content is greater than 95%, and is faint yellow, is as good as assorted flavor.
Embodiment 3
A. pre-treatment
Pre-treatment when (1) being raw material with the by product maize of W-Gum factory or corn distillery
Soak, wash: the tap water immersion 1h～2h of maize with 22 ℃ with flowing water rinsing gently, should be removed compositions such as remaining starch, small-particle endosperm and fiber then.Gained wet corn embryo is to carry out centrifugal dewatering under the condition of 2800r/min. at rotating speed, makes its water content 25～30%, carries out coarse reduction then, and making its granularity is 1mm～5mm.
B. microwave broken wall, drying, pulverizing
To stop 5min behind the maize microwave oscillation 4min after the pre-treatment, detect the maize water content, if water content is higher than 6%, then so carry out microwave oscillation 1 time again, detect the water content of this maize again, when recording its water content less than 6% the time, stop this microwave oscillation and drying, maize after this oven dry is carried out smart pulverization process, and making its granularity is 0.5mm～2mm, places shady and cool dry place to store standby.
C. supercritical CO
2Fluid extraction extracts purifying
Extracting pressure is 35Mpa, 35 ℃ of temperature, time 80min, CO
2Flow 30L/h.Gained extract corn omega 6 polyunsaturated fatty acid content is greater than 95%, and is faint yellow, is as good as assorted flavor.
The extracting and purifying method of sesame omega 6 polyunsaturated fatty acid
Raw material, sesame can be any kind of planting in the world, because of most of for containing grease, so directly adopt its seed in its seed.
Laboratory apparatus is the same.
Embodiment 4
A. pre-treatment
Washing is removed tramp materiaies such as its grass-seed that is mixed with, silt with sesame with the flowing water rinsing, carry out centrifugal dewatering then under rotating speed is the condition of 2800r/min, makes its water content 25%～30%, carries out coarse reduction, and making its granularity is 1mm～2mm.
B. microwave broken wall, drying, pulverizing.
To stop 1min behind the sesame microwave oscillation 1min after the pre-treatment, detect the sesame water content, if water content is higher than 8%, then so carry out microwave oscillation 1 time again, detect the water content of this sesame again, when recording its water content less than 8% the time, stop this microwave oscillation and drying, sesame after this oven dry is carried out smart pulverization process, and making its granularity is 0.5mm～1mm, places shady and cool dry place to store standby.
C. supercritical CO
2Fluid extraction extracts purifying
Extracting pressure is 15MPa, 45 ℃ of temperature, time, 140min, CO
2Flow 40L/h.Gained extract sesame omega 6 polyunsaturated fatty acid content is greater than 95%, and is faint yellow, is as good as assorted flavor.
Embodiment 5
A. pre-treatment
Washing is removed tramp materiaies such as its grass-seed that is mixed with, silt with sesame with the flowing water rinsing, carry out centrifugal dewatering then under rotating speed is the condition of 2800r/min, makes its water content 25%～30%, carries out coarse reduction, and making its granularity is 1mm～2mm.
B. microwave broken wall, drying, pulverizing
To stop 2min behind the sesame microwave oscillation 2min after the centrifuge dehydration, detect the sesame water content, if water content is higher than 7%, then so carry out microwave oscillation 1 time again, detect the water content of this sesame again, when recording its water content less than 7% the time, stop this microwave oscillation and drying, sesame after this oven dry is carried out smart pulverization process, and making its granularity is 0.5mm～1mm, places shady and cool dry place to store standby.
3. supercritical CO
2Fluid extraction extracts purifying
Extracting pressure is 25MPa, 40 ℃ of temperature, time 110min, CO
2Flow 30L/h.Gained extract sesame omega 6 polyunsaturated fatty acid content is greater than 95%, and is faint yellow, is as good as assorted flavor.
Embodiment 6
A. pre-treatment
Washing is removed tramp materiaies such as its grass-seed that is mixed with, silt with sesame with the flowing water rinsing, carry out centrifugal dewatering then under rotating speed is the condition of 2800r/min, makes its water content 25%～30%, carries out coarse reduction, and making its granularity is 1mm～2mm.
B. microwave broken wall, drying, pulverizing.
To stop 2min behind the sesame microwave oscillation 3min after the pre-treatment, detect the sesame water content, if water content is higher than 6%, then so carry out microwave oscillation 1 time again, detect the water content of this sesame again, when recording its water content less than 6% the time, stop this microwave oscillation and drying, sesame after this oven dry is carried out smart pulverization process, and making its granularity is 0.5mm～1mm, places shady and cool dry place to store standby.
3. supercritical CO
2Fluid extraction extracts purifying
Extracting pressure is 40MPa, 35 ℃ of temperature, time 80min, CO
2Flow 25L/h.Gained extract sesame omega 6 polyunsaturated fatty acid content is greater than 95%, and is faint yellow, is as good as assorted flavor.
The extracting and purifying method of walnut omega 6 polyunsaturated fatty acid
Raw material, walnut can be any kind of planting in the world.
Laboratory apparatus is the same.
Embodiment 7
A. pre-treatment
Clean walnut is removed tramp materiaies such as its leaf that is mixed with, dust, silt with the flowing water rinsing, under rotating speed is the condition of 2800r/min., carry out centrifugal dewatering then, air-dry under the clean state.
Shelling shells walnut gets walnut kernel, and it is that the particle of 3mm～5mm is standby that the walnut kernel coarse breaking is become granularity.
B. microwave broken wall, drying, pulverizing
Stop 2min behind the walnut kernel microwave oscillation 2min with above processing, detect the walnut kernel water content, if water content is higher than 8%, then so carry out microwave oscillation 1 time again, detect the water content of this walnut kernel again, when recording its water content less than 8% the time, stop this microwave oscillation and drying, walnut kernel after this oven dry is carried out smart pulverization process, and making its granularity is 0.5mm～2mm, places shady and cool dry place to store standby.
3. supercritical CO
2Fluid extraction extracts purifying
Extracting pressure is 20MPa, 55 ℃ of temperature, time 180min, CO
2Flow 30L/h.Gained extract walnut omega 6 polyunsaturated fatty acid content is greater than 95%, and is faint yellow, is as good as assorted flavor.
Embodiment 8
A. pre-treatment
Clean walnut is removed tramp materiaies such as its leaf that is mixed with, dust, silt with the flowing water rinsing, under rotating speed is the condition of 2800r/min., carry out centrifugal dewatering then, air-dry under the clean state.
Shelling shells walnut gets walnut kernel, and it is that the particle of 3mm～5mm is standby that the walnut kernel coarse breaking is become granularity.
B. microwave broken wall, drying, pulverizing
Stop 3min behind the walnut kernel microwave oscillation 4min with above processing, detect the walnut kernel water content, if water content is higher than 7%, then so carry out microwave oscillation 1 time again, detect the water content of this walnut kernel again, when recording its water content less than 7% the time, stop this microwave oscillation and drying, walnut kernel after this oven dry is carried out smart pulverization process, and making its granularity is 0.5mm～2mm, places shady and cool dry place to store standby.
C. supercritical CO
2Fluid extraction extracts purifying
Extracting pressure is 33MPa, 47 ℃ of temperature, time 130min, CO
2Flow 25L/h.Gained extract walnut omega 6 polyunsaturated fatty acid content is greater than 95%, and is faint yellow, is as good as assorted flavor.
Embodiment 9
A. pre-treatment
Clean walnut is removed tramp materiaies such as its leaf that is mixed with, dust, silt with the flowing water rinsing, under rotating speed is the condition of 2800r/min., carry out centrifugal dewatering then, air-dry under the clean state.
Shelling shells walnut gets walnut kernel, and it is that the particle of 3mm～5mm is standby that the walnut kernel coarse breaking is become granularity.
B. microwave broken wall, drying, pulverizing
Stop 5min behind the walnut kernel microwave oscillation 5min with above processing, detect the walnut kernel water content, if water content is higher than 6%, then so carry out microwave oscillation 1 time again, detect the water content of this walnut kernel again, when recording its water content less than 6% the time, stop this microwave oscillation and drying, walnut kernel after this oven dry is carried out smart pulverization process, and making its granularity is 0.5mm～2mm, places shady and cool dry place to store standby.
C. supercritical CO
2Fluid extraction extracts purifying
Extracting pressure is 45MPa, 35 ℃ of temperature, time 80min, CO
2Flow 20L/h.Gained extract walnut omega 6 polyunsaturated fatty acid content is greater than 95%, and is faint yellow, is as good as assorted flavor.
Claims (2)
1, the extracting method of omega 6 polyunsaturated fatty acid in a kind of plant seed comprises the steps:
A. the pre-treatment of plant seed, select edible plant seed, remove oil-containing is low in the seed part or unedible part, keep part edible, that contain innage, adopt then clean, washing and processed, removal is mixed in impurity wherein, carries out coarse reduction again, and making its granularity is 1mm～5mm;
B. microwave broken wall, drying, pulverizing stops 1min～5min behind microwave oscillation 1min～5min, detects material moisture, so carry out microwave oscillation, the embrittlement of material cell walls is broken, remove most of moisture simultaneously, detect material moisture 6%～8%, stop microwave oscillation; With the further smart pulverizing of the feed particulate material of dehydration broken wall, making its granularity is 0.5mm～2mm;
C. supercritical CO
2Abstraction purification obtains raw material to above-mentioned steps and carries out selective extraction and separate, during extracting pressure 35MPa～45MPa, and 35 ℃ of extraction temperature, extraction time 80min, CO
2Flow 20L/h～30L/h.
2, the extracting method of omega 6 polyunsaturated fatty acid in the plant seed according to claim 1 is characterized in that: the seed of selecting corn or sesame or walnut.
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Cited By (1)
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| CN103122273A (en) * | 2013-01-14 | 2013-05-29 | 河南科技大学 | Method for extracting oat oil through microwave pretreatment |
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| CN102993145B (en) * | 2011-09-19 | 2015-06-03 | 北大方正集团有限公司 | Lovastatin extraction and purification method |
| CN103755547B (en) * | 2014-01-22 | 2015-05-27 | 中国科学院地质与地球物理研究所兰州油气资源研究中心 | Novel method for extracting fatty acid in natural products by utilizing column chromatography on silica gel |
| CN109280576A (en) * | 2018-09-29 | 2019-01-29 | 普宁康特生物科技有限公司 | The preparation method of 3 unsaturated fatty acid of Ω is extracted from Tilapia mossambica mesh |
| CN113604278A (en) * | 2021-07-15 | 2021-11-05 | 广州大学 | Method for extracting unsaturated fatty acid from lobster liver |
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Non-Patent Citations (2)
| Title |
|---|
| 芝麻ω-6多不饱和脂肪酸提取技术及其应用的研究 马福敏，吉林农业大学硕士学位论文 2005 * |
| 超临界萃取技术提取石蒜中加兰他敏的工艺研究 肖观秀，天津大学硕士学位论文 2005 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103122273A (en) * | 2013-01-14 | 2013-05-29 | 河南科技大学 | Method for extracting oat oil through microwave pretreatment |
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Free format text: CORRECT: ADDRESS; FROM: 130118 CHANGCHUN, JILIN PROVINCE TO: 130031 CHANGCHUN, JILIN PROVINCE |
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Effective date of registration: 20150106 Address after: 130031, 11, liberty stone road, No. 4755, liberty Road, Jilin, Changchun Patentee after: Jilin governor Ji Ji development and construction of Modern Agricultural Investment Co., Ltd. Address before: 130118 Changchun City, Jilin Metro Street, No. 2888 Patentee before: Jilin Agricultural University |