CN105296136A - Method for extracting grease in gonad of sturgeon by utilizing aqueous enzymatic method - Google Patents

Method for extracting grease in gonad of sturgeon by utilizing aqueous enzymatic method Download PDF

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Publication number
CN105296136A
CN105296136A CN201510633775.7A CN201510633775A CN105296136A CN 105296136 A CN105296136 A CN 105296136A CN 201510633775 A CN201510633775 A CN 201510633775A CN 105296136 A CN105296136 A CN 105296136A
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China
Prior art keywords
grease
sturgeon
sexual gland
enzymolysis
utilize
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CN201510633775.7A
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Chinese (zh)
Inventor
董秀萍
邵淑双
王阳
潘锦锋
祁立波
李德阳
朱蓓薇
何超琪
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Dalian Polytechnic University
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Dalian Polytechnic University
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Abstract

The invention relates to a method for extracting grease and particularly relates to a method for extracting grease in gonad of sturgeon. According to the invention, gonad of sturgeon is used as a raw material; the grease in the raw material is extracted by adopting the aqueous enzymatic method; the aqueous enzymatic method can effectively extract the grease in the gonad of the sturgeon; when the grease is obtained, enzymolysis rich in polypeptide is effectively utilized and high-value use of a byproduct generated in the sturgeon machining process is implemented.

Description

A kind of method utilizing aqueous enzymatic extraction sturgeon sexual gland grease
Technical field
The present invention relates to a kind of method extracting grease, more particularly, relate to a kind of method extracting sturgeon sexual gland grease.
Background technology
Sturgeon is one of fingerling the most original and the most ancient on the earth, is also the fish of individual maximum, longest-lived in freshwater fish, have the title of " in water living fossil ".Sturgeon the whole body is precious, and caviare is the target product of sturgeon processing, and sturgeon sexual gland is not well studied as sturgeon processing " by product " and effectively utilizes.Sturgeon sexual gland accounts for fish body proportion about 2% (spermary is except lipid layer, ovary are except after ovum), is rich in grease, has bibliographical information sturgeon spermary fat content more than 70%.Therefore, in sturgeon industry development, how effectively to extract and then effectively to utilize grease to be the key issue that sturgeon sexual gland is applied.
Traditional fish oil extracting method has milling process, cooking process, solvent method etc., but in leaching process, there is distinct disadvantage, and such as the large production efficiency of milling process labour intensity is low; Cooking process effectively can not be separated the fat with protein bound, therefore extraction yield is relatively low, and affects oil quality because Extracting temperature is higher; Solvent method is because of with an organic solvent therefore security is poor.Aqueous enzymatic method is a kind of biotechnology of novelty, on the basis of physical disturbance material, first add water again enzyme-added, utilizing the decomposition katalysis of enzyme uniqueness fully to destroy material cellularstructure makes grease be easy to disengage from oil plant solid, utilize non-oil component (protein and carbohydrate) to oil and the difference of water avidity and the difference of profit proportion by oil and non-oil component separating, while can obtain the albumen of high-quality.Aqueous enzymatic method technical qualification are gentle, and extraction efficiency is high, green safety, and in system, degraded product generally can not react with extract, are conducive to protecting grease, albumen etc. can utilize the quality of composition, thus can improve fish oil quality and improve prepared using value.But not all glyceride stock is all suitable for adopting aqueous enzymatic method to carry out the extraction of grease, effective extracting method needs to carry out initial option according to raw material own characteristic, then carries out that corresponding experiment sieving could set up.
Well-known grease in storage because can oxidative rancidity be there is in the factor impacts such as light, oxygen, high temperature.The grease become sour not only nutritive value reduces, and often produces healthy harmful material in process of spoilage, as superoxide and free radical.In fact, unfavorable extracting method also can cause the deterioration of oil quality.Chinese Fishery fish oil industry standard SC/T3502-2000 specifies refined fish oil acid value≤2mg/g, crude fish oil acid value≤15mg/g (acid value is an important indicator of measure oil free fatty acid total amount, is one of leading indicator judging degree spoiled by rancid oil or fat).Therefore, in the performance history of oil and fat product, set up suitable extracting method for material characteristic most important.In addition, how by setting up rational extractive technique, ensure the extraction yield of the functional components such as ω-3 type unsaturated fatty acids timnodonic acid (EPA) and docosahexenoic acid (DHA) in prepared grease and activity also most important.The functional components such as EPA, DHA have special physiological action to human body, its distinctive biological activity can some disease of prevention and corntrol effectively, as hypertension, heart trouble, cancer and diabetes etc., therefore, these functional components are also usually by the important indicator be worth as evaluation grease.
This patent utilizes sturgeon sexual gland as raw material, adopts grease in the aqueous enzymatic method high efficiency extraction raw material of environmental protection, and then effectively utilizes, and obtains the enzymolysis solution being rich in polypeptide, achieve the gonadal high-valued comprehensive utilization of sturgeon while obtaining grease.
Summary of the invention
The object of the invention is to provide the aqueous enzymatic method preparation method of the sturgeon sexual gland grease that a kind of pretreatment process is simple, extraction efficiency is high, oil quality is good, adopt safe and reliable aqueous enzymatic method, coordinate simple raw materials pretreatment process, obtain the grease that quality is good, and utilize enzymolysis solution micro encapsulation to obtain polypeptide products, while realizing the higher value application of raw oil material, realize effective utilization of enzymolysis solution, really realize gonadal comprehensive utilization.
The invention provides a kind of method utilizing aqueous enzymatic extraction sturgeon sexual gland grease for achieving the above object, it is characterized in that, comprise the steps:
S1, raw materials pretreatment: get sturgeon sexual gland and rub, 0-4 DEG C of standing 10-30min, after layering, collect fluid layer layer solid with material respectively.
S2, enzymolysis: in the fluid layer obtained respectively to step S1 and the solid layer of material, 1:2 adds water in mass ratio; Then, add proteolytic enzyme respectively by the enzyme concentration of 3000U/g, enzymolysis 2-4h, control temperature is 40-50 DEG C, pH is 2.0-8.0; In reaction process, per half an hour regulates pH with about maintaining pH and being stabilized in the optimal pH of corresponding proteolytic enzyme with pH meter.
Under optimal way, described proteolytic enzyme is trypsinase, stomach en-, papoid or neutral protease or their combination.
Under optimal way, described utilize concentration to be 0.1mol/L HCl solution or NaOH solution adjust ph.
After S3, enzyme digestion reaction terminate, boiling water bath goes out enzyme 10-30min; Centrifugation, obtains grease and the enzymolysis solution containing polypeptide.Wherein, the solid layer upper strata after enzyme digestion reaction is centrifugal of fluid layer, material is grease, and lower floor is the enzymolysis solution containing polypeptide; Fluid layer is grease obtained more, and in the solid layer of material, enzymolysis solution is more.
Under optimal way, the condition of described centrifugation is centrifugal 10-25min under centrifugal force 3000-5000 × g.
Under optimal way, present invention also offers a kind of by the method for grease described in step S3 and described enzymolysis solution micro encapsulation, it is characterized in that, making step is as follows:
In grease obtained and enzymolysis solution, add carrageenin, gum arabic or maltodextrin respectively, addition is homogeneous under 20-35wt%, 40-50MPa pressure, carry out spraying dry (inlet temperature 180 DEG C-200 DEG C) powdery oil and powder polypeptide.
Quality evaluation: the grease obtained by the inventive method, color and luster presents pure transparent yellow, there is slight fishy smell, two portions acid value of lipids is all less than 2mg/g after measured, oil quality is good, the total amount of ω-3 type unsaturated fatty acids EPA and DHA close to 10%, based on sturgeon sexual gland fat content higher (gamogenesis gland fat content reaches 41.97%, 75.22% respectively), can as the good source of EPA and DHA.
3, the effect of this patent:
(1) this patent adopts aqueous enzymatic method high efficiency extraction sturgeon sexual gland grease, realizes the gonadal effective utilization of sturgeon processing " by product " sturgeon;
(2) utilize aqueous enzymatic method to obtain the second best in quality sturgeon sexual gland grease, utilize enzymolysis solution to prepare polypeptide products simultaneously, realize the comprehensive utilization of raw material.
Embodiment
The invention provides a kind of method utilizing aqueous enzymatic extraction sturgeon sexual gland grease for achieving the above object, it is characterized in that, comprise the steps:
S1, raw materials pretreatment: get that sturgeon sexual gland thaws naturally, stripping and slicing, rubbing be placed in corresponding container (centrifuge tube, beaker etc.), static 10-30min in mixture of ice and water, after rubbing after raw material layering, by separated for subsequent use for solid to fluid layer and material layer.
S2, enzymolysis
Above-mentioned fluid layer A and the solid layer B of material are weighed respectively, adds deionized water respectively by solid-liquid ratio w:w=1:2; Proteolytic enzyme (trypsinase, stomach en-, papoid or neutral protease) is added respectively by the enzyme concentration of 3000U/g, regulate temperature 40-50 DEG C, with concentration be 0.1MHCl/NaOH regulate pH2.0-8.0, reaction times 2-4h, in reaction process, per half an hour regulates a pH;
After enzyme digestion reaction terminates, boiling water bath goes out enzyme 10-30min, centrifugal 10-25min under centrifugal force 3000-5000 × g;
The solid layer B upper strata after enzyme digestion reaction is centrifugal of fluid layer A, material is grease, and lower floor is the enzymolysis solution containing polypeptide, and wherein, A is grease obtained more, and in B, enzymolysis solution is more.
S3, quality evaluation
Two portions acid value of lipids is all less than 2mg/g after measured, EPA and DHA accounts for lipid acid proportion total amount close to 10%.
S4, enzymolysis solution micro encapsulation
Carrageenin, gum arabic, maltodextrin (addition 20-35wt%) is added respectively in grease obtained and enzymolysis solution, homogeneous under 40-50MPa pressure, carries out spraying dry (inlet temperature 180 DEG C-200 DEG C) and obtains powdery oil and powder polypeptide.
Embodiment 1
S1, raw materials pretreatment
Get sturgeon Male reproduction (sturgeon spermary) naturally to thaw, stripping and slicing, rub; Take 40g and rub rear sample static 20min in 0-4 DEG C of mixture of ice and water, after layering, solid to fluid layer and material layer is filtered separated for subsequent use,
S2, enzymolysis
Above-mentioned fluid layer A and the solid layer B of material are weighed respectively, mixes after adding deionized water respectively by solid-liquid ratio w:w=1:2; With concentration be 0.1MHCl/NaOH regulate pH be 7.0, add neutral protease respectively by the enzyme concentration of 3000U/g, regulating thermostatic shaking water bath pot temperature of reaction 50 DEG C, enzyme digestion reaction time 4h, in reaction process, per half an hour regulates a pH, makes it maintain 7.0;
After enzyme digestion reaction terminates, boiling water bath goes out enzyme 10min, centrifugal 10min under centrifugal force 3000 × g;
The solid layer B upper strata after enzyme digestion reaction is centrifugal of fluid layer A, material is grease, and lower floor is the enzymolysis solution containing polypeptide, and wherein, A is grease obtained more, and in B, enzymolysis solution is more.Separate upper strata grease and enzymolysis solution.
S3, quality evaluation
A, B two portions acid value of lipids is respectively 0.63mg/g, 0.65mg/g after measured, EPA and DHA accounts for total fatty acids proportion altogether and be respectively 9.98%, 9.80%.
The micro encapsulation of S4, grease and enzymolysis solution
In the grease and enzymolysis solution of gained A, part B, add 20wt% maltodextrin, homogeneous under 40-50MPa pressure, carry out spraying dry (inlet temperature 180 DEG C-200 DEG C) and obtain powdery oil and powder polypeptide.
The grease obtained acid value of this method is low, and oil quality is good, and comparatively it is large that EPA and DHA accounts for total fatty acids proportion, is beneficial to the functional application of raw material.
Embodiment 2
S1, raw materials pretreatment
Get sturgeon female gonad (sturgeon ovary, remove ovum) naturally to thaw, stripping and slicing, rub; Take 40g and rub rear sample static 20min in 0-4 DEG C of mixture of ice and water, after layering, solid to fluid layer and material layer is filtered separated for subsequent use,
S2, enzymolysis
Above-mentioned fluid layer A and the solid layer B of material are weighed respectively, mixes after adding deionized water respectively by solid-liquid ratio w:w=1:2; With concentration be 0.1MHCl/NaOH regulate pH be 7.0, add neutral protease respectively by the enzyme concentration of 3000U/g, regulating thermostatic shaking water bath pot temperature of reaction 50 DEG C, enzyme digestion reaction time 4h, in reaction process, per half an hour regulates a pH, makes it maintain 7.0;
After enzyme digestion reaction terminates, boiling water bath goes out enzyme 10min, centrifugal 10min under centrifugal force 3000 × g;
The solid layer B upper strata after enzyme digestion reaction is centrifugal of fluid layer A, material is grease, and lower floor is the enzymolysis solution containing polypeptide, and wherein, A is grease obtained more, and in B, enzymolysis solution is more.Separate upper strata grease and enzymolysis solution.
S3, quality evaluation
A, B two portions acid value of lipids is respectively 1.04mg/g, 0.91mg/g after measured, EPA and DHA accounts for total fatty acids proportion altogether and be respectively 7.22%, 7.80%.
The micro encapsulation of S4, grease and enzymolysis solution
In the grease and enzymolysis solution of gained A, part B, add 20wt% maltodextrin, homogeneous under 40-50MPa pressure, carry out spraying dry (inlet temperature 180 DEG C-200 DEG C) and obtain powdery oil and powder polypeptide.
The grease obtained acid value of this method is lower, and oil quality is better.
Embodiment 3
Concrete steps are identical with embodiment 1, remove " take 40g and rub rear sample static 20min in 0-4 DEG C of mixture of ice and water, filter separated for subsequent use after layering by solid to fluid layer and material layer " step from, rub raw material entirety and carry out enzymolysis.
Acid value is that lipid acid proportion shared by 1.75mg/g, EPA and DHA and embodiment 1 are without significant difference after measured.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.

Claims (6)

1. utilize a method for aqueous enzymatic extraction sturgeon sexual gland grease, it is characterized in that, comprise the steps:
S1, raw materials pretreatment: get sturgeon sexual gland and rub, 0-4 DEG C of standing 10-30min, after layering, collect fluid layer layer solid with material respectively;
S2, enzymolysis: in the fluid layer obtained respectively to step S1 and the solid layer of material, 1:2 adds water in mass ratio; Then, add proteolytic enzyme respectively by the enzyme concentration of 3000U/g, enzymolysis 2-4h, control temperature is 40-50 DEG C, pH is 2.0-8.0;
After S3, enzyme digestion reaction terminate, boiling water bath goes out enzyme 10-30min; Centrifugation, obtains grease and enzymolysis solution.
2. utilize the method for aqueous enzymatic extraction sturgeon sexual gland grease according to claim 1, it is characterized in that,
Described step S1 rubs for getting sturgeon sexual gland, obtains sturgeon sexual gland mixed solution;
Described step S2 adds water in the sturgeon sexual gland mixed solution that 1:2 obtains to step S1 in mass ratio; Then add proteolytic enzyme by the enzyme concentration of 3000U/g, enzymolysis 2-4h, control temperature is 40-50 DEG C, pH is 2.0-8.0.
3. according to claim 1 or 2, utilize the method for aqueous enzymatic extraction sturgeon sexual gland grease, it is characterized in that, described proteolytic enzyme is trypsinase, stomach en-, papoid or neutral protease.
4. according to claim 1 or 2, utilize the method for aqueous enzymatic extraction sturgeon sexual gland grease, it is characterized in that, described utilize concentration to be 0.1mol/L HCl solution or 0.1mol/L NaOH solution regulate pH.
5. according to claim 1 or 2, utilize the method for aqueous enzymatic extraction sturgeon sexual gland grease, it is characterized in that, the condition of centrifugation described in step S3 is centrifugal 10-25min under centrifugal force 3000-5000 × g.
6. a method for grease and enzymolysis solution micro encapsulation, is characterized in that, making step is as follows:
In the grease and enzymolysis solution of step S3 gained, add carrageenin, gum arabic or maltodextrin respectively, addition is 20-35wt%; Homogeneous under 40-50MPa pressure, spraying dry, obtains powdery oil and powder polypeptide.
CN201510633775.7A 2015-09-30 2015-09-30 Method for extracting grease in gonad of sturgeon by utilizing aqueous enzymatic method Pending CN105296136A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108265097A (en) * 2018-03-07 2018-07-10 天津国际生物医药联合研究院 A kind of extracting method of sturgeon egg protein peptide and application
CN115074408A (en) * 2022-08-03 2022-09-20 湖北省农业科学院农产品加工与核农技术研究所 Preparation method of aquatic product polysaccharide peptide

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CN102260585A (en) * 2011-06-28 2011-11-30 泰祥集团技术开发有限公司 Method for extracting fish oil from squid viscera by using animal proteolytic enzyme
CN103773590A (en) * 2014-01-23 2014-05-07 吉首大学 Method for extracting fish oil from internal organs of elopichthys bambusa by utilizing neutral protease

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108265097A (en) * 2018-03-07 2018-07-10 天津国际生物医药联合研究院 A kind of extracting method of sturgeon egg protein peptide and application
CN115074408A (en) * 2022-08-03 2022-09-20 湖北省农业科学院农产品加工与核农技术研究所 Preparation method of aquatic product polysaccharide peptide

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