CN108208847B - Preparation method of marine-source amino acid compound calcium powder - Google Patents
Preparation method of marine-source amino acid compound calcium powder Download PDFInfo
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- CN108208847B CN108208847B CN201810043106.8A CN201810043106A CN108208847B CN 108208847 B CN108208847 B CN 108208847B CN 201810043106 A CN201810043106 A CN 201810043106A CN 108208847 B CN108208847 B CN 108208847B
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- 239000011575 calcium Substances 0.000 title claims abstract description 79
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 77
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 239000000843 powder Substances 0.000 title claims abstract description 45
- 150000001413 amino acids Chemical class 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 150000001875 compounds Chemical class 0.000 title claims abstract description 16
- 238000000855 fermentation Methods 0.000 claims abstract description 19
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- 239000002131 composite material Substances 0.000 claims description 14
- 230000000694 effects Effects 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
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- 102000005600 Cathepsins Human genes 0.000 claims description 8
- 108010084457 Cathepsins Proteins 0.000 claims description 8
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 8
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 8
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- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 claims description 4
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- 229960005261 aspartic acid Drugs 0.000 claims description 4
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- 239000000174 gluconic acid Substances 0.000 claims description 4
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- 238000000227 grinding Methods 0.000 claims description 4
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- 235000011090 malic acid Nutrition 0.000 claims description 4
- 238000004806 packaging method and process Methods 0.000 claims description 4
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 claims description 4
- XPFJYKARVSSRHE-UHFFFAOYSA-K trisodium;2-hydroxypropane-1,2,3-tricarboxylate;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical compound [Na+].[Na+].[Na+].OC(=O)CC(O)(C(O)=O)CC(O)=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O XPFJYKARVSSRHE-UHFFFAOYSA-K 0.000 claims description 4
- 241000186000 Bifidobacterium Species 0.000 claims description 3
- MBLBDJOUHNCFQT-LXGUWJNJSA-N aldehydo-N-acetyl-D-glucosamine Chemical compound CC(=O)N[C@@H](C=O)[C@@H](O)[C@H](O)[C@H](O)CO MBLBDJOUHNCFQT-LXGUWJNJSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 2
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- 239000002245 particle Substances 0.000 claims 1
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- 150000003839 salts Chemical class 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 7
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 3
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- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
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- 238000000643 oven drying Methods 0.000 description 2
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- QWJSAWXRUVVRLH-LREBCSMRSA-M 2-hydroxyethyl(trimethyl)azanium;(2r,3r)-2,3,4-trihydroxy-4-oxobutanoate Chemical compound C[N+](C)(C)CCO.OC(=O)[C@H](O)[C@@H](O)C([O-])=O QWJSAWXRUVVRLH-LREBCSMRSA-M 0.000 description 1
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- 239000004470 DL Methionine Substances 0.000 description 1
- 235000019733 Fish meal Nutrition 0.000 description 1
- 206010024642 Listless Diseases 0.000 description 1
- 229920002774 Maltodextrin Polymers 0.000 description 1
- 239000005913 Maltodextrin Substances 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 208000001132 Osteoporosis Diseases 0.000 description 1
- 238000012356 Product development Methods 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
- 238000010171 animal model Methods 0.000 description 1
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- 235000014590 basal diet Nutrition 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 239000011173 biocomposite Substances 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 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 1
- 239000001354 calcium citrate Substances 0.000 description 1
- 239000005018 casein Substances 0.000 description 1
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 description 1
- 235000021240 caseins Nutrition 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
- 239000004467 fishmeal Substances 0.000 description 1
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- 230000037308 hair color Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229940035034 maltodextrin Drugs 0.000 description 1
- FFEARJCKVFRZRR-UHFFFAOYSA-N methionine Chemical compound CSCCC(N)C(O)=O FFEARJCKVFRZRR-UHFFFAOYSA-N 0.000 description 1
- 229930182817 methionine Natural products 0.000 description 1
- 235000006109 methionine Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000003715 nutritional status Nutrition 0.000 description 1
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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
-
- 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
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
-
- 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
-
- 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
- A23V2400/00—Lactic or propionic acid bacteria
- A23V2400/51—Bifidobacterium
Abstract
The invention discloses a preparation method of marine amino acid compound calcium powder, which comprises the following steps: (1) washing aquatic product leftovers; (2) crushing; (3) desalting; (4) performing primary acidolysis; (5) microbial fermentation degradation; (6) carrying out enzymolysis; (7) compounding amino acid; (8) drying; (9) micronizing. The marine calcium powder is prepared by using marine biological resources such as shrimp shells, crab shells, fishbones and the like through a preparation process of enzymolysis, organic acid and amino acid compounding, and has high bioavailability and good application prospect. In the preparation process, the fermentation link is added, and the steps of enzymolysis and acidolysis which are alternately carried out are adopted, so that the extraction rate and the bioavailability of the biological calcium powder can be greatly improved.
Description
Technical Field
The invention relates to a preparation method of marine organism composite calcium powder, belonging to the technical field of biology.
Background
Calcium is an essential element for human bodies, the nutritional status of calcium in diet is closely related to growth and development of human bodies, cardiovascular diseases and chronic diseases, and sufficient calcium intake has an important effect on improving osteoporosis symptoms, at present, calcium agent products are mainly classified into inorganic calcium, organic calcium, amino acid calcium and the like, researches show that calcium is different in source and different in existing form, and has a large difference on the utilization rate of calcium, and for example, comparison of calcium absorption conditions of 8 calcium preparations in rats such as the Wangxing peak (2010) shows that the apparent absorption rate of the fishbone calcium group preparation can reach 93%, and the fishbone calcium group preparation is superior to animal calcium products; zhang Wen (2015) and the like find that PHC-Ca prepared from shrimp shells has the effect of promoting calcium absorption, and the bioavailability of the PHC-Ca is superior to that of calcium citrate and shrimp shell powder with the same calcium content, so that the preparation of calcium products by using marine biological resources is a development trend.
The coastal ocean resources of Zhejiang are rich, especially the yield of shrimps, crabs and fishes is high, but leftovers such as shrimp shells, crab shells, fishbones and the like are not effectively and comprehensively utilized every year, so that huge waste of resources is caused. At present, the bioactive calcium products in the market are fewer, the scale is not formed, and the utilization of marine biological calcium is worse.
The method has the advantages that the amount of shrimp shells, crab shells and fish bones which are leftovers of most aquatic product processing enterprises in Zhejiang is very large, the leftovers are mainly treated in the form of waste or low-value fish meal at present, and huge waste of resources is caused, even the environment is polluted, the research on the extraction of shrimp and crab shells marine biological calcium, the product development and the like is carried out, and the method has important significance for creating blue granaries in Zhejiang province, improving the marine resource utilization rate and the sustainable development of aquatic product processing: (1) the comprehensive utilization rate of ocean resources can be improved; (2) enriching the types of the current marine organism calcium products and optimizing the calcium consumption market; (3) the high-valued of the calcium source leftovers in the aquatic product processing is improved. The project conforms to the strategy of the ocean deep processing industry, has important significance for the construction of the current aquatic product processing industry structure, can play a demonstration and driving role in research and development and technical popularization of deep processing utilization in the same industry and similar industries, and can generate huge economic and social benefits.
Disclosure of Invention
In the prior art, the method for preparing the calcium powder by using the marine raw material is an enzymolysis method, but the enzymolysis efficiency is low, the yield of the obtained calcium powder is low, and the bioavailability is not high. The technical problem to be solved by the invention is as follows: provides a preparation method of marine organism composite calcium powder.
The preparation method of the marine source amino acid compound calcium powder provided by the invention comprises the following steps:
(1) washing aquatic product leftovers: washing the aquatic product leftovers with clear water for 2-3 times, and then drying.
(2) Crushing: crushing the dried aquatic product leftovers to obtain powder of 10-30 meshes.
(3) Desalting: soaking the product powder obtained in the step (2) in water in a mass ratio of 1:5 for 20-60min, setting the temperature of the soaking liquid at 50-100 ℃, and carrying out auxiliary ultrasound in the soaking process.
The salt content of marine raw materials is relatively high, so that salt is removed as much as possible to enhance the enzymolysis efficiency and reduce the salt content of the final product.
(4) Primary acidolysis: putting 100 parts by weight of the powder into 3-5 times of water by weight, boiling for 30min, cooling to 30-35 ℃, and adding 10-15 parts by weight of organic acid. The invention applies the step of preliminary acidolysis, and the preliminary acidolysis is carried out after the marine raw materials are boiled, thereby being beneficial to the microbial fermentation in the following steps.
(5) And (3) microbial fermentation degradation: heating the raw materials after primary acidolysis to 35-40 deg.C, adding Bacillus licheniformis, Bacillus bifidus and Bacillus subtilis strains 0.03-0.06 parts, stirring thoroughly, and fermenting for 1-2 days.
The invention applies the microbial fermentation to the preparation of biological calcium powder and improves the function and the efficacy, on one hand, the aim of decalcifying the raw material is achieved by separating out calcium element in the raw material by using the microbes, and simultaneously, various proteases and hydrolytic enzymes are generated by using related microbes in the fermentation process to further carry out enzymolysis on the raw material. For example, Bacillus licheniformis and Bacillus subtilis both produce various proteases, and the proteases produced during fermentation work together with the various enzymes added in step (6) below better hydrolyze the materials.
(6) Carrying out enzymolysis, namely heating the fermented material to inactivate bacteria, and then adding cathepsin and papain, wherein the weight of the cathepsin and the weight of the papain are respectively 0.5-2% and 1.5-3% of the weight of the material; maintaining the temperature at 30-50 deg.C, and stirring continuously; then heating to 80-90 ℃ to inactivate enzyme, then centrifuging and collecting supernatant.
(7) Amino acid compounding: adding 3-5 times of citric acid-sodium citrate buffer solution and 3-5 times of amino acid composite acid into the obtained supernatant, heating to 40-60 deg.C, and simultaneously performing ultrasonic treatment for 2-3 h. The invention selects a mode of combining amino acids to convert calcium into acid-calcium forms in various forms, thereby improving the bioavailability.
(8) And (3) drying: and (4) concentrating and drying the material obtained in the step (7) in vacuum at the absolute pressure of 0.06-0.2MPa and the temperature of 95-100 ℃ for 2-3 hours.
(9) Superfine grinding: pulverizing into 200 mesh granules, and sieving and packaging.
Preferably, the aquatic product leftovers of the invention are selected from shrimp shells, fishbones, crab shells and the like.
Preferably, (4) the organic acid in the preliminary acidolysis is selected from composite acids of citric acid, gluconic acid and malic acid, and the weight ratio of the three acids is 5:2-3: 1.
Preferably, the compound acid used in the amino acid compounding in the step (7) comprises tryptophan, phenylalanine, L-aspartic acid and glycine, and the weight ratio of the four acids is 1:2-5:3-7: 3-4.
Furthermore, in the preliminary acidolysis process in the step (4), in order to enhance the acidolysis effect, a certain guar gum solution can be added, guar gum can be used as a thickening agent in the food field, and in the invention, the guar gum is added to more tightly combine the cooked raw materials and the organic acid, so that a better acidolysis effect is achieved.
The invention has the beneficial effects that:
the marine calcium powder is prepared by using marine biological resources such as shrimp shells, crab shells, fishbones and the like through a preparation process of enzymolysis, organic acid and amino acid compounding, and has high bioavailability and good application prospect.
In the preparation process, the fermentation link is added, and the steps of enzymolysis and acidolysis which are alternately carried out are adopted, so that the extraction rate and the bioavailability of the biological calcium powder can be greatly improved.
Detailed Description
Example 1
The embodiment provides a preparation method for preparing marine-source amino acid composite calcium powder by using shrimp shells, which comprises the following steps:
(1) cleaning shrimp shells: washing shrimp shell with clear water for 3 times, and oven drying.
(2) Crushing: crushing the dried shrimp shells to obtain 20-mesh powder.
(3) Desalting: soaking the product powder obtained in the step (2) in water in a mass ratio of 1:5 for 40min, setting the temperature of the soaking liquid at 80 ℃, and performing ultrasonic assistance in the soaking process.
The salt content of marine raw materials is relatively high, so that salt is removed as much as possible to enhance the enzymolysis efficiency and reduce the salt content of the final product.
(4) Primary acidolysis: 100 parts by weight of the powder is put into 5 times of water by weight, boiled for 30min, cooled to 35 ℃, and added with 15 parts by weight of organic acid. After the marine raw materials are cooked, the marine raw materials are subjected to primary acidolysis, which is beneficial to microbial fermentation in the following steps.
(5) And (3) microbial fermentation degradation: heating the raw materials after the primary acidolysis to 40 ℃, adding 0.06 part of bacillus licheniformis, bifidobacterium and bacillus subtilis, fully and uniformly stirring, and fermenting for 1 day.
The microbial fermentation is applied to the preparation of biological calcium powder, the action and the effect of the biological calcium powder are improved, on one hand, the aim of decalcifying the raw material is achieved by separating out calcium element in the raw material by using the microbes, and meanwhile, various proteases and hydrolytic enzymes are generated by using related microbes in the fermentation process to further carry out enzymolysis on the raw material. For example, Bacillus licheniformis and Bacillus subtilis both produce various proteases, and the proteases produced during fermentation work together with the various enzymes added in step (6) below better hydrolyze the materials.
(6) Carrying out enzymolysis, namely heating the fermented material to inactivate bacteria, and then adding cathepsin and papain, wherein the weight of the cathepsin and the weight of the papain are respectively 2 percent and 3 percent of the weight of the material; maintaining the temperature at 50 ℃ and continuously stirring; then heating to 80-90 ℃ to inactivate enzyme, then centrifuging and collecting supernatant.
(7) Amino acid compounding: adding 5 times of citric acid-sodium citrate buffer solution and 5 times of amino acid composite acid into the obtained supernatant, heating to 60 ℃, and simultaneously performing ultrasonic treatment for 3 hours. The invention selects a mode of combining amino acids to convert calcium into acid-calcium forms in various forms, thereby improving the bioavailability.
(8) And (3) drying: and (4) concentrating and drying the material obtained in the step (7) in vacuum at the absolute pressure of 0.2MPa and the temperature of 95-100 ℃ for 3 hours.
(9) Superfine grinding: pulverizing into 200 mesh granules, and sieving and packaging.
(4) The organic acid in the preliminary acidolysis is selected from composite acid of citric acid, gluconic acid and malic acid, and the weight ratio of the three acids is 5:2: 1.
The compound acid used in the amino acid compounding in the step (7) comprises tryptophan, phenylalanine, L-aspartic acid and glycine, and the weight ratio of the four acids is 1:5:7: 4.
Further, in the primary acidolysis process in the step (4), in order to enhance the acidolysis effect, a certain amount of guar gum solution is added, and 5 parts by weight of guar gum solution with the mass concentration of 12% is added. Guar gum can be used as a thickening agent in the field of food, and in the invention, the addition of guar gum can more tightly combine the cooked raw material and organic acid, thereby having better acidolysis effect.
The calcium content of the product of the embodiment is determined by a flame atomic absorption method, the calcium content in the main component of the composite calcium powder reaches 45.3 percent, and the total amino acid content reaches 32.5 percent.
Example 2
The embodiment provides a preparation method for preparing marine-source amino acid compound calcium powder by using fishbones, which comprises the following steps:
(1) cleaning the fishbone: washing fishbone with clear water for 2 times, and oven drying.
(2) Crushing: crushing the dried fishbone to obtain 30-mesh powder.
(3) Desalting: soaking the product powder obtained in the step (2) in water in a mass ratio of 1:5 for 60min, setting the temperature of the soaking liquid at 90 ℃, and carrying out auxiliary ultrasound in the soaking process.
The salt content of marine raw materials is relatively high, so that salt is removed as much as possible to enhance the enzymolysis efficiency and reduce the salt content of the final product.
(4) Primary acidolysis: 100 parts by weight of the powder is put into 5 times of water by weight, boiled for 30min, cooled to 35 ℃, and 10 parts by weight of organic acid is added. After the marine raw materials are cooked, the marine raw materials are subjected to primary acidolysis, which is beneficial to microbial fermentation in the following steps.
(5) And (3) microbial fermentation degradation: heating the raw materials after the primary acidolysis to 40 ℃, adding 0.05 part of bacillus licheniformis, bifidobacterium and bacillus subtilis, fully and uniformly stirring, and fermenting for 2 days.
The microbial fermentation is applied to the preparation of biological calcium powder, the action and the effect of the biological calcium powder are improved, on one hand, the aim of decalcifying the raw material is achieved by separating out calcium element in the raw material by using the microbes, and meanwhile, various proteases and hydrolytic enzymes are generated by using related microbes in the fermentation process to further carry out enzymolysis on the raw material. For example, Bacillus licheniformis and Bacillus subtilis both produce various proteases, and the proteases produced during fermentation work together with the various enzymes added in step (6) below better hydrolyze the materials.
(6) Carrying out enzymolysis, namely heating the fermented material to inactivate bacteria, and then adding cathepsin and papain, wherein the weight of the cathepsin and the weight of the papain are respectively 1 percent and 2 percent of the weight of the material; maintaining the temperature at 40 ℃ and continuously stirring; then heating to 90 ℃ to inactivate enzyme, then centrifuging and collecting supernatant.
(7) Amino acid compounding: adding 5 times of citric acid-sodium citrate buffer solution and 5 times of amino acid composite acid into the obtained supernatant, heating to 60 ℃, and simultaneously performing ultrasonic treatment for 3 hours. The invention selects a mode of combining amino acids to convert calcium into acid-calcium forms in various forms, thereby improving the bioavailability.
(8) And (3) drying: and (4) concentrating and drying the material obtained in the step (7) in vacuum at the absolute pressure of 0.1MPa and the temperature of 100 ℃ for 3 hours.
(9) Superfine grinding: pulverizing into 200 mesh granules, and sieving and packaging.
(4) The organic acid in the preliminary acidolysis is selected from composite acid of citric acid, gluconic acid and malic acid, and the weight ratio of the three acids is 5:2: 1.
The compound acid used in the amino acid compounding in the step (7) comprises tryptophan, phenylalanine, L-aspartic acid and glycine, and the weight ratio of the four acids is 1:2:3: 3.
The calcium content of the product of the embodiment is measured by a flame atomic absorption method, the calcium content in the main component of the composite calcium powder reaches 39.2 percent, and the total amino acid content reaches 35.7 percent.
Example 3 bioabsorption utilization assay of biocomposite calcium prepared in accordance with the present invention:
the determination was performed using the complex calcium powder prepared in example 1. The determination of the bioabsorption utilization rate is carried out according to the report in the prior art, and in order to enhance the comparison effect of the bioabsorption utilization rate and the prior art, the optimization of the preparation process of the compound calcium powder in the shrimp shells and the evaluation of the absorption effect of rats which are published in food science by Zhang Wen Jing et al are carried out.
The specific experimental steps are as follows:
3.1 rat group
The average weight of 4-week-old weaned rats was 93g, and 100 rats with no significant difference in body weight were selected after 1 week of adaptive feeding with basal diet. The dosage of each group of calcium agents is calculated according to the calcium content in the composite calcium powder and the calcium carbonate, and the calcium agents are randomly divided into 5 groups: a low-calcium control group, a calcium carbonate control group, a compound calcium powder low-dose group, a medium-dose group and a high-dose group, wherein each group contains 20 calcium.
3.2 rat feeding mode
The low calcium control group was fed with a low calcium feed (low calcium feed formulation: casein 19.4%, corn starch 39.4%, soybean oil 10%, maltodextrin 13.6%, sucrose 8.7%, cellulose 5%, vitamin blend 1%, DL-methionine 0.1%, choline tartrate 0.25%, tert-butylhydroquinone 0.002%, mineral mix 2.5%, calcium 0.1%).
The low, medium and high dosage groups are filled with the compound calcium powder of low, medium and high dosage calcium every day on the basis of feeding the low-calcium feed for rats.
Gavage dose reference: 800 mg (adult body weight 60 kg) is converted into 13.3 mg/(kg. d), and the low, medium and high doses are 2, 5 and 10 times of the human body dose. The corresponding rat gavage calcium dosage is 26.6, 66.5 and 133 mg/(kg.d) (based on the calcium content and the weight of the rat). Each group of rats was fed in the same environment and fed freely, weighing 1 time per week. Each group of rats was fed in the same environment and fed freely, weighing 1 time per week.
3.3 evaluation of growth and calcium absorption effects of rat ingesting Complex calcium powder
During the feeding period, the experimental animals did not show diseases and death. The body quality and body length of each group of rats have no obvious difference at the initial stage of the experiment. After feeding for 3 weeks, rats with each dose of the compound calcium powder have good growth conditions. The quality of the rat body of each dosage group of the compound calcium powder is obviously higher than that of the rat body of the low-calcium control group. The growth index of the rats in the low-calcium control group is obviously lower than that of the rats in other dosage groups, and the hair color of the rats is dull and lusterless, and the rats are listless and slow to move. In particular to the influence of the compound calcium powder on the growth of rats shown in the table 1.
TABLE 1 Effect of Complex calcium powder on growth of rats
Claims (1)
1. A preparation method for preparing marine amino acid compound calcium powder by using shrimp shells comprises the following steps:
(1) cleaning shrimp shells: washing shrimp shell with clear water for 3 times, and drying;
(2) crushing: crushing the dried shrimp shells to obtain 20-mesh powder;
(3) desalting: soaking the product powder obtained in the step (2) in water in a mass ratio of 1:5 for 40min, setting the temperature of the soaking liquid at 80 ℃, and assisting ultrasonic treatment in the soaking process;
(4) primary acidolysis: putting 100 parts by weight of the powder into 5 times of water by weight, boiling for 30min, cooling to 35 ℃, and adding 15 parts by weight of organic acid;
(5) and (3) microbial fermentation degradation: heating the raw materials after the primary acidolysis to 40 ℃, adding 0.06 part of each of bacillus licheniformis, bifidobacterium and bacillus subtilis, fully and uniformly stirring, and fermenting for 1 day;
(6) carrying out enzymolysis, namely heating the fermented material to inactivate bacteria, and then adding cathepsin and papain, wherein the weight of the cathepsin and the weight of the papain are respectively 2 percent and 3 percent of the weight of the material; maintaining the temperature at 50 ℃ and continuously stirring; then heating to 80-90 ℃ to inactivate enzyme, centrifuging and collecting supernatant;
(7) amino acid compounding: adding 5 times of citric acid-sodium citrate buffer solution and 5 times of amino acid composite acid into the obtained supernatant, heating to 60 ℃, and simultaneously carrying out ultrasonic treatment for 3 hours;
(8) and (3) drying: concentrating and drying the material in the step (7) in vacuum at the absolute pressure of 0.2MPa and the temperature of 95-100 ℃ for 3 hours;
(9) superfine grinding: crushing into 200-mesh particles, and then screening and packaging;
the organic acid in the preliminary acidolysis in the step (4) is selected from composite acid of citric acid, gluconic acid and malic acid, and the weight ratio of the three acids is 5:2: 1;
the compound acid used in the amino acid compounding in the step (7) comprises tryptophan, phenylalanine, L-aspartic acid and glycine, and the weight ratio of the four acids is 1:5:7: 4;
in the primary acidolysis process in the step (4), in order to enhance the acidolysis effect, a certain amount of guar gum solution is added, and 5 parts by weight of guar gum solution with the mass concentration of 12% is added.
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