CN106478408A - The method for extracting DPA, EPA and DHA from fish processing by-product - Google Patents
The method for extracting DPA, EPA and DHA from fish processing by-product Download PDFInfo
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- CN106478408A CN106478408A CN201510550015.XA CN201510550015A CN106478408A CN 106478408 A CN106478408 A CN 106478408A CN 201510550015 A CN201510550015 A CN 201510550015A CN 106478408 A CN106478408 A CN 106478408A
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- dha
- epa
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses the method for extracting DPA, EPA and DHA from fish processing by-product.In byproduct after fish processing, fish oil content is very high, contain DPA, EPA and DHA in fish oil, fish processing by-product is worn into slurry by the present invention, extracted with organic solvent, extract esterification, distilled with wiped-film still again, by degassing, three technical steps of pre- thermal distillation and distillation, wherein de-airing step is carried out under conditions of 1-2mbar in temperature 20-30 DEG C, system pressure；Preheating distilation steps are distilled under conditions of temperature 170-200 DEG C, system pressure 0.001-0.01mbar, 150-250 rev/min of knifing spinner velocity；Distilation steps are distilled under conditions of temperature 250-350 DEG C, system pressure 0.001-0.01mbar, 150-250 rev/min of knifing spinner velocity, collect 290-310 DEG C when cut, that is, obtain the compound containing EPA, DHA and DPA of higher degree.Extract in separation process whole, pollution-free, product property is stable, is effectively utilized resource, reduces product cost, increased the competitiveness of product.
Description
Technical field
The present invention relates to the method for extracting DPA, EPA and DHA from fish processing by-product, belongs to marine product technical field of comprehensive utilization.
Background technology
Byproduct can be left after fish processing, including fish head, fish scale, fish oil and fish guts, the traditional processing method of these byproducts be dry after as produce feed raw material, but these byproducts are in dry run, the foul odour of effusion causes greatly pollution to environment, this rough machining method fails to make full use of to contained effective ingredient in fish processing by-product, causes waste.In byproduct after fish processing, fish oil content is very high, it is well known that containing DPA, EPA and DHA, i.e. clupanodonic acid, eicosapentaenoic acid and DHA in fish oil, they belong to ω -3 polyenoic fatty acid, and these three aliphatic acid have the BA of multiple uniquenesses to human body：EPA has to be improved blood circulation, softening blood vessel, adjustment blood fat, reduces blood pressure and blood sugar and antiinflammatory action；DHA and DPA have nutrition brain, the extension to nerve cell axons and the formation of new projection and play an important role; the normal physiological activity of nerve cell can be maintained; participate in human thinking and memory forming process; with anti-aging; reducing blood lipid and the sanguimotor effect of improvement, are the important composition compositions of brain cell film, participate in the formation of brain cell, promote fetus and children's brain development, protection eyesight, adjust immune and antitumaous effect.People have found that they have therapeutic action to some diseases again in the recent period：EPA has been developed that the medicine as treatment artery sclerosis and high fat of blood；Also find that they have treatment and prevention effect to type ii diabetes, fatty liver and prostatitis.Therefore, DPA, EPA and DHA are extracted using fish processing by-product, it is possible to increase the comprehensive utilization value of fish processed goods.
Content of the invention
The purpose of the present invention, it is exactly to provide one kind to extract DPA, EPA and DHA from fish processing by-product, method, using carrying out the mode of molecular clock and extracting DPA, EPA and the DHA in fish processing by-product separating after solvent extraction, overcome the shortcomings of that tradition is extracted existing for separate mode.
For achieving the above object, such measure present invention employs：The method for extracting DPA, EPA and DHA from fish processing by-product, comprises the steps：
（1）Byproduct after fish is processed is cleaned, and is 1 with solid-liquid weight ratio：The ratio of 1-1.2 adds water, and pulp of regrinding obtains the miscellaneous homogenate of fish；
（2）Take the miscellaneous homogenate organic solvent of fish to extract 1-3 time, the ratio of organic solvent homogenate volume miscellaneous with fish is 1：1.2-1.5, collects extract, and the extract obtained containing DPA, EPA and DHA grease is standby, and the organic solvent refers to petroleum ether or ether；
（3）Extract reclaims organic solvent, obtains the fish oil containing DPA, EPA and DHA, takes 0.3mol/L sodium methoxide isopyknic with fish oil and mix, and after nitrogen charging is stirred 10 minutes under room temperature condition, adjusts pH value to 7.0-7.2, reclaims methyl alcohol, obtain the fish oil of esterification；
（4）Molecular clock is carried out to esterification fish oil, including degassing, three technical steps of pre- thermal distillation and distillation, wherein de-airing step is de-gassed under conditions of 1-2mbar in temperature 20-30 DEG C, system pressure；Preheating distilation steps are sent in pre-thermal level distiller with 15-20 kg/hour of charging rate in fish oil, are distilled under conditions of temperature 170-200 DEG C, system pressure 0.001-0.01mbar, 150-250 rev/min of knifing spinner velocity；Distilation steps are sent in distiller with 5-20 kg/hour of charging rate, distill under conditions of temperature 250-350 DEG C, system pressure 0.001-0.01mbar, 150-250 rev/min of knifing spinner velocity, collect 290-310 DEG C when cut, that is, obtain the compound containing EPA, DHA and DPA of higher degree.
The present invention for taking above-mentioned measure, takes full advantage of remaining byproduct after fish processing, is comprehensively utilized, especially with organic solvent extractionprocess and molecularly distilled, effectively EPA, DHA and the DPA in the byproduct being present in after fish processing is extracted and separate, the compound of higher degree is achieved, is turned waste into wealth, extract in separation process whole, pollution-free, product property is stable, is effectively utilized resource, product cost is reduced, increased the competitiveness of product.
For describing the present invention in detail, the present invention is described in further detail with reference to embodiment：
Embodiment 1
（1）Take the byproduct after 100 kilograms of fish processing to clean, 100 kg of water are added, pulpous state is worn into fiberizer and obtains the miscellaneous homogenate of fish；
（2）The ratio of 1 liter of petroleum ether being added with the miscellaneous homogenate per 1.2 liters of fishes, petroleum ether being added and is extracted in the miscellaneous homogenate of fish, collects extract, the extract obtained containing DPA, EPA and DHA grease is standby；
（3）Extract reclaims organic solvent, obtains the fish oil containing DPA, EPA and DHA, takes 0.3mol/L sodium methoxide isopyknic with fish oil and mix, and after nitrogen charging is stirred 10 minutes under room temperature condition, adjusts pH value to 7.0-7.2, reclaims methyl alcohol, obtain the fish oil of esterification；
（4）Molecular clock is carried out to esterification fish oil, use wiped-film still, the whole workflow of wiped-film still includes degassing, three technical steps of pre- thermal distillation and distillation, and wherein de-airing step is de-gassed under conditions of 1mbar in 20 DEG C of temperature, system pressure；Preheating distilation steps are sent in pre-thermal level distiller with 15 kgs/hour of charging rate in fish oil, are distilled under conditions of 170 DEG C of temperature, system pressure 0.001mbar, 150 revs/min of knifing spinner velocity；Distilation steps are sent in distiller with 5 kgs/hour of charging rate, distill under conditions of 250 DEG C of temperature, system pressure 0.001mbar, 150 revs/min of knifing spinner velocity, collect 290 DEG C when cut, that is, obtain the compound containing EPA, DHA and DPA of higher degree.
Embodiment 2
（1）Take the byproduct after 100 kilograms of fish processing to clean, 120 kg water is added, pulpous state is worn into fiberizer and obtains the miscellaneous homogenate of fish；
（2）The ratio of 1 liter of ether being added with the miscellaneous homogenate per 1.5 liters of fishes, ether being added and extracted in the miscellaneous homogenate of fish, so extraction 3 times, collects extract, and the extract obtained containing DPA, EPA and DHA grease is standby；
（3）Extract reclaims organic solvent, obtains the fish oil containing DPA, EPA and DHA, takes 0.3mol/L sodium methoxide isopyknic with fish oil and mix, and after nitrogen charging is stirred 10 minutes under room temperature condition, adjusts pH value to 7.0-7.2, reclaims methyl alcohol, obtain the fish oil of esterification；
（4）Molecular clock is carried out to esterification fish oil, use wiped-film still, the whole workflow of wiped-film still includes degassing, three technical steps of pre- thermal distillation and distillation, and wherein de-airing step is de-gassed under conditions of 2mbar in 30 DEG C of temperature, system pressure；Preheating distilation steps are sent in pre-thermal level distiller with 20 kgs/hour of charging rate in fish oil, are distilled under conditions of 200 DEG C of temperature, system pressure 0.01mbar, 250 revs/min of knifing spinner velocity；Distilation steps are sent in distiller with 20 kgs/hour of charging rate, distill under conditions of 350 DEG C of temperature, system pressure 0.01mbar, 250 revs/min of knifing spinner velocity, collect 310 DEG C when cut, that is, obtain the compound containing EPA, DHA and DPA of higher degree.
Embodiment 3
（1）Take the byproduct after 100 kilograms of fish processing to clean, 110 kg of water are added, pulpous state is worn into fiberizer and obtains the miscellaneous homogenate of fish；
（2）The ratio of 1 liter of petroleum ether being added with the miscellaneous homogenate per 1.3 liters of fishes, petroleum ether being added and extracted in the miscellaneous homogenate of fish, so extraction 2 times, collects extract, and the extract obtained containing DPA, EPA and DHA grease is standby；
（3）Extract reclaims organic solvent, obtains the fish oil containing DPA, EPA and DHA, takes 0.3mol/L sodium methoxide isopyknic with fish oil and mix, and after nitrogen charging is stirred 10 minutes under room temperature condition, adjusts pH value to 7.2, reclaims methyl alcohol, obtain the fish oil of esterification；
（4）Molecular clock is carried out to esterification fish oil, use wiped-film still, the whole workflow of wiped-film still includes degassing, three technical steps of pre- thermal distillation and distillation, and wherein de-airing step is de-gassed under conditions of 1.5mbar in 25 DEG C of temperature, system pressure；Preheating distilation steps are sent in pre-thermal level distiller with 20 kgs/hour of charging rate in fish oil, are distilled under conditions of 190 DEG C of temperature, system pressure 0.005mbar, 200 revs/min of knifing spinner velocity；Distilation steps are sent in distiller with 15 kgs/hour of charging rate, distill under conditions of 300 DEG C of temperature, system pressure 0.005mbar, 200 revs/min of knifing spinner velocity, collect 300 DEG C when cut, that is, obtain the compound containing EPA, DHA and DPA of higher degree.
Claims (1)
1. the method for extracting DPA, EPA and DHA from fish processing by-product, it is characterised in that methods described comprises the steps：
（1）Byproduct after fish is processed is cleaned, and is 1 with solid-liquid weight ratio：The ratio of 1-1.2 adds water, and pulp of regrinding obtains the miscellaneous homogenate of fish；
（2）Take the miscellaneous homogenate organic solvent of fish to extract 1-3 time, the ratio of organic solvent homogenate volume miscellaneous with fish is 1：1.2-1.5, collects extract, and the extract obtained containing DPA, EPA and DHA grease is standby, and the organic solvent refers to petroleum ether or ether；
（3）Extract reclaims organic solvent, obtains the fish oil containing DPA, EPA and DHA, takes 0.3mol/L sodium methoxide isopyknic with fish oil and mix, and after nitrogen charging is stirred 10 minutes under room temperature condition, adjusts pH value to 7.0-7.2, reclaims methyl alcohol, obtain the fish oil of esterification；
（4）Molecular clock is carried out to esterification fish oil, including degassing, three technical steps of pre- thermal distillation and distillation, wherein de-airing step is de-gassed under conditions of 1-2mbar in temperature 20-30 DEG C, system pressure；Preheating distilation steps are sent in pre-thermal level distiller with 15-20 kg/hour of charging rate in fish oil, are distilled under conditions of temperature 170-200 DEG C, system pressure 0.001-0.01mbar, 150-250 rev/min of knifing spinner velocity；Distilation steps are sent in distiller with 5-20 kg/hour of charging rate, distill under conditions of temperature 250-350 DEG C, system pressure 0.001-0.01mbar, 150-250 rev/min of knifing spinner velocity, collect 290-310 DEG C when cut, that is, obtain the compound containing EPA, DHA and DPA of higher degree.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510550015.XA CN106478408A (en) | 2015-09-01 | 2015-09-01 | The method for extracting DPA, EPA and DHA from fish processing by-product |
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| CN201510550015.XA CN106478408A (en) | 2015-09-01 | 2015-09-01 | The method for extracting DPA, EPA and DHA from fish processing by-product |
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| CN106478408A true CN106478408A (en) | 2017-03-08 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108185427A (en) * | 2018-02-11 | 2018-06-22 | 成都图径生物科技有限公司 | Composition for relieving asthenopia containing flake, theanine and phosphatidylserine |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101255379A (en) * | 2007-08-16 | 2008-09-03 | 张义兴 | Purified fur seal oil and method for preparing the same |
| CN102839047A (en) * | 2012-09-12 | 2012-12-26 | 连云港职业技术学院 | Method for extracting fish oil and producing taurine seafood condiments by using hairtail and leftovers of hairtail |
| CN104478694A (en) * | 2014-12-02 | 2015-04-01 | 东莞市荷花食品有限公司 | Method for extracting docosahexenoic acid and eicosapentaenoic acid from seriola quinqueradiata |
-
2015
- 2015-09-01 CN CN201510550015.XA patent/CN106478408A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101255379A (en) * | 2007-08-16 | 2008-09-03 | 张义兴 | Purified fur seal oil and method for preparing the same |
| CN102839047A (en) * | 2012-09-12 | 2012-12-26 | 连云港职业技术学院 | Method for extracting fish oil and producing taurine seafood condiments by using hairtail and leftovers of hairtail |
| CN104478694A (en) * | 2014-12-02 | 2015-04-01 | 东莞市荷花食品有限公司 | Method for extracting docosahexenoic acid and eicosapentaenoic acid from seriola quinqueradiata |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108185427A (en) * | 2018-02-11 | 2018-06-22 | 成都图径生物科技有限公司 | Composition for relieving asthenopia containing flake, theanine and phosphatidylserine |
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Application publication date: 20170308 |