CN107699343A - A kind of degumming tech of tunny fish oil - Google Patents
A kind of degumming tech of tunny fish oil Download PDFInfo
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- CN107699343A CN107699343A CN201710747327.9A CN201710747327A CN107699343A CN 107699343 A CN107699343 A CN 107699343A CN 201710747327 A CN201710747327 A CN 201710747327A CN 107699343 A CN107699343 A CN 107699343A
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- fish oil
- degumming
- tuna
- enzymolysis
- acid
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/003—Refining fats or fatty oils by enzymes or microorganisms, living or dead
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/16—Refining fats or fatty oils by mechanical means
Abstract
The present invention relates to a kind of degumming tech of tunny fish oil, belong to technical field of aquatic product processing.The degumming tech of the present invention comprises the following steps：Tuna crude fish oil is pre-processed；Add distilled water in tuna crude fish oil after the pre-treatment, be stirring evenly and then adding into it is compound go glycosyl enzyme tentatively to be digested, obtain tentatively digesting fish oil；Compound protease is added in tentatively enzymolysis fish oil to be digested again, obtains digesting fish oil；Destroy the enzyme treatment is carried out to enzymolysis fish oil heating, room temperature is subsequently cooled to, centrifuges, take upper strata to float grease, be primary degumming fish oil；Acid degumming agent is added in primary degumming fish oil and carries out acid degumming, it is the tuna oil after degumming to be then centrifuged for taking supernatant.The degumming tech of the present invention, course of reaction is gentle, easily controllable, and degumming effect is good, efficiency high, does not destroy effective nutriment in tunny fish oil.
Description
Technical field
The invention belongs to technical field of aquatic product processing, is related to a kind of degumming tech of tunny fish oil.
Background technology
At present, production and processing sale of the domestic enterprise to tuna, in addition to marketing fresh, mainly in the form of frozen fish willow
Export to foreign countries, substantial amounts of discarded object, such as red meat part, fish head, fish-skin, internal organ, fin are produced in its process.Due to
Process technology falls behind, and these leftover bits and pieces are mainly produced and processed into fish meal by wet processing (boiling squeezing), are during which produced with fish meal
Raw crude fish oil is because color is deep, and refining degumming is decolourized difficult and producing level is not high, and this is also to perplex the problem of fish oil enterprise for many years,
Therefore, further research refining techniques to its intensive processing technology and comprehensively utilizes important in inhibiting.
The more alkali refinings that are directly entered without Degumming Procedures of fish oil refinery practice that domestic enterprise uses operate.With regard to tuna
For crude fish oil, although its content of phospholipid is not high, because it is rich in the impurity such as protein and mucus, viscosity is high, and color is deep,
Fishy smell weight, if directly carrying out alkali refining without degumming process, easily occur turning over bubble phenomenon in subsequent operation, and alkali can be increased
Alkali charge and carclazyte dosage during refining.Research shows that the domestic degumming research on deep sea fish oil is concentrated mainly on acid system degumming,
And use phosphoric acid more, fish oil is extracted from waste sleeve-fish liver as Chinese patent application CN201010176523.3 discloses one kind
Method, using phosphoric acid to obtained crude fish oil carry out degumming process, and test prove directly use phosphoric acid degumming for rich in
The crude fish oil degumming of various impurity is not appropriate for, and degumming rate is low and gained degummed oil color is deep.
The content of the invention
The purpose of the present invention is in view of the above-mentioned problems existing in the prior art, it is proposed that a kind of degumming work of tunny fish oil
Skill, course of reaction is gentle, easily controllable, and degumming effect is good, efficiency high, does not destroy effective nutriment in tunny fish oil.
The purpose of the present invention can be realized by following technical proposal：A kind of degumming tech of tunny fish oil, the degumming
Technique comprises the following steps：
Tuna crude fish oil is pre-processed；
Add distilled water in tuna crude fish oil after the pre-treatment, be stirring evenly and then adding into it is compound go glycosyl enzyme carry out just
Step enzymolysis, obtains tentatively digesting fish oil；
Compound protease is added in tentatively enzymolysis fish oil to be digested again, obtains digesting fish oil；
Destroy the enzyme treatment is carried out to enzymolysis fish oil heating, room temperature is subsequently cooled to, centrifuges, take upper strata to float grease, be first
Level degumming fish oil；
Acid degumming agent is added in primary degumming fish oil and carries out acid degumming, after being then centrifuged for taking supernatant to be degumming
Tuna oil.
The present invention is directed to the characteristics of content of phospholipid is few, protein and mucous substance are more in tuna crude fish oil, using first enzyme
Solution again acid degumming method to tuna crude fish oil carry out degumming process, course of reaction is gentle, easily controllable, degumming effect
It is good, efficiency high, after degumming crude fish oil color and luster be improved significantly, be advantageous to the progress of follow-up depickling decoloration and deodorization；Do not destroy fish
Effective nutriment in oil, the health-care fish oil rich in DHA and EPA can further be made, develop into the prevention and treatment heart
The functional products such as cranial vascular disease, brain tonic and intelligence development, there are wide market prospects.According to the existing conventional processing skill of tuna
Art, tuna crude fish oil are caused by processing again by removal fresh meat leftover bits and pieces, and content of phospholipid is low, rich in protein and glues
The impurity such as liquid, wherein mucous substance mainly include the various active materials such as mucopolysaccharide, glycolipid, glycoprotein, immunoglobulin and enzyme.
The characteristics of for tuna crude fish oil, the enzymolysis process in the present invention are carried out in two steps, and first remove glycosyl enzyme by sugared egg using compound
White and glycolipid sugar chain is removed and decomposed, and mucopolysaccharide is decomposed；Then compound protease is used again by protein degradation.
The small molecule carbohydrate and amino acid, small-molecular peptides of degraded generation are soluble in water, can be removed in the water-oil separating in later stage.After enzymolysis
Glycosyl enzyme and albumen enzyme-deactivating can will be removed by destroy the enzyme treatment, will be removed by centrifugal sedimentation in bottom.Tuna crude fish oil passes through
Enzymolysis processing is crossed, protein and polysaccharose substance are removed, and impurity is reduced, lighter, and clarification is a lot, but wherein also contains
A small amount of phosphatide, metal ion and other micro gelatin substances etc..These can be remained substantially by the use of acid degumming agent
Remaining impurity removes, and obtains the fish oil that color and luster is clarified well.
Preferably, the pretreatment is that tuna crude fish oil is heated into 80~100 DEG C of 3~5min of processing.
Except mucopolysaccharide, glycolipid, glycoprotein, immune globulin are ultrawhite in mucous substance in tuna crude fish oil, also contain
A variety of enzyme isoreactivity materials, the degumming tech in later stage can be had an impact, thus the present invention pretreatment when using high-temperature heating
Mode inactivates these active materials, degumming process is effectively carried out.
Preferably, the volume ratio of the tuna crude fish oil and distilled water is 1:(1~3).
To remove glycosyl enzyme and compound protease be mostly water-soluble enzyme due to compound, therefore the present invention adds in tuna crude fish oil
Add distilled water and be sufficiently stirred to form oil water mixture so that enzymolysis process can react on oil-water interfaces, and produce hydrolysis
Thing removing soluble in water.Water addition is excessive, is unfavorable for later stage water-oil separating, and water addition is very few, and formation oil-water interfaces are small, no
Carried out beneficial to enzyme digestion reaction.
Preferably, described, compound to remove glycosyl enzyme be that weight ratio is 10:(3~7):The exoglycosidase of (2~5), inscribe
The mixture of glycosidase and osamine enzyme.
Exoglycosidase can discharge oligosaccharides from the non-reducing end of sugar chain, and endo-type glycosidase can be single-minded inside sugar chain
Property cuts some glycosidic bond, and osamine enzyme (N~glycosidase) can hydrolyze oligosaccharides~G1cNAc~Asn~peptide, discharge complete widow
Sugar, and it is wider to oligosaccharide structure specificity, and mannose type, compound, hybrid type sugar chains are releasable, releasably containing 3~40
The glycosyl of the glycopeptide molecule of individual amino acid, can be by the quick and complete drop of the sugar chain of glycoprotein or glycolipid by the synergy of these enzymes
Solution.
Preferably, the addition for removing glycosyl enzyme is the 0.3~1.5% of tuna crude fish oil weight, preliminary enzymolysis
Process be at 35~55 DEG C, ultrasonic wave added stirring enzymolysis 30~60min.
Preferably, supersonic frequency during the preliminary enzymolysis is 26KHz, ultrasonic power is 20~40w.
It is compound to go glycosyl enzyme that there is optimal enzymolysis efficiency at 35~55 DEG C.Appropriate supersound process can strengthen enzyme
Hydrophobicity, the preferably same Binding Capacity in enzymolysis, improves the activity of resolvase, and the cavitation effect of ultrasonic wave can also improve enzymolysis
Speed, accelerate enzymolysis process.But ultrasonic power is too high, processing time it is long can be because of ultrasonic impact activity center, in certain journey
The structure of destructive enzyme on degree and reduce enzyme activity.
Preferably, it is 10 that the compound protease, which is weight ratio,:(5~8):(3~6):The neutral proteinase of (2~5),
Papain, flavor protease, the mixture of trypsase.
The present invention is compounded to thick according to the species and feature of protein in tuna crude fish oil from above-mentioned multiple protein enzyme
Fish oil is digested, and can obtain wider cleavage site, accelerates hydrolysis rate, reaches the more preferable effect of complete hydrolysis.
Preferably, the addition of the compound protease is the 0.5~1.5% of tuna crude fish oil weight, enzyme again
The process of solution is 40~75min of ultrasonic wave added stirring enzymolysis at 35~65 DEG C.
Preferably, during the enzymolysis again, temperature rises to 65 with 0.4~0.75 DEG C/min speed from 35 DEG C
℃。
Because the optimum temperature of different protease hydrolyzeds is different, the present invention is in enzymolysis process using the side gradually heated up
Formula can make different protease can fully be had an effect within the scope of most suitable temperature, be imitated with the enzymolysis for reaching optimal
Fruit.
Preferably, the supersonic frequency during enzymolysis again is 26KHz, ultrasonic power is 30~60w.
Preferably, the preliminary enzymolysis and during digesting again added with tuna crude fish oil weight 0.05~
0.1% surfactant.
The present invention with the addition of a small amount of surfactant in the enzymolysis process of tuna crude fish oil, its special parents' knot
Structure, the formation of oil-water emulsion and oil-water interfaces can be promoted so that reaction substrate is able to more fully emulsified, the smaller particle of formation,
So as to increase the surface area that substrate contacts with enzyme, the catalytic efficiency of enzyme is improved, and the addition of a small amount of surfactant will not
The undue emulsification of fish oil is caused, last oil-water separation is influenceed little.
Preferably, the surfactant is the one or more in polysorbas20, polysorbate60, span 20, sorbester p18.
Above-mentioned surfactant can not only improve the catalytic efficiency of enzyme, also have certain protection and stable work to protease
With.
Preferably, the process of the destroy the enzyme treatment is that enzymolysis liquid is heated into 80~100 DEG C of 3~5min of processing.
Preferably, it is (2~1) that the acid degumming agent, which is volume ratio,:The citric acid of (1~2) and the compound of acetic acid.
Under the premise of other conditions identical, a kind of acid is used alone degumming experiment, lemon are carried out to tuna crude fish oil
The degumming rate of acid and acetic acid is far superior to the degumming rate of phosphoric acid and sulfuric acid, and (citric acid degumming rate is 3.27, and the degumming rate of acetic acid is
3.21, the degumming rate of phosphoric acid is 1.56, and the degumming rate of sulfuric acid is that 1.21), the present invention selects citric acid and acetic acid compounding use, by
In the pH of citric acid and acetic acid, the difference of functional group's property, have not to different classes of phosphatide, metal ion and gelatin substance
Same effect, remaining phosphatide in crude fish oil, metal ion and other micro glue classes can be removed using the synergy of the two
Material.It is preferable to the removal effect of impurity in above-mentioned volume range, higher or lower than above-mentioned volume ratio, due to fluid
PH, which changes, can cause some impurity components therein to change, so as to reduce degumming rate.
Preferably, the process of the acid degumming is, by weight percentage, added in primary degumming fish oil
0.5%~1.5% acid degumming agent, 10~30min is stirred at 20~50 DEG C.
When acid degumming agent dosage is in 0.5%~1.5%, the increase of degumming efficiency is obvious, and almost linear growth, exceedes
After 1.5%, degumming rate amplitude of variation is little, it is contemplated that saves production cost, by the control of degumming agent dosage within the above range.Temperature
Degree is preferably beneficial to remove from during 20 DEG C are raised to 50 DEG C, degumming agent is combined with colloid, and degumming rate increases substantially, more than 50 DEG C
Afterwards, degumming rate increase is slow, therefore by degumming temperature control within the above range.Between 10~30min, with the increasing of usually time
Add, degumming rate increase is obvious, after 30min, is further added by the time, the change of degumming rate is no longer obvious, illustrates degumming agent and crude fish oil
Middle colloidal substance is reacted to up to saturation point, therefore controls usually time within the above range.
Compared with prior art, the invention has the advantages that：The present invention is first spent by the way of two steps enzymolysis
Glycosyl enzyme digests to tuna crude fish oil, then is digested with protease, preferentially removes the sugar chain of glycolipid and glycoprotein
And decompose, then by protein degradation, can effectively remove a large amount of existing mucopolysaccharide, glycolipid, glycoprotein and protein in crude fish oil
Deng impurity, and it is sufficiently reserved its active principle；The mode stirred in enzymolysis process using ultrasonic assistant improves enzyme activity, and adds
Added with a small amount of surfactant, so as to improve enzymolysis efficiency；Then degumming agent pair is used as using citric acid and acetic acid compounding again
Remaining impurity carries out degumming process in tuna crude fish oil, and degumming effect is far superior to the phosphoric acid and sulfuric acid that tradition uses；It is whole
Individual course of reaction is gentle, easily controllable, and degumming effect is good, efficiency high, after degumming crude fish oil color and luster be improved significantly, be advantageous to
The progress of follow-up depickling decoloration and deodorization；The effective nutriment not destroyed in fish oil, can further it be made rich in DHA's and EPA
Health-care fish oil, develop into functional products such as prevention and treatment cardiovascular and cerebrovascular disease, brain tonic and intelligence developments, there is wide market
Prospect.
Embodiment
It is the specific embodiment of the present invention below, technical scheme is further described, but the present invention is simultaneously
It is not limited to these embodiments.
The degumming tech in the present invention is further explained below by specific embodiment.
Embodiment 1~7
Degumming tech in the present invention comprises the following steps：
Tuna crude fish oil is heated to 80~100 DEG C and carries out 3~5min of pretreatment, by 1:The volume ratio of (1~3) is in gold
Distilled water is added in marlin crude fish oil, is stirred；
Then add the compound of the 0.3~1.5% of tuna crude fish oil weight and remove glycosyl enzyme and 0.05~0.1% surface
Activating agent, at 35~55 DEG C, ultrasonic wave added stirring carries out 30~60min of preliminary enzymolysis, obtains tentatively digesting fish oil, compound to go
Glycosyl enzyme is that weight ratio is 10:(3~7):The mixture of the exoglycosidase of (2~5), endoglycosidase and osamine enzyme, ultrasound
Frequency is 26KHz, and ultrasonic power is 20~40w；
Tentatively enzymolysis fish oil in add tuna crude fish oil weight 0.5~1.5% compound protease and 0.05~
0.1% surfactant, control temperature rise to 65 DEG C from 35 DEG C with 0.4~0.75 DEG C/min speed, ultrasonic wave added stirring
Carry out digesting 40~75min again, obtain digesting fish oil, compound protease is that weight ratio is 10:(5~8):(3~6):(2~
5) neutral proteinase, papain, flavor protease, the mixture of trypsase, supersonic frequency 26KHz, ultrasonic work(
Rate is 30~60w；
Preliminary enzymolysis and the again surfactant in enzymolysis process are polysorbas20, in polysorbate60, span 20, sorbester p18
It is one or more of.
Enzymolysis liquid is heated to 80~100 DEG C of progress 3~5min of destroy the enzyme treatment, room temperature is cooled to, centrifuges, take upper strata to float
Grease, obtain primary degumming fish oil；
By weight percentage, 0.5~1.5% acid degumming agent is added in primary degumming fish oil, at 20~50 DEG C
10~30min of lower stirring carries out acid degumming, and it is the tuna oil after degumming to be then centrifuged for taking supernatant, acid degumming agent
It is (2~1) for volume ratio:The citric acid of (1~2) and the compound of acetic acid.
Degumming process is carried out to the tuna crude fish oil in embodiment 1~7 according to the parameter of each step in table 1 respectively.
Table 1：The design parameter of tuna crude fish oil degumming tech in embodiment 1~7
Note：Ratio of the glycosyl enzyme proportioning for exoglycosidase, endoglycosidase and osamine enzyme is gone, protease proportioning is neutrality
Protease, papain, flavor protease, the ratio of trypsase, degumming agent proportioning is citric acid, the ratio of acetic acid, table
Face activating agent proportioning is polysorbas20, the ratio of polysorbate60, span 20, sorbester p18 (0 represents to be not added with the surfactant).
Comparative example 1
To tuna crude fish oil without using going glycosyl enzyme to digest, digested using only protease, other and the phase of embodiment 1
Together.
Comparative example 2
Acid degumming is carried out to tuna crude fish oil using phosphoric acid as degumming agent, other are same as Example 1.
Comparative example 3
Acid degumming is carried out to tuna crude fish oil using sulfuric acid as degumming agent, other are same as Example 1.
The present invention is taken off using degumming rate and color and luster as index to tuna crude fish oil in embodiment 1~7, comparative example 1~3
Glue effect is compared, and is taken tuna crude fish oil to be scanned in 190~1100nm wavelength, is found there is absorption maximum at 450nm
Peak, therefore select 450nm absorbance to weigh influence of the degumming agent to tuna crude fish oil color and luster, the comparative result such as institute of table 2
Show.
Table 2：The degumming effect of tuna crude fish oil in embodiment 1~7, comparative example 1~3
In summary, the present invention in caused tuna crude fish oil in existing process according to the characteristics of impurity, passing through
Two steps enzymolysis removes the impurity such as mucopolysaccharide, glycoprotein, glycolipid and protein in tuna crude fish oil, then is gone by acid degumming
Except remaining phosphatide, metal ion and other micro gelatin substances, whole course of reaction is gentle, easily controllable, and degumming effect is good,
Efficiency high, after degumming crude fish oil color and luster be improved significantly, be advantageous to the progress of follow-up depickling decoloration and deodorization；Do not destroy in fish oil
Effective nutriment.
Specific embodiment described herein is only to spirit explanation for example of the invention.Technology belonging to the present invention is led
The technical staff in domain can be made various modifications or supplement to described specific embodiment or be replaced using similar mode
Generation, but without departing from the spiritual of the present invention or surmount scope defined in appended claims.
Claims (10)
1. a kind of degumming tech of tunny fish oil, it is characterised in that the degumming tech comprises the following steps：
Tuna crude fish oil is pre-processed；
Distilled water is added in tuna crude fish oil after the pre-treatment, stirs and adjusts to add after temperature and compound remove glycosyl enzyme
Tentatively digested, obtain tentatively digesting fish oil；
Compound protease is added in tentatively enzymolysis fish oil to be digested again, obtains digesting fish oil；
To enzymolysis fish oil heating progress destroy the enzyme treatment, room temperature is subsequently cooled to, is centrifuged, takes upper strata to float grease, is taken off to be primary
Glue fish oil；
Acid degumming agent is added in primary degumming fish oil and carries out acid degumming, it is the gold after degumming to be then centrifuged for taking supernatant
Marlin fish oil.
2. degumming tech according to claim 1, it is characterised in that the pretreatment is to be heated to tuna crude fish oil
80~100 DEG C of 3~5min of processing.
3. degumming tech according to claim 1, it is characterised in that described compound to remove glycosyl enzyme be that weight ratio is 10:(3
~7):The mixture of the exoglycosidase of (2~5), endoglycosidase and osamine enzyme.
4. the degumming tech according to claim 1 or 3, it is characterised in that the addition for removing glycosyl enzyme is tuna
The 0.3~1.5% of crude fish oil weight, the process tentatively digested be at 35~55 DEG C, ultrasonic wave added stirring enzymolysis 30~
60min。
5. degumming tech according to claim 1, it is characterised in that the compound protease is that weight ratio is 10:(5~
8):(3~6):Neutral proteinase, papain, flavor protease, the mixture of trypsase of (2~5).
6. degumming tech according to claim 1 or 5, it is characterised in that the addition of the compound protease is golden rifle
The 0.5~1.5% of fish crude fish oil weight, the process of enzymolysis is 40~75min of ultrasonic wave added stirring enzymolysis at 35~65 DEG C.
7. according to the degumming tech described in claim 1,3 or 5, it is characterised in that the preliminary mistake for digesting and digesting again
Cheng Zhongjun is added with the surfactant of tuna crude fish oil weight 0.05~0.1%.
8. degumming tech according to claim 7, it is characterised in that the surfactant is polysorbas20, polysorbate60, department
One or more in disk 20, sorbester p18.
9. degumming tech according to claim 1, it is characterised in that the acid degumming agent is that volume ratio is (2~1):
The citric acid of (1~2) and the compound of acetic acid.
10. degumming tech according to claim 1, it is characterised in that the process of the acid degumming is, by weight percentage
Than meter, the acid degumming agent of addition 0.5%~1.5% in primary degumming fish oil, 10~30min is stirred at 20~50 DEG C.
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| CN116622436A (en) * | 2023-07-25 | 2023-08-22 | 烟台海润嘉生物科技有限公司 | Production method for synchronously extracting tuna fish oil and collagen peptide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109234007A (en) * | 2018-10-16 | 2019-01-18 | 华南理工大学 | A kind of fish oil degumming discoloration method |
| CN116622436A (en) * | 2023-07-25 | 2023-08-22 | 烟台海润嘉生物科技有限公司 | Production method for synchronously extracting tuna fish oil and collagen peptide |
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Application publication date: 20180216 |