CN113575966B - Egg white peptide chelated calcium and preparation method thereof - Google Patents
Egg white peptide chelated calcium and preparation method thereof Download PDFInfo
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- 102000002322 Egg Proteins Human genes 0.000 title claims abstract description 95
- 108010000912 Egg Proteins Proteins 0.000 title claims abstract description 95
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 75
- 239000011575 calcium Substances 0.000 title claims abstract description 75
- 108090000765 processed proteins & peptides Proteins 0.000 title claims abstract description 65
- QCVGEOXPDFCNHA-UHFFFAOYSA-N 5,5-dimethyl-2,4-dioxo-1,3-oxazolidine-3-carboxamide Chemical compound CC1(C)OC(=O)N(C(N)=O)C1=O QCVGEOXPDFCNHA-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 210000000969 egg white Anatomy 0.000 title claims abstract description 37
- 235000014103 egg white Nutrition 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 210000003278 egg shell Anatomy 0.000 claims abstract description 60
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 45
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 37
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 24
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 238000000498 ball milling Methods 0.000 claims abstract description 12
- 102000003846 Carbonic anhydrases Human genes 0.000 claims abstract description 11
- 108090000209 Carbonic anhydrases Proteins 0.000 claims abstract description 11
- 239000013522 chelant Substances 0.000 claims abstract description 7
- 238000004108 freeze drying Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 238000000108 ultra-filtration Methods 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 239000012528 membrane Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000011049 filling Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 239000012141 concentrate Substances 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 5
- 150000007524 organic acids Chemical class 0.000 abstract description 3
- 235000001968 nicotinic acid Nutrition 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 229960005069 calcium Drugs 0.000 description 66
- 102000005701 Calcium-Binding Proteins Human genes 0.000 description 12
- 108010045403 Calcium-Binding Proteins Proteins 0.000 description 12
- 102000057297 Pepsin A Human genes 0.000 description 6
- 108090000284 Pepsin A Proteins 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 230000029087 digestion Effects 0.000 description 6
- 238000000338 in vitro Methods 0.000 description 6
- 230000014759 maintenance of location Effects 0.000 description 6
- 229940111202 pepsin Drugs 0.000 description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 235000013601 eggs Nutrition 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 238000000464 low-speed centrifugation Methods 0.000 description 4
- 235000013305 food Nutrition 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 206010006956 Calcium deficiency Diseases 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- FNAQSUUGMSOBHW-UHFFFAOYSA-H calcium citrate Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O FNAQSUUGMSOBHW-UHFFFAOYSA-H 0.000 description 2
- 239000001354 calcium citrate Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 235000013337 tricalcium citrate Nutrition 0.000 description 2
- BCZXFFBUYPCTSJ-UHFFFAOYSA-L Calcium propionate Chemical compound [Ca+2].CCC([O-])=O.CCC([O-])=O BCZXFFBUYPCTSJ-UHFFFAOYSA-L 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 208000001132 Osteoporosis Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 1
- 239000001639 calcium acetate Substances 0.000 description 1
- 235000011092 calcium acetate Nutrition 0.000 description 1
- 229960005147 calcium acetate Drugs 0.000 description 1
- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 description 1
- 239000001527 calcium lactate Substances 0.000 description 1
- 229960002401 calcium lactate Drugs 0.000 description 1
- 235000011086 calcium lactate Nutrition 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 239000004330 calcium propionate Substances 0.000 description 1
- 235000010331 calcium propionate Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 210000002969 egg yolk Anatomy 0.000 description 1
- 235000013345 egg yolk Nutrition 0.000 description 1
- 206010016256 fatigue Diseases 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 108010007119 flavourzyme Proteins 0.000 description 1
- 208000018944 leg cramp Diseases 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007084 physiological dysfunction Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/16—Inorganic salts, minerals or trace elements
- A23L33/165—Complexes or chelates
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L15/00—Egg products; Preparation or treatment thereof
- A23L15/25—Addition or treatment with microorganisms or enzymes
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L15/00—Egg products; Preparation or treatment thereof
- A23L15/30—Addition of substances other than those covered by A23L15/20 – A23L15/25
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/015—Inorganic compounds
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Polymers & Plastics (AREA)
- Nutrition Science (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Mycology (AREA)
- Microbiology (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Peptides Or Proteins (AREA)
Abstract
The invention relates to an egg white peptide chelated calcium and a preparation method thereof. The invention puts the nanometer eggshell calcium powder obtained by eggshell ball milling into carbonic anhydrase solution, continuously stirs and introduces CO 2 Releasing calcium ions into the solution, and centrifuging to obtain a calcium ion solution; acidolysis of egg white protein with acetic acid to obtain protein peptide with rich calcium ion binding site, ultrafiltering and concentrating to obtain protein peptide concentrate; mixing the protein peptide concentrated solution with a calcium ion solution, regulating the pH value, stirring at a low speed to fully chelate the protein peptide concentrated solution and the calcium ion solution, ultrafiltering, concentrating and freeze-drying to obtain the egg white peptide chelated calcium. The invention utilizes the bionics principle and combines with organic acid to hydrolyze protein, thereby realizing the efficient utilization of waste eggshells and providing a feasible way for green and efficient preparation of the egg white peptide chelated calcium.
Description
Technical Field
The invention relates to the field of egg product processing, in particular to egg white peptide chelated calcium and a preparation method thereof.
Background
With the continuous improvement of the living standard of people, the food processing industry rapidly develops, and eggs are widely applied to the fields of catering, food processing and the like, but only edible parts of the eggs, namely egg white and egg yolk, are mainly utilized, and the egg shells are discarded. Eggshells contain 93% of calcium carbonate and 3.2% of calcium phosphate, and are good sources of biological calcareous resources. The accumulated and discarded eggshells seriously pollute the environment, waste of a large amount of calcium resources is caused, and the problem of how to fully excavate the potential utilization value in the eggshells by utilizing the natural calcium resources of the eggshells is solved.
The resident in China has the symptom of calcium deficiency, especially the old and children. Calcium deficiency can lead to various physiological dysfunctions such as hypoevolutism, fatigue, leg cramp, osteoporosis, childhood growth pain, etc. Therefore, the resource utilization of the waste eggshells of the egg processing industry is increased, the biological tissue is used as a natural green calcium source to prepare a peptide calcium product with high bioavailability, the pollution of the eggshells to the ecological environment can be reduced, and the construction of a resource-saving environment-friendly society is facilitated.
Eggshell calcium mainly exists in the form of inorganic calcium carbonate, is not easy to digest and absorb in animal bodies, and cannot be directly used for producing foods, and in order to improve the absorption rate of calcium in eggshells, inorganic calcium is usually converted into an organic calcium or peptide calcium product with high calcium bioavailability. The traditional eggshell calcium product mainly comprises calcium acetate, calcium propionate, calcium citrate and egg white peptide chelated calcium. The traditional preparation process of eggshell organic calcium is mostly a calcination method and an acid-base neutralization method, and has the problems of high energy consumption, serious environmental pollution of waste liquid, high cost of raw material organic acid, high product cost, low purity and the like. The eggshell is fermented by microorganisms, calcium ions are released during acid production, and various organic calcium (calcium citrate, calcium lactate and the like) is produced in a combined way, but the eggshell has the defects of long production period, high energy consumption, low efficiency and the like, and is not beneficial to green and large-scale preparation.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of egg white peptide chelated calcium, which solves the problems in the prior art, adopts a bionics principle to prepare egg white peptide chelated calcium, and realizes green ecological conversion of egg shell calcium into a peptide calcium product with high calcium bioavailability.
The technical scheme adopted by the invention is as follows:
a method for preparing egg white peptide chelated calcium, comprising the following steps:
(1) Preparing eggshell calcium ions: adding carbonic anhydrase into nano eggshell calcium powder obtained by eggshell ball milling, stirring for reaction, and centrifuging to obtain a calcium ion solution;
(2) Egg white protein peptide preparation: acidolysis of egg white protein by acetic acid and first ultrafiltration concentration to obtain protein peptide concentrated solution;
(3) Egg white peptide chelated calcium preparation: mixing the protein peptide concentrated solution with the calcium ion solution, stirring to fully chelate the protein peptide concentrated solution and the calcium ion solution, and freeze-drying after the second ultrafiltration concentration to obtain the egg white peptide chelated calcium.
Preferably, in the step (1), ball milling conditions of eggshells are: ball material ratio (4-6) is 1, solid-liquid ratio is 1, liquid is absolute ethyl alcohol, filling rate is 15-25%, and ball milling is carried out for 10-15 hours under the condition of rotating speed 350-450 r/min.
Preferably, in the step (1), the carbonic anhydrase is used in an amount of 100-150U/g nano eggshell calcium powder.
Preferably, in the step (1), CO is introduced during stirring 2 The reaction conditions are as follows: reacting at 33-42 ℃ for 24-36 hours.
Preferably, in the step (1), the nano eggshell calcium powder is added into deionized water according to the proportion of 1 (8-12).
Preferably, in the step (2), the concentration of acetic acid is 4.0-6.0g/100ml, and the acidolysis condition is: the time is 48-72 hours, and the temperature is 40-50 ℃.
Preferably, the membrane size of the first ultrafiltration concentration in the step (2) is 5kDa, and the membrane size of the second ultrafiltration concentration in the step (3) is 2kDa.
Preferably, in the step (3), the pH is adjusted to 7.5-8.0 before stirring.
The invention has the beneficial effects that:
1. the invention puts the nanometer eggshell calcium powder obtained by eggshell ball milling into carbonic anhydrase solution, continuously stirs and introduces CO 2 Releasing calcium ions into the solution, and centrifuging to obtain a calcium ion solution; acidolysis of egg white protein with acetic acid to obtain protein peptide with rich calcium ion binding site, ultrafiltering and concentrating to obtain protein peptide concentrate; mixing the protein peptide concentrated solution with calcium ion solution, regulating pH value, stirring at low speed to chelate the two,and (5) performing ultrafiltration concentration and freeze drying to obtain the egg white peptide chelated calcium. Realize the high-efficiency utilization of the waste eggshells, provide a feasible way for the green preparation of the egg white peptide chelated calcium, and can not pollute the environment.
2. The method has the advantages of effectively solving the problems of high energy consumption, serious environmental pollution, high product cost, low purity and the like caused by the common method for converting eggshell calcium into organic calcium, namely a chemical neutralization method for preparing calcium oxide by calcining and replacing organic acid with a chemical reagent under the condition of a certain pH value.
3. Compared with the microbial fermentation eggshell, the method has the advantages of short production period, low energy consumption and high efficiency.
Detailed Description
The following description of the embodiments of the present invention will clearly and fully describe the technical solutions of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A method for preparing egg white peptide chelated calcium, comprising the following steps:
(1) Preparing eggshell calcium ions: ball milling the cleaned eggshells for 13 hours under the conditions of a ball-material ratio of 5:1, a solid-liquid ratio of 1:2, a filling rate of 20 percent and a rotating speed of 400 r/min to obtain the nano eggshell calcium powder. Adding deionized water into the nano eggshell calcium powder according to the ratio of 1:10, and then adding carbonic anhydrase into the nano eggshell calcium powder according to the ratio of 135U/g. Continuously stirring and introducing CO 2 The reaction was carried out at 37℃for 34 hours. And releasing calcium ions into the solution, and obtaining the calcium ion solution after low-speed centrifugation.
(2) Egg white protein peptide preparation: the egg white is diluted 1:1 with water, stirred at low speed and acetic acid is slowly added until the acetic acid concentration is 6.0g/100ml. Acidolysis was carried out at a constant temperature of 45℃for 55 hours. Acidolysis of egg white protein with acetic acid to obtain protein peptide with rich calcium ion binding site, and ultrafiltering and concentrating with 5kDa ultrafilter membrane to obtain protein peptide concentrate.
(3) Egg white peptide chelated calcium preparation: mixing the protein peptide concentrated solution with calcium ion solution, adjusting pH value to 7.5-8.0, and stirring at low speed to make the two fully chelate reaction. And (3) performing ultrafiltration concentration by using a 2kDa ultrafiltration membrane, and performing freeze drying to obtain the egg white peptide chelated calcium.
The egg white peptide chelated calcium product prepared in example 1 had a calcium binding capacity of 115.3mg/g, a pepsin in vitro digestion calcium binding capacity retention of 75.7%, and an eggshell calcium conversion of 86.1%.
Example 2
A method for preparing egg white peptide chelated calcium, comprising the following steps:
(1) Preparing eggshell calcium ions: ball milling the cleaned eggshells for 13 hours under the conditions of a ball-material ratio of 5:1, a solid-liquid ratio of 1:2, a filling rate of 20 percent and a rotating speed of 400 r/min to obtain the nano eggshell calcium powder. Adding deionized water into the nano eggshell calcium powder according to the ratio of 1:10, and then adding carbonic anhydrase into the nano eggshell calcium powder according to the ratio of 150U/g. Continuously stirring and introducing CO 2 The reaction was carried out at 39℃for 32 hours. And releasing calcium ions into the solution, and obtaining the calcium ion solution after low-speed centrifugation.
(2) Egg white protein peptide preparation: the egg white liquid is diluted by adding water according to the ratio of 1:1, stirred at a low speed and acetic acid is slowly added until the concentration of the acetic acid is 5.5g/100ml. Acidolysis was carried out at a constant temperature of 48℃for 60 hours. Acidolysis of egg white protein with acetic acid to obtain protein peptide with rich calcium ion binding site, and ultrafiltering and concentrating with 5kDa ultrafilter membrane to obtain protein peptide concentrate.
(3) Egg white peptide chelated calcium preparation: mixing the protein peptide concentrated solution with calcium ion solution, adjusting pH value to 7.5-8.0, and stirring at low speed to make the two fully chelate reaction. And (3) performing ultrafiltration concentration by using a 2kDa ultrafiltration membrane, and performing freeze drying to obtain the egg white peptide chelated calcium.
The egg white peptide chelated calcium product prepared in example 2 had a calcium binding capacity of 126.4mg/g, a pepsin in vitro digestion calcium binding capacity retention rate of 82.7%, and an eggshell calcium conversion rate of 84.5%.
Example 3
A method for preparing egg white peptide chelated calcium, comprising the following steps:
(1) Preparing eggshell calcium ions: ball milling the cleaned eggshells for 13 hours under the conditions of a ball-material ratio of 5:1, a solid-liquid ratio of 1:2, a filling rate of 20 percent and a rotating speed of 400 r/min to obtain the nano eggshell calcium powder. Adding deionized water into the nano eggshell calcium powder according to the ratio of 1:10, and then adding carbonic anhydrase into the nano eggshell calcium powder according to the ratio of 125U/g. Continuously stirring and introducing CO 2 The reaction was carried out at 40℃for 36 hours. And releasing calcium ions into the solution, and obtaining the calcium ion solution after low-speed centrifugation.
(2) Egg white protein peptide preparation: the egg white liquid is diluted by adding water according to the ratio of 1:1, stirred at a low speed and acetic acid is slowly added until the concentration of the acetic acid is 5.0g/100ml. Acidolysis was carried out at a constant temperature of 50℃for 72 hours. Acidolysis of egg white protein with acetic acid to obtain protein peptide with rich calcium ion binding site, and ultrafiltering and concentrating with 5kDa ultrafilter membrane to obtain protein peptide concentrate.
(3) Egg white peptide chelated calcium preparation: mixing the protein peptide concentrated solution with calcium ion solution, adjusting pH value to 7.5-8.0, and stirring at low speed to make the two fully chelate reaction. And (3) performing ultrafiltration concentration by using a 2kDa ultrafiltration membrane, and performing freeze drying to obtain the egg white peptide chelated calcium.
The egg white peptide chelated calcium product prepared in this example 3 had a calcium binding capacity of 112.3mg/g, a pepsin in vitro digestion calcium binding capacity retention of 78.6%, and an eggshell calcium conversion of 83.7%.
Comparative example 1
Based on example 3, no carbonic anhydrase, CO are added in step (1) 2 Otherwise, as in example 3, the step (1) is specifically:
(1) Preparing eggshell calcium ions: ball milling the cleaned eggshells for 13 hours under the conditions of a ball-material ratio of 5:1, a solid-liquid ratio of 1:2, a filling rate of 20 percent and a rotating speed of 400 r/min to obtain the nano eggshell calcium powder.
The egg white peptide chelated calcium product prepared in the comparative example 1 has the following calcium binding amount: 27.9mg/g, the retention rate of calcium binding by pepsin in vitro digestion is 71.6%, and the conversion rate of eggshell calcium is 22.5%.
Comparative example 2
Based on example 3, CO was not introduced in step (1) 2 Otherwise, the same as in embodiment 3 is specifically:
(1) Preparing eggshell calcium ions: ball milling the cleaned eggshells for 13 hours under the conditions of a ball-material ratio of 5:1, a solid-liquid ratio of 1:2, a filling rate of 20 percent and a rotating speed of 400 r/min to obtain the nano eggshell calcium powder. Adding deionized water into the nano eggshell calcium powder according to the ratio of 1:10, and then adding carbonic anhydrase into the nano eggshell calcium powder according to the ratio of 125U/g. Stirring was continued and the reaction was carried out at 40℃for 36 hours. And releasing calcium ions into the solution, and obtaining the calcium ion solution after low-speed centrifugation.
The egg white peptide chelated calcium product prepared in the comparative example 2 has the following calcium binding amount: 42.5mg/g, the retention rate of calcium binding by pepsin in vitro digestion is 74.1%, and the conversion rate of eggshell calcium is 34.8%.
Comparative example 3
Based on example 3, the egg white protein peptide in step (2) adopts an enzymolysis process, and the other steps are as follows in example 3:
(2) Egg white protein peptide preparation: diluting the egg white liquid with water according to a ratio of 1:2, stirring at a low speed, slowly adding 5600U/g flavourzyme, and carrying out enzymolysis under the following conditions: the temperature is 50 ℃, the pH value is 7.5, and the enzymolysis time is 4 hours. And (3) carrying out ultrafiltration concentration on the enzymolysis liquid through a 5kDa ultrafiltration membrane to obtain a protein peptide concentrated solution.
The egg white peptide chelated calcium product prepared in the comparative example 2 has the following calcium binding amount: 76.2mg/g, the retention rate of calcium binding by pepsin in vitro digestion is 70.9%, and the conversion rate of eggshell calcium is 53.5%.
The specific embodiments described herein are offered by way of example only to illustrate the spirit of the invention. Those skilled in the art may make various modifications or additions to the described embodiments or substitutions thereof without departing from the spirit of the invention or exceeding the scope of the invention as defined in the accompanying claims.
Claims (1)
1. A preparation method of egg white peptide chelated calcium is characterized by comprising the following steps: the method comprises the following steps:
(1) Preparing eggshell calcium ions: adding deionized water and carbonic anhydrase in the ratio of 1 (8-12), wherein the dosage of carbonic anhydrase is 100-150U/g nanometerStirring and reacting the rice eggshell calcium powder, and introducing CO during stirring 2 The reaction conditions are as follows: reacting for 24-36 hours at the temperature of 33-42 ℃, and centrifuging to obtain a calcium ion solution;
(2) Egg white protein peptide preparation: acidolysis of egg white protein by acetic acid and first ultrafiltration concentration to obtain protein peptide concentrated solution;
(3) Egg white peptide chelated calcium preparation: mixing the protein peptide concentrated solution with a calcium ion solution, stirring to fully chelate the protein peptide concentrated solution and the calcium ion solution, and freeze-drying after ultrafiltration and concentration for the second time to obtain egg white peptide chelated calcium; in the step (1), ball milling conditions of eggshells are as follows: ball milling for 10-15 hours under the conditions of ball material ratio (4-6) of 1, solid-liquid ratio of 1 (1-3), filling rate of 15-25% and rotating speed of 350-450 r/min; in the step (2), the concentration of acetic acid is 4.0-6.0g/100ml, and acidolysis conditions are as follows: the time is 48-72 hours, and the temperature is 40-50 ℃; the membrane specification of the first ultrafiltration concentration in the step (2) is 5kDa, and the membrane specification of the second ultrafiltration concentration in the step (3) is 2kDa; in the step (3), the pH is adjusted to 7.5-8.0 before stirring.
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| CN202110745814.8A CN113575966B (en) | 2021-07-01 | 2021-07-01 | Egg white peptide chelated calcium and preparation method thereof |
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