CN101353612B - Method for enriching polyunsaturated fatty acid from pine caterpillar - Google Patents
Method for enriching polyunsaturated fatty acid from pine caterpillar Download PDFInfo
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- CN101353612B CN101353612B CN2008100321312A CN200810032131A CN101353612B CN 101353612 B CN101353612 B CN 101353612B CN 2008100321312 A CN2008100321312 A CN 2008100321312A CN 200810032131 A CN200810032131 A CN 200810032131A CN 101353612 B CN101353612 B CN 101353612B
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- polyunsaturated fatty
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Abstract
The invention discloses a method for concentrating polyunsaturated fatty acid from the pine moth, which comprises the following steps: a urea adduct method is adopted to separate a fatty acid mixture according to the unsaturated degree difference of the fatty acid, the polyunsaturated fatty acid such as Alpha-linolenic acid, etc. is concentrated from the pine moth to obtain the polyunsaturated fatty acid product with higher purity, and the content of the polyunsaturated fatty acid reaches 80 to 90 percent. The method of the invention has wide raw material sources, low cost and high production efficiency, thus being a simple and practical technology.
Description
Technical field
The invention belongs to functional grease extractive technique field, be specifically related to a kind of from pine moth the method for enriching polyunsaturated fatty acid.
Background technology
The exploitation of functional grease at present,--polyunsaturated fatty acid is an integral part of functional foodstuff exploitation.All the time, people to the research of polyunsaturated fatty acid composition mostly based on marine fishes, seldom to the research of insect polyunsaturated fatty acid.
Pine moth (Dendrolimus spp.) is the most serious injurious forest-insect of China, can be rated as the hill fire of not smoldering.Since the seventies in 20th century, area takes place and is about annual 150～2,000,000 hm in China pine moth
2, its direct economic loss that causes is above 1,000,000,000 yuan.In addition, also can bring ecology and the environmental loss that uses agricultural chemicals to cause because of a large amount of.Since the seventies in last century, area takes place and is about annual 150-200 ten thousand hm2 in China pine moth, open-air stock number is very huge, it is reported, Zhejiang Province only, annual can receive 1,400,000 kg pine moths approximately, when Hubei Province Hong'an County pine moth was taken place in a large number in 1972, by government department mobilize the masses adopt altogether pine caterpillar 180,000 kg.
Yet the past people do not know to contain in the pine moth polyunsaturated fatty acid of more rich high value.We discover, contain more rich polyunsaturated fatty acid alpha-linolenic acid and α-linolic acid in the grease of pine moth, and wherein the content of alpha-linolenic acid is especially up to 25.2%.
Alpha-linolenic acid is a kind of polyunsaturated fatty acid that has important nutrition and health care to be worth, and it can not synthesize at inside of human body, can only absorb from food, and its nourishing function mainly contains: 1) increase intelligence, improve vision protection; 2) blood fat reducing, reduction hypertension, inhibition thrombotic diseases, prevention myocardial infarction and cerebral infarction promote insulin secretion, prolongation hypoglycemic effect, inhibition complication; 3) recover human nerve internal secretion, removing interior free yl, enhancing body immunologic function, reparation damaged cell, endocrine regulation; 4) generation and the transfer of inhibition cancer.
Because fatty acid component is complicated in the natural fats and oils, and the existence of saturated fatty acid often influences tiring of polyunsaturated fatty acid physiological function.Therefore, enrichment from natural fats and oils such as polyunsaturated fatty acid such as alpha-linolenic acid, α-linolic acid, DHA is come out, become a quite valuable practical technique.
The method of enriching polyunsaturated fatty acid has the crystallizing process under low temperature, an alkali metal salt precipitator method, molecular distillation method, urea adduct method, silver ion complexation partition method, lipase method of enrichment etc. at present.(Hubei Polytichnic College's journal, 2000,15 (1): the unsaturated fatty acids in the silkworm chrysalis oil that 58-60) adopted the freeze crystallization enrichment such as Zhang Yingqing.(amino acid and Biological resources, 2006,28 (1): 80-82) adopt organic solvent to study the extractive technique of tussah pupal fat such as Li Zhidong.The grease that above document relates to silkworm chrysalis or certain insect extracts, but does not have the relevant report of extraction of pine moth grease and polyunsaturated fatty acid enrichment.
Summary of the invention
The object of the present invention is to provide the beneficiation technologies of the polyunsaturated fatty acid that is rich in alpha-linolenic acid that a kind of raw material sources are extensive, with low cost, production efficiency is high.
The urea adduct method that the present invention adopts is characterized in fatty acid mixt is separated by the difference of lipid acid degree of unsaturation, its principle is that urea molecule can form more stable crystal inclusion compound with saturated fatty acid or monounsaturated fatty acids and separates out in crystallisation process, and polyunsaturated fatty acid is because pair keys are more, carbochain is crooked, have certain sterie configuration is difficult for by urea clathration.Therefore, adopt filtration or centrifugal method to remove the inclusion compound that saturated fatty acid and single not inclusion lipid acid and urea form, can obtain the polyunsaturated fatty acid of higher degree.
The present invention's method of enriching polyunsaturated fatty acid from pine moth may further comprise the steps:
1) dry, pulverizing: with the layering of pine moth larva, every layer thickness is no more than 3cm, places xeothermic equipment crushed after being dried;
2) grease extracts: the pine moth after the pulverizing was extracted 3-5 hour down at 40～60 ℃ with the sherwood oil of 10 times of volumes, and the centrifuging and taking supernatant obtains the pine moth grease under 30 ℃, after steaming petroleum ether on the rotatory evaporator;
3) grease is refining: with resulting pine moth grease in-4 ℃, 5000 rev/mins centrifugal 15 minutes, obtain the pine moth grease after refining;
4) urea clathration: was that 1:4 prepares with urea and alcohol by mass volume ratio, is stirred to solution clarification under 40～60 ℃, mixes back stirring 4～6 hours with purified pine moth grease, in-10 ℃～1 ℃ following freezing and crystallizing 10～16 hours; The quality of described urea and mixed fatty acid is preferably than scope and is 6:1～3:1
5) results polyunsaturated fatty acid: the crystallisate behind the inclusion is centrifugal 15 minutes in-4 ℃, 5000 rev/mins, remove crystal clathrate, boil off urea and alcohol under 30 ℃ on rotatory evaporator, promptly obtain polyunsaturated fatty acid product, wherein content of polyunsaturated fatty acid is 80～90%.
Described 1) preferably the pine moth larva is placed 55 ℃ of dry 24h of xeothermic equipment in the step, be ground into the sample of 60 order thicknesses.
Described 2) available filtration method replaces centrifugation in the step.
Compared with prior art, the present invention has following advantage:
1, first with the Biological resources of forest major pest pine moth as the production polyunsaturated fatty acid.Because pine moth is very huge in the stock number of occurring in nature, the past all treats as insect and rubbish, does not obtain utilizing.Therefore, the cost that adopts the technology of the present invention to produce polyunsaturated fatty acid will significantly reduce, and economic benefit is fairly obvious.
2, after the technology of the present invention industrialization, pine moth can significantly be reduced its harm amount at occurring in nature by the mass-producing development and use, reduces the forestry loss, has also avoided the use of a large amount of chemical pesticides simultaneously, has good ecological.
3, adopt the refining pine moth grease of refrigerated centrifugation, convenient and swift and can prevent the oxidation of unsaturated fatty acids, be a kind of simple and practical technology.
Embodiment
Embodiment 1:
20kg pine moth larva divided be placed in 55 ℃ of xeothermic equipment of air blast dry 24 hours, every layer thickness is 2cm.Be ground into the sample of 60 order thicknesses then with pulverizer.The sherwood oil that with boiling range is 10 times of volumes of 30-60 ℃ extracted 5 hours down at 40 ℃, and centrifugal steaming petroleum ether obtains pine moth oil 2.9kg.This oil is-4 ℃, 5000 rev/mins following frozen centrifugations 15 minutes, obtains the pine moth oil 2.8kg after refining.Then 17kg urea and 68L alcohol are mixed, under 40 ℃, in reactor, be stirred to the solution clarification, mix with the 2.8kg treated oil then, stirred 4 hours, again in-10 ℃ of following freezing and crystallizings 10 hours.Take out material ,-4 ℃, 5000 rev/mins following frozen centrifugations 15 minutes, remove crystal clathrate, boil off solvent, obtain polyunsaturated fatty acid product 0.53kg, content of polyunsaturated fatty acid is 81.2%.
Embodiment 2:
20kg pine moth larva divided be placed in 55 ℃ of xeothermic equipment of air blast dry 24 hours, every layer thickness is 3cm.Be ground into the sample of 60 order thicknesses then with pulverizer.The sherwood oil that with boiling range is 10 times of volumes of 30-60 ℃ extracted 4 hours down at 50 ℃, and centrifugal steaming petroleum ether obtains pine moth oil 3.1kg.This oil is-4 ℃, 5000 rev/mins frozen centrifugations 15 minutes, obtains the pine moth oil 3.0kg after refining.15kg urea and 60L alcohol are mixed, under 50 ℃, in reactor, be stirred to the solution clarification, mix with the 3.0kg treated oil then, stirred 5 hours, again in-4 ℃ of following freezing and crystallizings 12 hours.Take out material ,-4 ℃, 5000 rev/mins following frozen centrifugations 15 minutes, remove crystal clathrate, boil off solvent, obtain polyunsaturated fatty acid product 0.66kg, content of polyunsaturated fatty acid is 83.6%.
Embodiment 3:
20kg pine moth larva divided be placed in 55 ℃ of xeothermic equipment of air blast dry 24 hours, every layer thickness is 2cm.Be ground into the sample of 60 order thicknesses then with pulverizer.The sherwood oil that with boiling range is 10 times of volumes of 30-60 ℃ extracted 5 hours down at 60 ℃, and centrifugal steaming petroleum ether obtains pine moth oil 3.3kg.This oil is-4 ℃, 5000 rev/mins frozen centrifugations 15 minutes, obtains the pine moth oil 3.1kg after refining.12kg urea and 48L alcohol are mixed, under 60 ℃, in reactor, be stirred to the solution clarification, mix with the 3.1kg treated oil then, stirred 6 hours, again in-4 ℃ of following freezing and crystallizings 16 hours.Take out material ,-4 ℃, 5000 rev/mins following frozen centrifugations 15 minutes, remove crystal clathrate, boil off solvent, obtain polyunsaturated fatty acid product 0.72kg, content of polyunsaturated fatty acid is 84.2%.
Embodiment 4:
20kg pine moth larva divided be placed in 55 ℃ of xeothermic equipment of air blast dry 24 hours, every layer thickness is 2cm.Be ground into the sample of 60 order thicknesses then with pulverizer.The sherwood oil that with boiling range is 10 times of volumes of 30-60 ℃ extracted 3 hours down at 50 ℃, and centrifugal steaming petroleum ether obtains pine moth oil 3.1kg.This oil is-4 ℃, 5000 rev/mins following frozen centrifugations 15 minutes, obtains the pine moth oil 3.0kg after refining.12kg urea and 48L alcohol are mixed, under 60 ℃, in reactor, be stirred to the solution clarification, mix with the 3.0kg treated oil then, stirred 5 hours, again in-4 ℃ of following freezing and crystallizings 13 hours.Take out material ,-4 ℃, 5000 rev/mins following frozen centrifugations 15 minutes, remove crystal clathrate, boil off solvent, obtain polyunsaturated fatty acid product 0.68kg, content of polyunsaturated fatty acid is 86.2%.
Embodiment 5:
20kg pine moth larva divided be placed in 55 ℃ of xeothermic equipment of air blast dry 24 hours, every layer thickness is 2cm.Be ground into the sample of 60 order thicknesses then with pulverizer.The sherwood oil that with boiling range is 10 times of volumes of 30-60 ℃ extracted 3 hours down at 60 ℃, and centrifugal steaming petroleum ether obtains pine moth oil 3.2kg.This oil is-4 ℃, 5000 rev/mins following frozen centrifugations 15 minutes, obtains the pine moth oil 3.1kg after refining.10kg urea and 40L alcohol are mixed, under 55 ℃, in reactor, be stirred to the solution clarification, mix with the 3.1kg treated oil then, stirred 5 hours, again in-4 ℃ of following freezing and crystallizings 14 hours.Take out material ,-4 ℃, 5000 rev/mins following frozen centrifugations 15 minutes, remove crystal clathrate, boil off solvent, obtain polyunsaturated fatty acid product 0.65kg, content of polyunsaturated fatty acid is 81.9%.
Embodiment 6:
20kg pine moth larva divided be placed in 55 ℃ of xeothermic equipment of air blast dry 24 hours, every layer thickness is 2cm.Be ground into the sample of 60 order thicknesses then with pulverizer.The sherwood oil that with boiling range is 10 times of volumes of 30-60 ℃ extracted 5 hours down at 45 ℃, and centrifugal steaming petroleum ether obtains pine moth oil 3.1kg.This oil is-4 ℃, 5000 rev/mins following frozen centrifugations 15 minutes, obtains the pine moth oil 3.0kg after refining.12kg urea and 48L alcohol are mixed, under 60 ℃, in reactor, be stirred to the solution clarification, mix with the 3.0kg treated oil then, stirred 5 hours, again in 0 ℃ of following freezing and crystallizing 15 hours.Take out material ,-4 ℃, 5000 rev/mins following frozen centrifugations 15 minutes, remove crystal clathrate, boil off solvent, obtain polyunsaturated fatty acid product 0.68kg, content of polyunsaturated fatty acid is 83.8%.
Embodiment 7:
20kg pine moth larva divided be placed in 55 ℃ of xeothermic equipment of air blast dry 24 hours, every layer thickness is 2cm.Be ground into the sample of 60 order thicknesses then with pulverizer.The sherwood oil that with boiling range is 10 times of volumes of 30-60 ℃ extracted 3 hours down at 60 ℃, and centrifugal steaming petroleum ether obtains pine moth oil 3.2kg.This oil is-4 ℃, 5000 rev/mins following frozen centrifugations 15 minutes, obtains the pine moth oil 3.1kg after refining.12kg urea and 48L alcohol are mixed, under 60 ℃, in reactor, be stirred to the solution clarification, mix with the 3.1kg treated oil then, stirred 3 hours, again in 0 ℃ of following freezing and crystallizing 15 hours.Take out material ,-4 ℃, 5000 rev/mins following frozen centrifugations 15 minutes, remove crystal clathrate, boil off solvent, obtain polyunsaturated fatty acid product 0.63kg, content of polyunsaturated fatty acid is 82.1%.
Claims (4)
1. the method for an enriching polyunsaturated fatty acid from pine moth is characterized in that: may further comprise the steps:
1) dry, pulverizing: with the layering of pine moth larva, every layer thickness is no more than 3cm, places xeothermic equipment crushed after being dried;
2) grease extracts: the pine moth after the pulverizing was extracted 3-5 hour down at 40～60 ℃ with the sherwood oil of 10 times of volumes, and the centrifuging and taking supernatant liquor obtains the pine moth grease after the steaming petroleum ether;
3) grease is refining: with resulting pine moth grease in-4 ℃, 5000 rev/mins centrifugal 15 minutes, obtain the pine moth grease after refining;
4) urea clathration: is to prepare at 1: 4 urea and alcohol by mass volume ratio, under 40～60 ℃, be stirred to the solution clarification, mixing the back with purified pine moth grease stirred 4～6 hours, in-10 ℃～1 ℃ following freezing and crystallizing 10～16 hours, wherein urea and purified pine moth oil quality ratio were 6: 1～3: 1;
5) results polyunsaturated fatty acid: with the crystallisate behind the inclusion in-4 ℃, 5000 rev/mins centrifugal 15 minutes, remove crystal clathrate, boil off alcohol, promptly obtain polyunsaturated fatty acid product.
2. according to claim 1 a kind of from pine moth the method for enriching polyunsaturated fatty acid, it is characterized in that: 1) in the step pine moth larva is placed 55 ℃ of dry 24h of xeothermic equipment, be ground into the sample of 60 order thicknesses.
3. according to claim 1 a kind of from pine moth the method for enriching polyunsaturated fatty acid, it is characterized in that: 2) available filtration method replaces centrifugation in the step.
4. according to claim 1 a kind of from pine moth the method for enriching polyunsaturated fatty acid, it is characterized in that: content of polyunsaturated fatty acid is 80～90% in the product.
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| CN103333747A (en) * | 2013-06-05 | 2013-10-02 | 安徽农业大学 | Method for gathering and purifying polyunsaturated fatty acid from mixed fatty acid of trichosanthes seed oil |
| CN105316113A (en) * | 2015-04-21 | 2016-02-10 | 江南大学 | Polyunsaturated fatty acid enriching method |
| CN108441319A (en) * | 2018-03-15 | 2018-08-24 | 佛山汇沐化学科技有限公司 | A kind of extracting method of julid oil and its application |
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| CN1696261A (en) * | 2005-06-25 | 2005-11-16 | 中国科学院新疆理化技术研究所 | Method for gathering jpolyunsaturated fatty acid and esterified matters oil through inclusion method of urea |
| CN101050171A (en) * | 2005-04-11 | 2007-10-10 | 东部韩农化学株式会社 | Method for producing unsaturated fatty acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101050171A (en) * | 2005-04-11 | 2007-10-10 | 东部韩农化学株式会社 | Method for producing unsaturated fatty acid |
| CN1696261A (en) * | 2005-06-25 | 2005-11-16 | 中国科学院新疆理化技术研究所 | Method for gathering jpolyunsaturated fatty acid and esterified matters oil through inclusion method of urea |
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| 刘高强等.松毛虫作为新资源食品的可行性及其前景分析.中国食品学报.2003,504-507. * |
| 刘高强等.松毛虫资源开发及其资源化管理的初步设想.西北林学院学报.2004,19(4),119-123. * |
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