CN105994932B - A kind of fat-soluble walnut peptide and preparation method thereof - Google Patents
A kind of fat-soluble walnut peptide and preparation method thereof Download PDFInfo
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- CN105994932B CN105994932B CN201610339161.2A CN201610339161A CN105994932B CN 105994932 B CN105994932 B CN 105994932B CN 201610339161 A CN201610339161 A CN 201610339161A CN 105994932 B CN105994932 B CN 105994932B
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
- A23J3/00—Working-up of proteins for foodstuffs
- A23J3/14—Vegetable proteins
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
- A23J3/00—Working-up of proteins for foodstuffs
- A23J3/30—Working-up of proteins for foodstuffs by hydrolysis
- A23J3/32—Working-up of proteins for foodstuffs by hydrolysis using chemical agents
- A23J3/34—Working-up of proteins for foodstuffs by hydrolysis using chemical agents using enzymes
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
- A23J3/00—Working-up of proteins for foodstuffs
- A23J3/30—Working-up of proteins for foodstuffs by hydrolysis
- A23J3/32—Working-up of proteins for foodstuffs by hydrolysis using chemical agents
- A23J3/34—Working-up of proteins for foodstuffs by hydrolysis using chemical agents using enzymes
- A23J3/346—Working-up of proteins for foodstuffs by hydrolysis using chemical agents using enzymes of vegetable proteins
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Abstract
The present invention relates to a kind of fat-soluble walnut peptides and preparation method thereof, prepared method is successively the following steps are included: walnut dregs clean impurity elimination, protease gradient digests, filter, fat-soluble wall material is embedded, is centrifugated, it is dry, obtain fat-soluble walnut peptide.Avoid the sodium cellulose glycolate used in the prior art reduces the intake of people's sodium ion, keeps product more healthy as wall material, and the quality of walnut peptide is greatly improved.
Description
Technical field
The invention belongs to polypeptide preparation and deep process technology fields, and in particular to a kind of preparation side of fat-soluble walnut peptide
Method.
Background technique
Walnut, also known as English walnut, Qiang peach are one of world-renowned four big dry fruits.The medical value and nutritive value of walnut
It is all very high, containing a large amount of protein, unsaturated fatty acid and vitamin, minerals etc., be a kind of pair of human body have benefiting qi and nourishing blood,
Invigorate the kidney and stop nocturnal emission, warm lung goes cough, the excellent peaberry food of blacking hair and strengthening brain, the good merchantable brand that lengthens one's life is considered as by physician and health.Walnut
The nutrition very abundant of benevolence, every 100 grams of walnut kernel contain high-quality fat 63.7g, protein 14.6g, carbohydrate 10.3g, phosphorus
280mg, calcium 85mg, iron 2.6mg, potassium 3.0mg, vitamin A 0.036mg, vitamin B10.26mg, vitamin B20.15mg, niacin
1.0mg, niacin 1.0mg additionally contain the nutriments such as the minerals and vitamins K such as manganese, chromium, and lecithin rich in
Rouge, amino acid and unsaturated fatty acid, it is cholesterol-free.Walnut protein is mainly made of four proteinoid, i.e. albumin, ball egg
White, alcohol soluble protein and glutelin account for 6.81%, 17.57%, 5.33% and the 70.11% of walnut protein total amount, after degreasing respectively
Walnut dregs in protein content up to 60% or more, containing the 18 kind amino acid beneficial to human body, and 8 kinds of ammonia needed by human
Base acid content is reasonable, and wherein arginine, glutamic acid, histidine and tyrosine content are higher, has high value of exploiting and utilizing.
The unsaturated fatty acid contents such as oleic acid, linoleic acid, linolenic acid and arachidonic acid in walnut kernel grease are up to 90%,
Other greases cannot compare, therefore walnut kernel in the market is mainly processed into walnut oil, and byproduct walnut slag does not have
There is further processing to utilize；Using biological enzymolysis technology, walnut slag is developed into walnut peptide, it is possible to reduce the waste of resource mentions
The added value of high walnut product.
It is especially more to the document of polypeptide functional activity research in recent years, studies at home and abroad show that, walnut protein passes through biology
The walnut peptide of enzyme enzymatic hydrolysis preparation has anti-oxidant, raising immunity, antifatigue, blood pressure lowering and improvement learning memory and other effects,
And polypeptide and grease combine the function that its blood pressure lowering can be enhanced and improve learning memory, but insoluble due to polypeptide and grease
Limit its application in functional food.
It is taught application No. is 201310485124.9,200810236514.1 and 201310655750.8 and prepares walnut
The technique of peptide has been all made of the mode that various protease participate in enzymolysis process together, but has differed greatly between various protease,
It can be interfered between each other with interreaction, enzymolysis process is unsatisfactory, to influence the quality of walnut peptide.
Application No. is 201310655750.8 patents to describe a kind of technology by walnut peptide microencapsulation, uses carboxylic first
As auxiliary material by walnut peptide microencapsulation, the sodium carboxymethylcellulose used is more, increases for base sodium cellulosate and beta-cyclodextrin
The sodium ion of product, so obtained walnut peptide micro-capsule is unfavorable for taking for hypertensive patient.
Lecithin belongs to a kind of mixture, is one group of filemot grease being present among animal vegetable tissue and yolk
Property substance, constituent includes phosphoric acid, choline, fatty acid, glycerol, glycolipid, triglyceride and phosphatide, and lecithin is main
Ingredient is pure phosphatidyl choline, is a kind of ionic surfactant containing amphiphilic group, and hydrophobic end is grease, the phosphorus of long-chain
Rouge, fatty acid, glycerol, glycolipid, triglyceride etc., water-wet side are the moieties of choline, and choline is (β-hydroxyl second in chemistry
Base) hydroxide of trimethyl ammonia has very strong hygroscopicity, is exposed in air in the white slurries of water solubility of colourless bitter
It can absorb water quickly.
Magnesium stearate is also known as magnesium octadecanate, is white easily without grittiness fine powder, has soapy feeling, large specific surface area has pole
Strong suction-operated and hygroscopicity.As a kind of fatty acid salt form anionic surfactant, emulsifier can be increased in oily phase
In dissolubility, improve embedding rate and micro-capsule stability.
Polyglyceryl fatty acid ester is a kind of novel, efficient nonionic surfactant.It is by natural glycerin and rouge
Made of fat acid is esterified at high temperature, since polyglyceryl fatty acid ester has more hydroxyls, emulsifiability is sweeter than fatty acid list
Ester is superior more, in the metabolic process, can be analyzed to sweet oil & fat, to be absorbed by the body or excrete, has height
Safety.Its maximum feature is quite stable in alkalinity, neutral, acidic environment.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for preparing and extracting walnut peptide, using a kind of novel Water-In-Oil technique
Embedding microencapsulation is carried out to walnut peptide, obtains the walnut peptide with fat-soluble characteristic, mixture can be prepared with grease type by reaching
Purpose.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
Step 1: after taking walnut dregs to mix with 10 times of water (w/v), at 110 DEG C, handling 30 minutes, go under the conditions of 120KPa
It is primary to add water mixing, washing for clear liquid；
Step 2: the walnut dregs for taking step 1 to obtain add water to 1 ﹕ 15 (w/v) of solid-liquid ratio, and calcium hydroxide adjusts pH value 9.0,
55 DEG C are warming up to, alkali protease is added and digests 0.5 hour, papain is added and continues enzymatic hydrolysis 3.5 hours, be eventually adding flavor
Enzyme continues enzymatic hydrolysis 0.5 hour, enzyme deactivation, filtering, collects filtrate and obtains walnut peptidase hydrolyzed liquor；
Step 3: being concentrated by double-effect concentration evaporator, be concentrated into the concentrate of Baume degrees 12；
Step 4: being placed in acetone and alcohol mixeding liquid according to 1 ﹕ 5 (w/v) by wall material is embedded, being heated to 40 DEG C keeps its molten
Solution, stirs and is slowly added to 20-40% (v/v) walnut peptide concentrate, colloid mill homogeneous 3-5h is immediately evaporated mixed liquor
Recycling design, gained sediment are freeze-dried, and walnut peptide micro-capsule is obtained.
As a preferred embodiment, the dosage of the alkali protease of enzymatic hydrolysis described in step 2 is the 2% of walnut dregs quality, wood
Melon enzyme dosage is the 1% of walnut dregs quality, flavor enzyme dosage is walnut dregs quality 1%.
As a preferred embodiment, thickening temperature described in step 3 is 75 DEG C, vacuum degree 0.065mPa.
As a preferred embodiment, embedding wall material described in step 4 is 1 ﹕ 1 (w/w/w) of mass ratio 1-2 ﹕ lecithin, hard
The in the mixed solvent acetone and ethyl alcohol volume ratio of fatty acid magnesium and polyglyceryl fatty acid ester, the acetone and ethyl alcohol are 1 ﹕ 3 (v/v).
As another preferred embodiment, the temperature of evaporation recycling design is 40-50 DEG C described in step 4, and vacuum degree is
0.065mpa。
The utility model has the advantages that
1. the present invention is strong using the small molecule walnut peptide hydrophily of the preparation of gradient enzyme solution, it is easier to the embedding of wall material
Fat-soluble walnut peptide is prepared, shows to emulsify in different pH value (3-10) oil-phase solutions carrying out experiment in vitro
Effect, and walnut peptide is substantially all package and does not generate layering in the oil, and stability is good；
2. the embedding wall material that the present invention uses avoids existing skill for embedded materials such as lecithin, polyglyceryl fatty acid esters
The sodium cellulose glycolate used in art reduces the intake of people's sodium ion, keeps product more healthy.
Specific embodiment
Form remakes a kind of fat-soluble walnut peptide of the present invention and preparation method thereof further detailed by the following examples
It describes in detail bright, but this should not be interpreted as to the scope of the above subject matter of the present invention is limited to the following embodiments, it is all based in the present invention
The technology that content is realized is stated to all belong to the scope of protection of the present invention.
The preparation of the fat-soluble walnut peptide of embodiment 1
Walnut dregs are weighed, after adding 10 times of water (w/v) to be mixed, at 110 DEG C, handles 30 minutes, goes under the conditions of 120KPa
Supernatant adds water stirring washing once, and moisturizing to 1 ﹕ 15 (w/v) of solid-liquid ratio, calcium hydroxide adjusts PH9.0, is warming up to 55 DEG C,
The alkali protease that walnut dregs quality 2% is added digests 0.5 hour, and the papain for adding walnut dregs quality 1% continues to digest
It 3.5 hours, is eventually adding 1% food flavor enzyme of walnut dregs quality and continues enzymatic hydrolysis 0.5 hour, be warming up to 100 DEG C of enzyme deactivations 10 minutes, mistake
Filter, collection filtered fluid are placed in double-effect concentration evaporator and are concentrated under the conditions of 75 DEG C, vacuum degree 0.065mPa, are concentrated into Baume
The concentrate of degree 12 is placed in wall material is embedded in acetone and ethyl alcohol (1 ﹕ 3) (v/v) mixed liquor according to 1 ﹕ 5 (w/v), embeds wall material
For lecithin, magnesium stearate and the polyglyceryl fatty acid ester of 1 ﹕ of mass ratio, 1 ﹕ 1 (w/w/w), 40 DEG C of dissolutions are heated to, stirs and delays
It is slow that 20% (v/v) walnut peptide concentrate, colloid mill homogeneous 3h, to mixed liquor under the conditions of 50 DEG C, vacuum degree 0.065mPa is added
It is evaporated recycling design, gained sediment is freeze-dried, and finished product is made, protein content 51.6%, polypeptide in finished product
Content 45.7%.
The preparation of the fat-soluble walnut peptide of embodiment 2
Walnut dregs are weighed, after adding 10 times of water (w/v) to be mixed, at 110 DEG C, handles 30 minutes, goes under the conditions of 120KPa
Supernatant adds water stirring washing once, and moisturizing to 1 ﹕ 15 (w/v) of solid-liquid ratio, calcium hydroxide adjusts PH9.0, is warming up to 55 DEG C,
The alkali protease that walnut dregs quality 2% is added digests 0.5 hour, and the papain for adding walnut dregs quality 1% continues to digest
It 3.5 hours, is eventually adding 1% food flavor enzyme of walnut dregs quality and continues enzymatic hydrolysis 0.5 hour, be warming up to 100 DEG C of enzyme deactivations 10 minutes, mistake
Filter, collection filtered fluid are placed in double-effect concentration evaporator and are concentrated under the conditions of 75 DEG C, vacuum degree 0.065mPa, are concentrated into Baume
The concentrate of degree 12 is placed in wall material is embedded in acetone and ethyl alcohol (1 ﹕ 3) (v/v) mixed liquor according to 1 ﹕ 5 (w/v), embeds wall material
For lecithin, magnesium stearate and the polyglyceryl fatty acid ester of 1.5 ﹕ of mass ratio, 1 ﹕ 1 (w/w/w), 40 DEG C of dissolutions are heated to, stirring is simultaneously
It is slowly added to 30% (v/v) walnut peptide concentrate, colloid mill homogeneous 4h；To mixing under the conditions of 40 DEG C, vacuum degree 0.065mPa
Liquid is evaporated recycling design, and gained sediment is freeze-dried, and finished product is made, protein content 58.2%, more in finished product
Peptide content 49.6%.
The preparation of the fat-soluble walnut peptide of embodiment 3
Walnut dregs are weighed, after adding 10 times of water (w/v) to be mixed, at 110 DEG C, handles 30 minutes, goes under the conditions of 120KPa
Supernatant adds water stirring washing once, and moisturizing to 1 ﹕ 15 (w/v) of solid-liquid ratio, calcium hydroxide adjusts PH9.0, is warming up to 55 DEG C,
The alkali protease that walnut dregs quality 2% is added digests 0.5 hour, and the papain for adding walnut dregs quality 1% continues to digest
It 3.5 hours, is eventually adding 1% food flavor enzyme of walnut dregs quality and continues enzymatic hydrolysis 0.5 hour, be warming up to 100 DEG C of enzyme deactivations 10 minutes, mistake
Filter, collection filtered fluid are placed in double-effect concentration evaporator and are concentrated under the conditions of 75 DEG C, vacuum degree 0.065mPa, are concentrated into Baume
The concentrate of degree 12；It is placed in acetone and ethyl alcohol (1 ﹕ 3) (v/v) mixed liquor according to 1 ﹕ 5 (w/v) by wall material is embedded, embeds wall material
For lecithin, magnesium stearate and the polyglyceryl fatty acid ester of 2 ﹕ of mass ratio, 1 ﹕ 1 (w/w/w), 40 DEG C of dissolutions are heated to, stirs and delays
It is slow that 40% (v/v) walnut peptide concentrate, colloid mill homogeneous 5h is added；To mixed liquor under the conditions of 40 DEG C, vacuum degree 0.065mPa
It is evaporated recycling design, gained sediment is freeze-dried, and finished product is made, protein content 65.2%, polypeptide in finished product
Content 54.1%.
The toxicity test of the fat-soluble walnut peptide of embodiment 4 is studied
Example 1, embodiment 2, the fat-soluble walnut peptide micro-capsule of embodiment 3, according to " health food is examined and assessment technique
Specification ", using kunming mice as experimental animal, half male and half female is tested using maximum stomach-filling amount method (MTD), and dose design is
10.0g/kg.bw, interior stomach-filling 3 times for 24 hours；It is observed continuously two weeks, three embodiment group mouse are without death, hair color gloss, weight
Increased, does not have significant difference with blank control group ratio.Consolidate the fat-soluble walnut peptide micro-capsule of invention belong to it is practical nontoxic
Substance.
Claims (1)
1. a kind of preparation method of fat-soluble walnut peptide, which is characterized in that it is prepared by following steps:
Step 1: it takes walnut dregs to mix with water according to mass volume ratio 1:10, at 110 DEG C, is handled 30 minutes under the conditions of 120KPa,
Supernatant is removed, it is primary to add water mixing, washing；
Step 2: the walnut dregs for taking step 1 to obtain add water to mass volume ratio 1:15, and calcium hydroxide adjusts pH value 9.0, is warming up to
55 DEG C, alkali protease is added and digests 0.5 hour, add papain and continue enzymatic hydrolysis 3.5 hours, is eventually adding food flavor enzyme continuation
Enzymatic hydrolysis 0.5 hour, enzyme deactivation, filtering collect filtrate and obtain walnut peptidase hydrolyzed liquor；
Wherein, the dosage of enzymatic hydrolysis alkali protease is the 2% of walnut dregs quality, and the pawpaw enzyme dosage is walnut dregs matter
The 1% of amount, the flavor enzyme dosage are the 1% of walnut dregs quality；
Step 3: being concentrated by double-effect concentration evaporator, be concentrated into the concentrate of Baume degrees 12；
The temperature of the concentration is 75 DEG C, and the vacuum degree of the concentration is 0.065mPa；
Step 4: being placed in acetone and alcohol mixeding liquid according to 1 ﹕ 5 of mass volume ratio by wall material is embedded, being heated to 40 DEG C keeps its molten
Solution, stirs and is slowly added to concentration expressed in percentage by volume 20-40% walnut peptide concentrate, colloid mill homogeneous 3-5h, immediately to mixed liquor
It is evaporated recycling design, gained sediment is freeze-dried, and walnut peptide micro-capsule is obtained；
Lecithin, magnesium stearate and the polyglyceryl fatty acid ester that the embedding wall material mass ratio is 1 ﹕ 1 of 1-2 ﹕, the acetone and second
The in the mixed solvent acetone and ethyl alcohol volume ratio of alcohol are 1 ﹕ 3；
The temperature of the evaporation recycling design is 40-50 DEG C, and the vacuum degree of the evaporation recycling design is 0.065mpa.
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| CN107874259A (en) * | 2017-12-28 | 2018-04-06 | 武汉天天好生物制品有限公司 | More oligopeptide mixtures of acer truncatum seed oil and preparation method thereof |
| CN109122877A (en) * | 2018-08-10 | 2019-01-04 | 河北养元智汇饮品股份有限公司 | A kind of walnut polypeptide cream and preparation method thereof |
| CN110643661A (en) * | 2019-09-12 | 2020-01-03 | 浙江李子园食品股份有限公司 | Method for rapidly separating and purifying walnut protein from walnuts |
| CN111518858B (en) * | 2020-05-14 | 2022-10-11 | 武汉天天好生物制品有限公司 | Vegetable protein peptide and preparation method thereof |
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| CN103652314A (en) * | 2013-12-06 | 2014-03-26 | 陈栋梁 | Microencapsulated walnut peptide and preparation method thereof |
| CN104293870A (en) * | 2014-09-25 | 2015-01-21 | 汾州裕源土特产品有限公司 | Preparation method of antioxidant walnut polypeptide health product |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103652314A (en) * | 2013-12-06 | 2014-03-26 | 陈栋梁 | Microencapsulated walnut peptide and preparation method thereof |
| CN104293870A (en) * | 2014-09-25 | 2015-01-21 | 汾州裕源土特产品有限公司 | Preparation method of antioxidant walnut polypeptide health product |
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