CN112913962A - Preparation method of protein powder - Google Patents
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- CN112913962A CN112913962A CN202110122237.7A CN202110122237A CN112913962A CN 112913962 A CN112913962 A CN 112913962A CN 202110122237 A CN202110122237 A CN 202110122237A CN 112913962 A CN112913962 A CN 112913962A
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Images
Classifications
-
- 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
- A23J1/00—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
- A23J1/20—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from milk, e.g. casein; from whey
- A23J1/205—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from milk, e.g. casein; from whey from whey, e.g. lactalbumine
-
- 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
- A23J3/04—Animal proteins
- A23J3/08—Dairy proteins
-
- 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
- A23J3/341—Working-up of proteins for foodstuffs by hydrolysis using chemical agents using enzymes of animal proteins
- A23J3/343—Working-up of proteins for foodstuffs by hydrolysis using chemical agents using enzymes of animal proteins of dairy proteins
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Zoology (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Dairy Products (AREA)
Abstract
The invention discloses a preparation method of protein powder, which comprises the steps of firstly obtaining skim milk, removing fat, then carrying out centrifugal separation for the first time, separating out partial other high-abundance protein, further using high-speed centrifugal separation to obtain a whey protein solution, then purifying the whey protein, further using the whey protein solution to be mixed with precooled acetone with four times of volume, stirring to obtain a precipitate, wherein the precipitate is whey protein, then hydrolyzing the whey protein, redissolving the precipitate by using urea, adding trypsin to hydrolyze the whey protein at 37 ℃, carrying out high-speed centrifugal separation to collect supernatant after full reaction, and finally desalting the supernatant, carrying out vacuum centrifugal drying and then obtaining the protein powder which is easy to digest by human bodies and has high purity.
Description
Technical Field
The invention relates to the field of protein powder, and in particular relates to a preparation method of protein powder.
Background
Protein is an important component for composing all cells and tissues of human body. All important components of the body require the involvement of proteins. Generally, proteins account for about 18% of the total mass of the human body, and most importantly, are related to life phenomena.
Proteins (proteins) are the material basis of life, are organic macromolecules, are basic organic substances constituting cells, and are the main players of life activities. Without proteins, no life is present. Amino acids are the basic building blocks of proteins. It is a substance that is closely related to life and to various forms of life activities. Proteins are involved in every cell and all important components of the body. The protein accounts for 16-20% of the weight of the human body, namely, about 9.6-12 kg of the protein is contained in a 60kg adult. The human body protein has many kinds, different properties and functions, but is composed of 20 kinds of amino acids (amino acids) in different proportions, and is constantly metabolized and renewed in vivo.
First, the nutritional value of whey protein is the highest among various proteins. In general, proteins having complete types and contents of essential amino acids and providing human needs can be called high-quality proteins, also called complete proteins. Here, the concept of essential amino acids is mentioned, and essential amino acids refer to amino acids which are necessary for the human body but cannot be synthesized by itself and must be taken from food. Among the plant proteins, only soybean protein is a complete protein, and soybean protein lacks methionine and needs to be complementary to cereals, and soybean protein is not superior to animal protein of good quality in absorption. The whey protein belongs to high-quality complete protein and is also animal protein. It contains 8 kinds of amino acids essential for human body, and has reasonable proportion and human body requirement ratio, and is essential matter for human body growth, development, senility resisting and other life activities.
Secondly, whey protein is easier to digest and absorb, and the milk contains 60% of whey protein and 40% of casein, so that the feces of the infants who drink the breast milk are softer and less in amount. In addition, whey is rich in cysteine and methionine, which maintain antioxidant levels in humans. Many experimental studies have also demonstrated that administration of whey protein concentrates can promote humoral and cellular immunity, stimulate the immune system of the human body, and prevent the development of chemically induced cancers. Therefore, the whey protein is a very good protein for enhancing immunity.
Thirdly, whey protein is low in fat and lactose, but it contains beta-lactoglobulin, alpha-lactalbumin, immunoglobulin, and other active ingredients. It is these active ingredients that provide whey protein with many health benefits to the human body and therefore it is considered to be one of the high quality protein sources required by the human body.
The existing whey protein powder is prepared by generally sterilizing, separating whey, purifying at low temperature and drying and dehydrating, and at present, no comprehensive utilization technology of whey protein with independent intellectual property rights exists in China, and foreign technologies are protected by patents, so that the development and utilization of whey protein resources and the sustainable development of the dairy industry in China are severely restricted. It is understood that a large amount of desalted whey powder, whey protein concentrate, whey protein isolate, lactose and other whey products are still required to be imported to be used for formula food, candy production and ice cream ingredients every year in China, and the cost is huge, so that the research and development of a method with high purity and high human body absorption rate are particularly important.
Disclosure of Invention
In view of the problems of the prior art, the invention aims to provide a method for preparing protein powder, which solves the problem that the prepared protein powder has low human body absorptivity,
In a first aspect: the invention provides a preparation method of protein powder, which comprises the following steps:
1) centrifuging sterilized milk at 4 deg.C and 3000r/min for 15min, and removing upper layer fat to obtain skimmed milk;
2) centrifuging skim milk at 4 deg.C and 5000r/min for 20min, and collecting supernatant;
3) centrifuging the supernatant obtained in the step 2) for 1h at 100000r/min, and collecting the supernatant to obtain a whey protein solution;
4) mixing the whey protein solution with four times volume of precooled acetone, slightly shaking, centrifuging at 12000r/m for 40min, and collecting precipitate;
5) re-dissolving the precipitate obtained in the step 4) with urea, adding a trypsin solution, reacting for 12h at 37 ℃ under regulation, centrifuging for 10min at 12000r/min, and collecting supernatant;
6) desalting the supernatant obtained in the step 5), carrying out vacuum centrifugal drying, and carrying out vacuum packaging to obtain protein powder.
Preferably, the step 1) is specifically:
1) freezing sterilized milk, refrigerating at-20 deg.C for 24 hr, thawing, centrifuging at 4 deg.C and 3000r/min for 15min, and removing upper fat to obtain skimmed milk.
Preferably, the step 2) is specifically:
2) adjusting pH of skim milk to 4.6, centrifuging at 4 deg.C and 5000r/min for 20min, and collecting supernatant.
Preferably, the step 3) is specifically:
3) centrifuging the supernatant obtained in the step 2) for 1h at 100000r/min, collecting the supernatant, centrifuging the supernatant for 1h at 100000r/min again, and collecting the supernatant to obtain the whey protein solution.
Preferably, the step 4) is specifically: mixing the whey protein solution with four times volume of precooled acetone, slightly shaking, storing for 20h at-20 ℃, centrifuging for 40min at 12000r/m, and collecting the precipitate.
Preferably, the step 5) is specifically: re-dissolving the precipitate with urea, adding trypsin solution, reacting at 37 deg.C for 12h, centrifuging at 12000r/min for 10min, and collecting supernatant.
Preferably, the supernatant is desalted using dialysis.
Preferably, the vacuum centrifugal drying is drying the desalted supernatant by using a vacuum freeze-dryer.
Preferably, the step 5) is specifically: dissolving urea and sediment again, adding a complex enzyme solution, reacting for 12h at 37 ℃, centrifuging for 10min at 12000r/min, and collecting supernatant, wherein the complex enzyme solution comprises the following substances: trypsin solution, serrapeptase solution, and subtilisin solution; the solubility of the trypsin, the serrapeptase and the subtilisin is 1mol/L, and the volume ratio of the protease solution to the serrapeptase solution to the subtilisin solution is 2: 1: 1.
preferably, the dialysis desalination comprises the steps of:
(1) putting the dialysis tube into 1mol/L EDTA solution, heating to boil, adding sodium bicarbonate solution, boiling for 15 min;
(2) adding ammonium sulfate into the supernatant obtained in the step 5), stirring to fully dissolve, and standing for 20min at the temperature of 4 ℃ to obtain a precipitation solution;
(3) and (3) centrifuging the precipitation solution obtained in the step (2) for 20min at the speed of 1000r/min, removing supernatant, adding distilled water to dissolve the precipitation, putting the precipitation solution into the dialysis tube treated in the step (1), dialyzing for 2h, continuously stirring the solution during dialysis, and completing desalination after dialysis is completed.
Has the advantages that:
the method comprises the steps of firstly obtaining skim milk, removing fat, then carrying out centrifugal separation for the first time, separating out part of other high-abundance proteins, further carrying out high-speed centrifugal separation to obtain a whey protein solution, then purifying the whey protein, mixing the whey protein solution with precooled acetone with four times of volume, stirring to obtain a precipitate, wherein the precipitate is the whey protein, then hydrolyzing the whey protein, redissolving the precipitate by using urea, adding trypsin to hydrolyze the whey protein at 37 ℃, carrying out high-speed centrifugal separation to collect supernatant after full reaction, and finally desalting and carrying out vacuum centrifugal drying on the supernatant to obtain protein powder which is easy to digest by a human body and has high purity.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIG. 1 is a flow chart of a method for preparing protein powder according to an embodiment of the present invention;
FIG. 2 is a flow chart of another method of protein powder production in accordance with an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, fig. 1 shows a flow chart of a protein powder preparation method,
step 102: centrifuging skim milk at 4 deg.C and 5000r/min for 20min, and collecting supernatant;
step 103: centrifuging the supernatant obtained in the step 2) for 1h at 100000r/min, and collecting the supernatant to obtain a whey protein solution;
step 104: mixing the whey protein solution with four times volume of precooled acetone, slightly shaking, centrifuging at 12000r/m for 40min, and collecting precipitate;
105, redissolving the precipitate obtained in the step 4) by using urea, adding a trypsin solution, reacting for 12 hours at 37 ℃ under regulation, centrifuging for 10 minutes at 12000r/min, and collecting supernatant;
step 106: desalting the supernatant obtained in the step 5), carrying out vacuum centrifugal drying, and carrying out vacuum packaging to obtain protein powder.
In the above process, firstly obtaining skim milk in step 101, removing fat, then performing first centrifugal separation in step 102 to separate part of other abundant proteins, then obtaining whey protein solution by high-speed centrifugal separation in step 103, then preparing to purify whey protein in step 104, then mixing the whey protein solution with four times volume of precooled acetone, stirring to obtain precipitate, wherein the precipitate is whey protein, then hydrolyzing the whey protein in step 105, redissolving the precipitate by urea, adding trypsin to hydrolyze the whey protein at 37 ℃, after sufficient reaction, performing high-speed centrifugal separation to collect supernatant, finally desalting the supernatant obtained in step 105, performing vacuum centrifugal drying to obtain protein powder easy to digest by human body, and performing multiple procedures on the sterilized milk in the process to obtain whey protein, and hydrolyzing the whey protein to finally obtain protein powder which is easy to digest by human bodies.
Referring to fig. 2, fig. 2 is a flow chart of a protein powder preparation method, which is further defined by the flow chart shown in fig. 1;
step 201 in the figure: freezing sterilized milk, refrigerating at-20 deg.C for 24 hr, thawing, centrifuging at 4 deg.C and 3000r/min for 15min, and removing upper fat to obtain skimmed milk;
step 202: adjusting pH of skim milk to 4.6, centrifuging at 4 deg.C and 5000r/min for 20min, and collecting supernatant;
step 203: centrifuging the supernatant obtained in the step 2) for 1h at 100000r/min, collecting the supernatant, centrifuging the supernatant for 1h at 100000r/min again, and collecting the supernatant to obtain the whey protein solution.
Step 204: mixing the whey protein solution with four times volume of precooled acetone, slightly shaking, storing for 20h at-20 ℃, centrifuging for 40min at 12000r/m, and collecting the precipitate.
Step 205: re-dissolving urea and the precipitate, adding sodium bicarbonate, adding a trypsin solution, reacting at 37 ℃ for 12h, centrifuging at 12000r/min for 10min, and collecting the supernatant;
step 206: desalting the supernatant obtained in the step 5), carrying out vacuum centrifugal drying, and carrying out vacuum packaging to obtain protein powder.
In the flow shown in fig. 2, comparing with fig. 1, in step 201, milk is frozen, refrigerated for 24h and then degreased to ensure thorough degreasing and further improve the purity of the finally obtained protein powder, in step 202, the pH is adjusted to 4.6, then the milk is centrifuged at 4 ℃ and 5000r/min for 20min to further improve the removal of other abundant proteins in the milk, in step 203, high-speed centrifugation is performed twice to ensure the purity of the obtained whey protein, in step 204, the whey protein solution is mixed with four times the volume of precooled acetone, slightly vibrated, stored for 20h at-20 ℃, centrifuged again to reduce the loss of the whey protein, then in step 205, urea and precipitate are used for redissolving, sodium bicarbonate is added, trypsin is added, complete reaction is further ensured, and finally in step 206, supernatant is desalted, Vacuum centrifugal drying to obtain protein powder with high purity and easy absorption by human body.
Example 1
1) Centrifuging 10L sterilized milk at 4 deg.C and 3000r/min for 15min to obtain skimmed milk;
2) centrifuging the skim milk obtained in the step 1) at 4 ℃ at 5000r/min for 20min, and collecting supernatant;
3) centrifuging the supernatant obtained in the step 2) for 1h at 100000r/min, and collecting the supernatant to obtain a whey protein solution;
4) mixing the whey protein solution with four times volume of precooled acetone, slightly shaking, centrifuging at 12000r/m for 40min, and collecting precipitate;
5) re-dissolving the precipitate obtained in the step 4) with urea, adding 4ml of trypsin solution with the solubility of 1mol/L, reacting at 37 ℃ for 12h, centrifuging at 12000r/min for 10min, and collecting the supernatant;
6) desalting the supernatant obtained in step 5), wherein the desalting by dialysis comprises the following steps:
(1) putting the dialysis tube into 1mol/L EDTA solution, heating to boil, adding sodium bicarbonate solution, boiling for 15 min;
(2) adding ammonium sulfate into the supernatant obtained in the step 5), stirring to fully dissolve, and standing for 20min at the temperature of 4 ℃ to obtain a precipitation solution;
(3) and (3) centrifuging the precipitation solution obtained in the step (2) for 20min at the speed of 1000r/min, removing supernatant, adding distilled water to dissolve the precipitation, putting the precipitation solution into the dialysis tube treated in the step (1), dialyzing for 2h, continuously stirring the solution during the dialysis, completing desalination after the dialysis is completed, performing vacuum centrifugal drying, and performing vacuum packaging to obtain protein powder.
Example 2
1) Freezing 10L sterilized milk, refrigerating at-20 deg.C for 24 hr, thawing, centrifuging at 4 deg.C and 3000r/min for 15min, and removing upper fat to obtain skimmed milk;
2) centrifuging the skim milk obtained in the step 1) at 4 ℃ at 5000r/min for 20min, and collecting supernatant;
3) centrifuging the supernatant obtained in the step 2) for 1h at 100000r/min, and collecting the supernatant to obtain a whey protein solution;
4) mixing the whey protein solution with four times volume of precooled acetone, slightly shaking, centrifuging at 12000r/m for 40min, and collecting precipitate;
5) re-dissolving the precipitate obtained in the step 4) with urea, adding 4ml of trypsin solution with the solubility of 1mol/L, reacting at 37 ℃ for 12h, centrifuging at 12000r/min for 10min, and collecting the supernatant;
6) desalting the supernatant obtained in step 5), wherein the desalting by dialysis comprises the following steps:
(1) putting the dialysis tube into 1mol/L EDTA solution, heating to boil, adding sodium bicarbonate solution, boiling for 15 min;
(2) adding ammonium sulfate into the supernatant obtained in the step 5), stirring to fully dissolve, and standing for 20min at the temperature of 4 ℃ to obtain a precipitation solution;
(3) and (3) centrifuging the precipitation solution obtained in the step (2) for 20min at the speed of 1000r/min, removing supernatant, adding distilled water to dissolve the precipitation, putting the precipitation solution into the dialysis tube treated in the step (1), dialyzing for 2h, continuously stirring the solution during the dialysis, completing desalination after the dialysis is completed, performing vacuum centrifugal drying, and performing vacuum packaging to obtain protein powder.
Example 3
1) Centrifuging 10L sterilized milk at 4 deg.C and 3000r/min for 15min to obtain skimmed milk;
2) adjusting the pH value of the skim milk obtained in the step 1) to 4.6, centrifuging the skim milk at the temperature of 4 ℃ and at the speed of 5000r/min for 20min, and collecting supernatant;
3) centrifuging the supernatant obtained in the step 2) for 1h at 100000r/min, and collecting the supernatant to obtain a whey protein solution;
4) mixing the whey protein solution with four times volume of precooled acetone, slightly shaking, centrifuging at 12000r/m for 40min, and collecting precipitate;
5) re-dissolving the precipitate obtained in the step 4) with urea, adding 4ml of trypsin solution with the solubility of 1mol/L, reacting at 37 ℃ for 12h, centrifuging at 12000r/min for 10min, and collecting the supernatant;
6) desalting the supernatant obtained in step 5), wherein the desalting by dialysis comprises the following steps:
(1) putting the dialysis tube into 1mol/L EDTA solution, heating to boil, adding sodium bicarbonate solution, boiling for 15 min;
(2) adding ammonium sulfate into the supernatant obtained in the step 5), stirring to fully dissolve, and standing for 20min at the temperature of 4 ℃ to obtain a precipitation solution;
(3) and (3) centrifuging the precipitation solution obtained in the step (2) for 20min at the speed of 1000r/min, removing supernatant, adding distilled water to dissolve the precipitation, putting the precipitation solution into the dialysis tube treated in the step (1), dialyzing for 2h, continuously stirring the solution during the dialysis, completing desalination after the dialysis is completed, performing vacuum centrifugal drying, and performing vacuum packaging to obtain protein powder.
Example 4
1) Centrifuging 10L sterilized milk at 4 deg.C and 3000r/min for 15min to obtain skimmed milk;
2) centrifuging the skim milk obtained in the step 1) at 4 ℃ at 5000r/min for 20min, and collecting supernatant;
3) centrifuging the supernatant obtained in the step 2) for 1h at 100000r/min, collecting the supernatant, centrifuging the supernatant for 1h at 100000r/min again, and collecting the supernatant to obtain a whey protein solution;
4) mixing the whey protein solution with four times volume of precooled acetone, slightly shaking, centrifuging at 12000r/m for 40min, and collecting precipitate;
5) re-dissolving the precipitate obtained in the step 4) with urea, adding 4ml of trypsin solution with the solubility of 1mol/L, reacting at 37 ℃ for 12h, centrifuging at 12000r/min for 10min, and collecting the supernatant;
6) desalting the supernatant obtained in step 5), wherein the desalting by dialysis comprises the following steps:
(1) putting the dialysis tube into 1mol/L EDTA solution, heating to boil, adding sodium bicarbonate solution, boiling for 15 min;
(2) adding ammonium sulfate into the supernatant obtained in the step 5), stirring to fully dissolve, and standing for 20min at the temperature of 4 ℃ to obtain a precipitation solution;
(3) and (3) centrifuging the precipitation solution obtained in the step (2) for 20min at the speed of 1000r/min, removing supernatant, adding distilled water to dissolve the precipitation, putting the precipitation solution into the dialysis tube treated in the step (1), dialyzing for 2h, continuously stirring the solution during the dialysis, completing desalination after the dialysis is completed, performing vacuum centrifugal drying, and performing vacuum packaging to obtain protein powder.
Example 5
1) Centrifuging 10L sterilized milk at 4 deg.C and 3000r/min for 15min to obtain skimmed milk;
2) centrifuging the skim milk obtained in the step 1) at 4 ℃ at 5000r/min for 20min, and collecting supernatant;
3) centrifuging the supernatant obtained in the step 2) for 1h at 100000r/min, and collecting the supernatant to obtain a whey protein solution;
4) mixing the whey protein solution with four times volume of precooled acetone, slightly shaking, storing for 20h at-20 ℃, centrifuging for 40min at 12000r/m, and collecting precipitate;
5) re-dissolving the precipitate obtained in the step 4) with urea, adding 4ml of trypsin solution with the solubility of 1mol/L, reacting at 37 ℃ for 12h, centrifuging at 12000r/min for 10min, and collecting the supernatant;
6) desalting the supernatant obtained in step 5), wherein the desalting by dialysis comprises the following steps:
(1) putting the dialysis tube into 1mol/L EDTA solution, heating to boil, adding sodium bicarbonate solution, boiling for 15 min;
(2) adding ammonium sulfate into the supernatant obtained in the step 5), stirring to fully dissolve, and standing for 20min at the temperature of 4 ℃ to obtain a precipitation solution;
(3) and (3) centrifuging the precipitation solution obtained in the step (2) for 20min at the speed of 1000r/min, removing supernatant, adding distilled water to dissolve the precipitation, putting the precipitation solution into the dialysis tube treated in the step (1), dialyzing for 2h, continuously stirring the solution during the dialysis, completing desalination after the dialysis is completed, performing vacuum centrifugal drying, and performing vacuum packaging to obtain protein powder.
Example 6
1) Centrifuging 10L sterilized milk at 4 deg.C and 3000r/min for 15min to obtain skimmed milk;
2) centrifuging the skim milk obtained in the step 1) at 4 ℃ at 5000r/min for 20min, and collecting supernatant;
3) centrifuging the supernatant obtained in the step 2) for 1h at 100000r/min, and collecting the supernatant to obtain a whey protein solution;
4) mixing the whey protein solution with four times volume of precooled acetone, slightly shaking, centrifuging at 12000r/m for 40min, and collecting precipitate;
5) dissolving urea and the precipitate obtained in the step 4) again, adding sodium bicarbonate with the addition of 2mg, adding a trypsin solution, reacting for 12h at 37 ℃, centrifuging for 10min at 12000r/min, and collecting the supernatant;
6) desalting the supernatant obtained in step 5), wherein the desalting by dialysis comprises the following steps:
(1) putting the dialysis tube into 1mol/L EDTA solution, heating to boil, adding sodium bicarbonate solution, boiling for 15 min;
(2) adding ammonium sulfate into the supernatant obtained in the step 5), stirring to fully dissolve, and standing for 20min at the temperature of 4 ℃ to obtain a precipitation solution;
(3) and (3) centrifuging the precipitation solution obtained in the step (2) for 20min at the speed of 1000r/min, removing supernatant, adding distilled water to dissolve the precipitation, putting the precipitation solution into the dialysis tube treated in the step (1), dialyzing for 2h, continuously stirring the solution during the dialysis, completing desalination after the dialysis is completed, performing vacuum centrifugal drying, and performing vacuum packaging to obtain protein powder.
Example 7
1) Freezing sterilized milk, refrigerating at-20 deg.C for 24 hr, thawing, centrifuging at 4 deg.C and 3000r/min for 15min, and removing upper fat to obtain skimmed milk;
2) adjusting pH of skim milk to 4.6, centrifuging at 4 deg.C and 5000r/min for 20min, and collecting supernatant;
3) centrifuging the supernatant obtained in the step 2) for 1h at 100000r/min, collecting the supernatant, centrifuging the supernatant for 1h at 100000r/min again, and collecting the supernatant to obtain the whey protein solution.
4) Mixing the whey protein solution with four times volume of precooled acetone, slightly shaking, storing for 20h at-20 ℃, centrifuging for 40min at 12000r/m, and collecting the precipitate.
5) Adding sodium bicarbonate into urea and precipitate for redissolution, and adding a complex enzyme solution, wherein the complex enzyme solution comprises the following substances: trypsin solution, serrapeptase solution, and subtilisin solution; the solubility of the trypsin, the serrapeptase and the subtilisin is 1mol/L, and the volume ratio of the protease solution to the serrapeptase solution to the subtilisin solution is 2: 1: 1, adding 4ml of complex enzyme solution, reacting at 37 ℃ for 12h, centrifuging at 12000r/min for 10min, and collecting supernatant;
6) desalting the supernatant obtained in step 5), wherein the desalting by dialysis comprises the following steps:
(1) putting the dialysis tube into 1mol/L EDTA solution, heating to boil, adding sodium bicarbonate solution, boiling for 15 min;
(2) adding ammonium sulfate into the supernatant obtained in the step 5), stirring to fully dissolve, and standing for 20min at the temperature of 4 ℃ to obtain a precipitation solution;
(3) and (3) centrifuging the precipitation solution obtained in the step (2) for 20min at the speed of 1000r/min, removing supernatant, adding distilled water to dissolve the precipitation, putting the precipitation solution into the dialysis tube treated in the step (1), dialyzing for 2h, continuously stirring the solution during the dialysis, completing desalination after the dialysis is completed, performing vacuum centrifugal drying, and performing vacuum packaging to obtain protein powder.
Comparative example 1
The comparative example 1 is different from example 1 in that step 2) is eliminated, and other preparation conditions are identical to those of example 1.
Comparative example 2
The difference between the comparative example 2 and the example 1 is that the step 3) is to centrifuge the supernatant obtained in the step 2) for 1h at 50000r/min, and other preparation conditions are the same as those in the example 1.
Comparative example 3
The comparative example 3 differs from example 1 in that step 4) is specifically to mix the whey protein solution with four times the volume of pre-chilled acetone, shake slightly, collect the precipitate after standing, and the other preparation conditions are the same as example 1.
Comparative example 4
The difference between the comparative example 4 and the example 1 is that the step 5) is specifically to use urea to re-dissolve the precipitate obtained in the step 4), a pepsin solution is added, the solubility of the pepsin solution is 1mol/L, the addition amount is 4ml, the reaction is carried out for 12h under the regulation of 37 ℃, the centrifugation is carried out for 10min at 12000r/min, the supernatant is collected, and other preparation conditions are consistent with those of the example 1.
Comparative example 5
The comparative example 5 is different from the example 6 only in that the complex enzyme solution does not contain trypsin, and other preparation conditions are consistent with those of the example 1.
Comparative example 6
The comparative example 6 is different from example 6 only in that the other preparation conditions without serrapeptase in the complex enzyme solution are the same as those of example 1.
Comparative example 7
The comparative example 6 is different from the example 6 only in that the complex enzyme solution does not contain subtilisin, and other preparation conditions are the same as those of the example 1.
The protein powders prepared in examples 1 to 6 and comparative examples 1 to 7 were examined, and the examination results are shown in Table 1 below
TABLE 1
It can be seen from table 1 that the protein powder prepared by the present invention has high conversion rate, high purity and high absorption rate, as seen by comparing comparative examples 1-4 with example 1, each preparation step in example 1 has a serious influence on the quality of the obtained protein powder, and as seen by comparing comparative examples 5-7 with example 6, trypsin in the complex enzyme solution is a main effect enzyme, and the effect of combining serratipeptidase with subtilisin and trypsin is better, thereby greatly improving the absorption rate of the protein powder.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for preparing protein powder, which comprises the following steps:
1) centrifuging sterilized milk at 4 deg.C and 3000r/min for 15min, and removing upper layer fat to obtain skimmed milk;
2) centrifuging skim milk at 4 deg.C and 5000r/min for 20min, and collecting supernatant;
3) centrifuging the supernatant obtained in the step 2) for 1h at 100000r/min, and collecting the supernatant to obtain a whey protein solution;
4) mixing the whey protein solution with four times volume of precooled acetone, slightly shaking, centrifuging at 12000r/m for 40min, and collecting precipitate;
5) re-dissolving the precipitate obtained in the step 4) with urea, adding a trypsin solution, reacting for 12h at 37 ℃ under regulation, centrifuging for 10min at 12000r/min, and collecting supernatant;
6) desalting the supernatant obtained in the step 5), carrying out vacuum centrifugal drying, and carrying out vacuum packaging to obtain protein powder.
2. The method according to claim 1, wherein the step 1) is specifically:
1) freezing sterilized milk, refrigerating at-20 deg.C for 24 hr, thawing, centrifuging at 4 deg.C and 3000r/min for 15min, and removing upper fat to obtain skimmed milk.
3. The method according to claim 1, wherein the step 2) is specifically:
2) adjusting pH of skim milk to 4.6, centrifuging at 4 deg.C and 5000r/min for 20min, and collecting supernatant.
4. The method according to claim 1, wherein the step 3) is specifically:
3) centrifuging the supernatant obtained in the step 2) for 1h at 100000r/min, collecting the supernatant, centrifuging the supernatant for 1h at 100000r/min again, and collecting the supernatant to obtain the whey protein solution.
5. The method according to claim 1, wherein the step 4) is specifically:
mixing the whey protein solution with four times volume of precooled acetone, slightly shaking, storing for 20h at-20 ℃, centrifuging for 40min at 12000r/m, and collecting the precipitate.
6. The method according to claim 1, wherein the step 5) is specifically:
dissolving urea and precipitate again, adding sodium bicarbonate, adding trypsin solution, reacting at 37 deg.C for 12h, centrifuging at 12000r/min for 10min, and collecting supernatant.
7. The method of claim 1, wherein the supernatant is desalted using dialysis.
8. The method of claim 1, wherein the vacuum centrifugal drying is drying the desalted supernatant using a vacuum freeze-dryer.
9. The method according to claim 6, wherein the step 5) is specifically: dissolving urea and sediment again, adding a complex enzyme solution, reacting for 12h at 37 ℃, centrifuging for 10min at 12000r/min, and collecting supernatant, wherein the complex enzyme solution comprises the following substances: trypsin solution, serrapeptase solution, and subtilisin solution; the solubility of the trypsin, the serrapeptase and the subtilisin is 1mol/L, and the volume ratio of the protease solution to the serrapeptase solution to the subtilisin solution is 2: 1: 1.
10. the method of claim 7, wherein the dialysis desalination comprises the steps of:
(1) putting the dialysis tube into 1mol/L EDTA solution, heating to boil, adding sodium bicarbonate solution, boiling for 15 min;
(2) adding ammonium sulfate into the supernatant obtained in the step 5), stirring to fully dissolve, and standing for 20min at the temperature of 4 ℃ to obtain a precipitation solution;
(3) and (3) centrifuging the precipitation solution obtained in the step (2) for 20min at the speed of 1000r/min, removing supernatant, adding distilled water to dissolve the precipitation, putting the precipitation solution into the dialysis tube treated in the step (1), dialyzing for 2h, continuously stirring the solution during dialysis, and completing desalination after dialysis is completed.
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| CN114651871A (en) * | 2022-04-26 | 2022-06-24 | 沈阳农业大学 | Sheep colostrum protein milk beverage based on pilose antler polypeptide and preparation method thereof |
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