CN108354183A - The method for preparing the compound calcium powder of high-quality ocean source amino acid - Google Patents
The method for preparing the compound calcium powder of high-quality ocean source amino acid Download PDFInfo
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- CN108354183A CN108354183A CN201810043137.3A CN201810043137A CN108354183A CN 108354183 A CN108354183 A CN 108354183A CN 201810043137 A CN201810043137 A CN 201810043137A CN 108354183 A CN108354183 A CN 108354183A
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- Prior art keywords
- acid
- amino acid
- compound
- calcium powder
- calcium
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000011575 calcium Substances 0.000 title claims abstract description 79
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 78
- 150000001413 amino acids Chemical class 0.000 title claims abstract description 55
- 150000001875 compounds Chemical class 0.000 title claims abstract description 47
- 239000000843 powder Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000000855 fermentation Methods 0.000 claims abstract description 24
- 230000004151 fermentation Effects 0.000 claims abstract description 24
- 235000021190 leftovers Nutrition 0.000 claims abstract description 20
- 230000000813 microbial effect Effects 0.000 claims abstract description 14
- 150000007524 organic acids Chemical class 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 238000013329 compounding Methods 0.000 claims abstract description 11
- 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 abstract description 9
- 238000010612 desalination reaction Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 235000001014 amino acid Nutrition 0.000 claims description 50
- 239000000047 product Substances 0.000 claims description 35
- 239000000463 material Substances 0.000 claims description 20
- 230000000694 effects Effects 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 18
- 108091005804 Peptidases Proteins 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 16
- 102000004190 Enzymes Human genes 0.000 claims description 14
- 108090000790 Enzymes Proteins 0.000 claims description 14
- 229940088598 enzyme Drugs 0.000 claims description 14
- 238000010792 warming Methods 0.000 claims description 14
- 239000004365 Protease Substances 0.000 claims description 13
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 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
- 230000008569 process Effects 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000011260 aqueous acid Substances 0.000 claims description 8
- 239000000872 buffer Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 8
- 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 8
- 238000002525 ultrasonication Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 241000194108 Bacillus licheniformis Species 0.000 claims description 7
- 102000016943 Muramidase Human genes 0.000 claims description 7
- 108010014251 Muramidase Proteins 0.000 claims description 7
- 108010062010 N-Acetylmuramoyl-L-alanine Amidase Proteins 0.000 claims description 7
- 229960000274 lysozyme Drugs 0.000 claims description 7
- 239000004325 lysozyme Substances 0.000 claims description 7
- 235000010335 lysozyme Nutrition 0.000 claims description 7
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 4
- 244000063299 Bacillus subtilis Species 0.000 claims description 4
- 235000014469 Bacillus subtilis Nutrition 0.000 claims description 4
- 102000005600 Cathepsins Human genes 0.000 claims description 4
- 108010084457 Cathepsins Proteins 0.000 claims description 4
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 4
- 239000004471 Glycine Substances 0.000 claims description 4
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 claims description 4
- QIVBCDIJIAJPQS-VIFPVBQESA-N L-tryptophane Chemical compound C1=CC=C2C(C[C@H](N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-VIFPVBQESA-N 0.000 claims description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 4
- QIVBCDIJIAJPQS-UHFFFAOYSA-N Tryptophan Natural products C1=CC=C2C(CC(N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 239000002585 base Substances 0.000 claims description 4
- 235000015165 citric acid Nutrition 0.000 claims description 4
- 230000009849 deactivation Effects 0.000 claims description 4
- 239000001630 malic acid Substances 0.000 claims description 4
- 235000011090 malic acid Nutrition 0.000 claims description 4
- 238000004806 packaging method and process Methods 0.000 claims description 4
- 239000002245 particle Substances 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
- 238000012216 screening Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- 235000002906 tartaric acid Nutrition 0.000 claims description 4
- 241000238557 Decapoda Species 0.000 claims description 3
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 claims 1
- 241000235342 Saccharomycetes Species 0.000 claims 1
- 235000003704 aspartic acid Nutrition 0.000 claims 1
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 2
- 241000700159 Rattus Species 0.000 description 19
- 244000005700 microbiome Species 0.000 description 9
- 229920002907 Guar gum Polymers 0.000 description 6
- 239000000665 guar gum Substances 0.000 description 6
- 229960002154 guar gum Drugs 0.000 description 6
- 235000010417 guar gum Nutrition 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 230000037396 body weight Effects 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 241000143060 Americamysis bahia Species 0.000 description 3
- 241000193830 Bacillus <bacterium> Species 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 3
- 244000025254 Cannabis sativa Species 0.000 description 3
- 241000726221 Gemma Species 0.000 description 3
- 102000004157 Hydrolases Human genes 0.000 description 3
- 108090000604 Hydrolases Proteins 0.000 description 3
- 102000035195 Peptidases Human genes 0.000 description 3
- 230000003185 calcium uptake Effects 0.000 description 3
- 230000009920 chelation Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 229920001184 polypeptide Polymers 0.000 description 3
- 102000004196 processed proteins & peptides Human genes 0.000 description 3
- 108090000765 processed proteins & peptides Proteins 0.000 description 3
- 230000013777 protein digestion Effects 0.000 description 3
- 229940024999 proteolytic enzymes for treatment of wounds and ulcers Drugs 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- DWNBOPVKNPVNQG-LURJTMIESA-N (2s)-4-hydroxy-2-(propylamino)butanoic acid Chemical compound CCCN[C@H](C(O)=O)CCO DWNBOPVKNPVNQG-LURJTMIESA-N 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 2
- 244000003416 Asparagus officinalis Species 0.000 description 2
- 235000005340 Asparagus officinalis Nutrition 0.000 description 2
- 206010018910 Haemolysis Diseases 0.000 description 2
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000705 flame atomic absorption spectrometry Methods 0.000 description 2
- 230000008588 hemolysis Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002562 thickening agent Substances 0.000 description 2
- 230000003442 weekly effect Effects 0.000 description 2
- 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
- 208000017667 Chronic Disease Diseases 0.000 description 1
- 229920002261 Corn starch Polymers 0.000 description 1
- 244000303965 Cyamopsis psoralioides Species 0.000 description 1
- 239000004470 DL Methionine Substances 0.000 description 1
- 235000019733 Fish meal Nutrition 0.000 description 1
- 241000282412 Homo Species 0.000 description 1
- 239000005913 Maltodextrin Substances 0.000 description 1
- 229920002774 Maltodextrin Polymers 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
- 230000009471 action Effects 0.000 description 1
- 238000010171 animal model Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001669 calcium Chemical class 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
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000008120 corn starch Substances 0.000 description 1
- 229940099112 cornstarch Drugs 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000004467 fishmeal Substances 0.000 description 1
- 239000004459 forage Substances 0.000 description 1
- 238000003304 gavage Methods 0.000 description 1
- 230000037308 hair color Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229940035034 maltodextrin Drugs 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 238000005259 measurement Methods 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
- 239000000203 mixture Substances 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000003305 oral gavage Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 239000004250 tert-Butylhydroquinone Substances 0.000 description 1
- 235000019281 tert-butylhydroquinone Nutrition 0.000 description 1
- 235000013337 tricalcium citrate Nutrition 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 238000005303 weighing Methods 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
- A23L17/00—Food-from-the-sea products; Fish products; Fish meal; Fish-egg substitutes; Preparation or treatment thereof
-
- 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
- A23L33/17—Amino acids, peptides or proteins
- A23L33/175—Amino acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/14—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
- C07C227/18—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D209/02—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom condensed with one carbocyclic ring
- C07D209/04—Indoles; Hydrogenated indoles
- C07D209/10—Indoles; Hydrogenated indoles with substituted hydrocarbon radicals attached to carbon atoms of the hetero ring
- C07D209/18—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D209/20—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals substituted additionally by nitrogen atoms, e.g. tryptophane
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Nutrition Science (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Mycology (AREA)
- Zoology (AREA)
- Marine Sciences & Fisheries (AREA)
- Inorganic Chemistry (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Meat, Egg Or Seafood Products (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a kind of methods preparing the compound calcium powder of high-quality ocean source amino acid, include the following steps：（1）Aquatic product leftovers clean；（2）It is broken；（3）Desalination；（4）Preliminary acidolysis；（5）Microbial fermentation is degraded；（6）Amino acid tentatively compounds；（7）Enzymolysis；（8）The secondary compounding of amino acid；（9）It is dry；（10）Ultramicro grinding.Using living marine resources such as shrimp shell, crab shell, fish-bones marine organisms calcium powder is made, bioavailability is high, has a good application prospect by the preparation process of enzymolysis, organic acid, amino acid compounding in the present invention.The present invention increases fermenting step, while the step of alternateing progress using enzymolysis and acidolysis, can greatly improve the recovery rate and bioavailability of biological calcium powder in preparation process.
Description
Technical field
The present invention relates to a kind of methods preparing the compound calcium powder of high-quality ocean source amino acid, belong to biotechnology.
Background technology
Calcium is the essential element of human body, calcium nutrition condition and growth in humans's development in diet, angiocardiopathy and
Chronic disease is closely related, takes in enough calcium and is played an important role to improving osteoporosis symptoms, the product of calcium agent at present is main
It is divided into the classifications such as inorganic calcium, calcium of organic acid, amino acid calcium, research finds that the source of calcium is different, existence form difference is to the profit of calcium
There are larger difference, such as the peaks Wang Xiao with rate（2010）It is found Deng being compared to the calcium uptake situation of 8 kinds of calcium preparations in rats, fish-bone
The apparent absorptivity of calcium group preparation is better than animal calcium product up to 93%；Zhang Wenjing（2015）It is produced from shrimp shell Deng discovery
PHC-Ca has the effect for promoting calcium uptake, bioavailability to be better than the calcium citrate and shrimp shell meal of identical calcium content, because
This prepares calcium class product using living marine resources becomes the trend of development.
Along Zhejiang Coast marine resources are abundant, and especially shrimps, crab class, total fish catches are larger, however annual shrimp shell, crab shell,
The leftover bits and pieces such as fish-bone are not comprehensively utilized effectively, and the huge waste of resource is caused.Biological active calcium produces currently on the market
Product are less, and there is no formation scales, and the utilization of marine organism calcium is worse.
Zhejiang has most shrimps, crab class, the leftover bits and pieces shrimp shell of fish aquatic products processing enterprise, crab shell, fish-bone quantity very more, mesh
Front lower heel mainly with waste or the formal layout of low value fish meal, causes the huge waste of resource even to pollute environment, this
The researchs such as extraction, the product development of shrimp and crab shells marine organism calcium are carried out in invention, make " blue silo " to Zhejiang Province, promote ocean
Resource utilization and aquatic products processing sustainable development are of great significance：（1）The comprehensive utilization ratio of marine resources can be improved；
（2）Enrich current marine organism calcium product category, optimization calcium agent consumption market；（3）Promote the height of aquatic products processing calcium source leftover bits and pieces
Value.This project meets the strategy of ocean intensive processing industry, has important meaning to the construction of the current aquatic products processing industrial structure
Justice, while the research and development that can be utilized for the intensive processing of of the same trade, similar industry and Technique Popularizing play demonstration and driving role, it must
Huge economical, societal benefits will be generated.
Invention content
It is the method for using enzymolysis to prepare calcium powder all with marine feedstock in the prior art, and still, enzymolysis efficiency is low, acquisition
Calcium powder output capacity is low, and bioavailability is not high.The technical problem to be solved by the present invention is to：It provides and a kind of preparing high-quality ocean
The method of the compound calcium powder of source amino acid.
The method provided by the invention for preparing the compound calcium powder of high-quality ocean source amino acid, which is characterized in that including following
Step：
（1）Aquatic product leftovers clean：Aquatic product leftovers are cleaned 2-3 times with clear water, are then dried.
（2）It is broken：The aquatic product leftovers of drying are subjected to break process, obtain 10-30 mesh powders.
（3）Desalination：By step（2）The product powder of acquisition is with 1:The hydrochloric acid of a concentration of 0.5-1mol/L of 3-5 mass ratioes
Solution is impregnated, and 20-30min, soaking process assisting ultrasonic are impregnated.
In marine feedstock, salt content is relatively high, therefore to be eliminated as much as salinity, to enhance enzymolysis efficiency and drop
The salt content of low finished product.
（4）Preliminary acidolysis：The powder of 100 parts by weight is put into the water of 3-5 times of weight, while 10-15 weight is added
The organic acid of number, boils 30min, is cooled to 30-35 DEG C, maintains 3-5h.
The step of invention applies preliminary acidolysis carries out preliminary acidolysis after marine feedstock is cooked, and is conducive to later step
Microbial fermentation.
（5）Microbial fermentation is degraded：Raw material after preliminary acidolysis is warming up to 35-40 DEG C, bacillus licheniformis, ferment is added
0.03-0.06 parts of female bacterium and Bacillus subtilis strain, are fully mixed thoroughly, are fermented 1-2 days.
Microbial fermentation is applied in the preparation of biological calcium powder by the present invention, and its perfect effect and effect, on the one hand
It is that the calcium constituent in raw material is precipitated using microorganism, that is, achievees the purpose that raw material decalcification, meanwhile, existed using relevant microorganism
Various protease and hydrolase are generated in fermentation process, further digest raw material.For example, bacillus licheniformis and withered grass gemma
Bacillus can generate various protease, the protease and following step that fermentation process generates（6）The various enzymes of middle addition
One piece preferably digests raw material.
（6）Amino acid tentatively compounds：1-2 times of citric acid-sodium citrate buffer is added in the material that fermentation is obtained
The compound aqueous acid of amino acid with 1-3 times, is warming up to 40-60 DEG C, while ultrasonication 1-2h.
For increase amino acid and calcium source chelation percent, the present invention using two steps compound the step of, adopted after microbial fermentation
It is compounded with an amino acid, compounds primary, increase amino acid and the chelating probability that calcium is precipitated again after enzymolysis.
（7）Enzymolysis:Alkali protease, cathepsin and lysozyme are added in the material after amino acid tentatively compounds,
The weight of three kinds of enzymes is respectively 1.5-3%, 0.5-2% and 0.05-0.5% of weight of material；Temperature maintains 30-40 DEG C, maintains
Then time 2-5h is warming up to 80-90 DEG C of enzyme deactivation activity, is then centrifuged for, collect supernatant.
Three kinds of enzymes that the present invention selects, can by the protein digestion in aquatic product leftovers be polypeptide and amino acid, together
When, lysozyme can digest the microorganism in material, release more proteolytic enzymes.
（8）The secondary compounding of amino acid：By obtained supernatant be added 3-5 times citric acid-sodium citrate buffer with
3-5 times of the compound aqueous acid of amino acid, is warming up to 40-70 DEG C, while ultrasonication 2-3h.
（9）It is dry：By step（8）Material using drying is concentrated in vacuo, absolute pressure 0.06-0.2MPa, temperature is
It is 95-100 DEG C, 1-2 hours dry.
（10）Ultramicro grinding：It is ground into the particle of 200 mesh, then screening packaging.
Preferably, aquatic product leftovers are selected from shrimp shell, shrimp head, fish-bone, crab shell etc..
Preferably,（4）Organic acid in preliminary acidolysis is selected from the Compound-acid of citric acid, tartaric acid, malic acid, and three kinds sour
Weight ratio 5:2-3:1.
Preferably, step（6）And step（8）Compound-acid in middle amino acid compounding includes tryptophan, phenylalanine, L-
Asparatate and glycine, four kinds of sour weight ratios are 1:2-5:3-7:The mass percent of 3-4, Ammonia In Aqueous Solution base acid is
20-35%。
Further, in step（4）In preliminary acid hemolysis process, in order to enhance acidolysis effect, certain Guar can be added
Sol solution, guar gum can be used as thickener in field of food, in the present invention, the raw material after guar gum can will be cooked be added
The closer combination with organic acid, plays better acidolysis effect.
The beneficial effects of the invention are as follows：
The present invention passes through the preparation work of enzymolysis, organic acid, amino acid compounding using living marine resources such as shrimp shell, crab shell, fish-bones
Marine organisms calcium powder is made in skill, and bioavailability is high, has a good application prospect.
The present invention increases fermenting step, while the step of alternateing progress using enzymolysis and acidolysis in preparation process,
The recovery rate and bioavailability of biological calcium powder can be greatly improved.
Specific implementation mode
Embodiment 1
The present embodiment provides a kind of methods preparing the compound calcium powder of high-quality ocean source amino acid using shrimp shell, including following step
Suddenly：
（1）Aquatic product leftovers clean：Aquatic product leftovers are cleaned 3 times with clear water, are then dried.
（2）It is broken：The aquatic product leftovers of drying are subjected to break process, obtain 30 mesh powders.
（3）Desalination：By step（2）The product powder of acquisition is with 1:The hydrochloric acid solution of a concentration of 1mol/L of 5 mass ratioes into
Row impregnates, and impregnates 30min, soaking process assisting ultrasonic.
In marine feedstock, salt content is relatively high, therefore to be eliminated as much as salinity, to enhance enzymolysis efficiency and drop
The salt content of low finished product.
（4）Preliminary acidolysis：The powder of 100 parts by weight is put into the water of 5 times of weight, while 15 parts by weight are added
Organic acid boils 30min, is cooled to 35 DEG C, maintains 5h.
The step of invention applies preliminary acidolysis carries out preliminary acidolysis after marine feedstock is cooked, and is conducive to later step
Microbial fermentation.
（5）Microbial fermentation is degraded：Raw material after preliminary acidolysis is warming up to 40 DEG C, bacillus licheniformis, yeast is added
Bacterium and each 0.06 part of Bacillus subtilis strain, are fully mixed thoroughly, are fermented 2 days.
Microbial fermentation is applied in the preparation of biological calcium powder by the present invention, and its perfect effect and effect, on the one hand
It is that the calcium constituent in raw material is precipitated using microorganism, that is, achievees the purpose that raw material decalcification, meanwhile, existed using relevant microorganism
Various protease and hydrolase are generated in fermentation process, further digest raw material.For example, bacillus licheniformis and withered grass gemma
Bacillus can generate various protease, the protease and following step that fermentation process generates（6）The various enzymes of middle addition
One piece preferably digests raw material.
（6）Amino acid tentatively compounds：2 times of citric acid-sodium citrate buffer and 2 is added in the material that fermentation is obtained
The compound aqueous acid of amino acid again, is warming up to 60 DEG C, while ultrasonication 2h.
For increase amino acid and calcium source chelation percent, the present invention using two steps compound the step of, adopted after microbial fermentation
It is compounded with an amino acid, compounds primary, increase amino acid and the chelating probability that calcium is precipitated again after enzymolysis.
（7）Enzymolysis:Alkali protease, cathepsin and lysozyme are added in the material after amino acid tentatively compounds,
The weight of three kinds of enzymes is respectively 3%, 1% and the 0.5% of weight of material；Temperature maintains 40 DEG C, and hold time 5h, then heats up
It to 90 DEG C of enzyme deactivation activity, is then centrifuged for, collects supernatant.
Three kinds of enzymes that the present invention selects, can by the protein digestion in aquatic product leftovers be polypeptide and amino acid, together
When, lysozyme can digest the microorganism in material, release more proteolytic enzymes.
（8）The secondary compounding of amino acid：By obtained supernatant be added 5 times citric acid-sodium citrate buffer and 5 times
The compound aqueous acid of amino acid, be warming up to 60 DEG C, while ultrasonication 3h.
（9）It is dry：By step（8）Material using be concentrated in vacuo drying, absolute pressure 0.2MPa, temperature be 100 DEG C,
It is 1.5 hours dry.
（10）Ultramicro grinding：It is ground into the particle of 200 mesh, then screening packaging.
（4）Organic acid in preliminary acidolysis is selected from the Compound-acid of citric acid, tartaric acid, malic acid, three kinds of sour weight ratios
Example 2-1.
Step（6）And step（8）Compound-acid in middle amino acid compounding includes tryptophan, phenylalanine, L- lucid asparagus
Propylhomoserin and glycine, four kinds of sour weight ratios are 1:3:5:4, the mass percent of Ammonia In Aqueous Solution base acid is 35%.
In step（4）In preliminary acid hemolysis process, in order to enhance acidolysis effect, certain guar gum solution is added, 5 weights are added
Guar gum solution that measure number, that mass concentration is 12%.Guar gum can be used as thickener in field of food, in the present invention
In, be added guar gum can will it is cooked after raw material and the closer combination of organic acid, play better acidolysis effect.
Using the calcium content of flame atomic absorption spectrometry the present embodiment product, calcium content reaches in compound calcium powder main component
To 51.4%, total amino acid amount reaches 43.8%.
Embodiment 2
The present embodiment provides a kind of methods preparing the compound calcium powder of high-quality ocean source amino acid using fish-bone, including following step
Suddenly：
（1）Aquatic product leftovers clean：Aquatic product leftovers are cleaned 2 times with clear water, are then dried.
（2）It is broken：The aquatic product leftovers of drying are subjected to break process, obtain 20 mesh powders.
（3）Desalination：By step（2）The product powder of acquisition is with 1:The hydrochloric acid solution of a concentration of 1mol/L of 4 mass ratioes into
Row impregnates, and impregnates 20-30min, soaking process assisting ultrasonic.
In marine feedstock, salt content is relatively high, therefore to be eliminated as much as salinity, to enhance enzymolysis efficiency and drop
The salt content of low finished product.
（4）Preliminary acidolysis：The powder of 100 parts by weight is put into the water of 4 times of weight, while 15 parts by weight are added
Organic acid boils 30min, is cooled to 35 DEG C, maintains 5h.
The step of invention applies preliminary acidolysis carries out preliminary acidolysis after marine feedstock is cooked, and is conducive to later step
Microbial fermentation.
（5）Microbial fermentation is degraded：Raw material after preliminary acidolysis is warming up to 40 DEG C, bacillus licheniformis, yeast is added
Bacterium and each 0.06 part of Bacillus subtilis strain, are fully mixed thoroughly, are fermented 2 days.
Microbial fermentation is applied in the preparation of biological calcium powder by the present invention, and its perfect effect and effect, on the one hand
It is that the calcium constituent in raw material is precipitated using microorganism, that is, achievees the purpose that raw material decalcification, meanwhile, existed using relevant microorganism
Various protease and hydrolase are generated in fermentation process, further digest raw material.For example, bacillus licheniformis and withered grass gemma
Bacillus can generate various protease, the protease and following step that fermentation process generates（6）The various enzymes of middle addition
One piece preferably digests raw material.
（6）Amino acid tentatively compounds：2 times of citric acid-sodium citrate buffer and 3 is added in the material that fermentation is obtained
The compound aqueous acid of amino acid again, is warming up to 60 DEG C, while ultrasonication 2h.
For increase amino acid and calcium source chelation percent, the present invention using two steps compound the step of, adopted after microbial fermentation
It is compounded with an amino acid, compounds primary, increase amino acid and the chelating probability that calcium is precipitated again after enzymolysis.
（7）Enzymolysis:Alkali protease, cathepsin and lysozyme are added in the material after amino acid tentatively compounds,
The weight of three kinds of enzymes is respectively 3%, 2% and the 0.5% of weight of material；Temperature maintains 40 DEG C, and hold time 4h, then heats up
It to 890 DEG C of enzyme deactivation activity, is then centrifuged for, collects supernatant.
Three kinds of enzymes that the present invention selects, can by the protein digestion in aquatic product leftovers be polypeptide and amino acid, together
When, lysozyme can digest the microorganism in material, release more proteolytic enzymes.
（8）The secondary compounding of amino acid：By obtained supernatant be added 5 times citric acid-sodium citrate buffer and 5 times
The compound aqueous acid of amino acid, be warming up to 70 DEG C, while ultrasonication 2-3h.
（9）It is dry：By step（8）Material using be concentrated in vacuo drying, absolute pressure 0.2MPa, temperature be 100 DEG C,
It is 2 hours dry.
（10）Ultramicro grinding：It is ground into the particle of 200 mesh, then screening packaging.
（4）Organic acid in preliminary acidolysis is selected from the Compound-acid of citric acid, tartaric acid, malic acid, three kinds of sour weight ratios
Example 5:2-3:1.
Step（6）And step（8）Compound-acid in middle amino acid compounding includes tryptophan, phenylalanine, L- lucid asparagus
Propylhomoserin and glycine, four kinds of sour weight ratios are 1:5:3:3, the mass percent of Ammonia In Aqueous Solution base acid is 35%.
Using the calcium content of flame atomic absorption spectrometry the present embodiment product, calcium content reaches in compound calcium powder main component
To 43.6%, total amino acid amount reaches 39.8%.
The bio-absorbable of biological composite calcium prepared by 3 present invention of embodiment utilizes measurement：
The compound calcium powder prepared using embodiment 1 is measured.The bio-absorbable utilization rate of the present invention is measured according to the prior art
In report carry out, for the enhancing present invention and the contrast effect of the prior art, delivered in Food Science according to Zhang Wenjing etc.《Shrimp
The evaluation of the optimum preparation condition of compound calcium powder and rat to its assimilation effect in shell》.
Steps are as follows for specific experiment：
3.1 rat groups
4 week old weaning rats, average weight 83g select body weight after basal feed adaptable fed 1 week after weighing
The rat that there was no significant difference 100.Each group calcium agent dosage is calculated according to the calcium content in the compound calcium powder of the present invention and calcium carbonate,
It is randomly divided into 5 groups：Low calcium control group, calcium carbonate control group, compound calcium powder low dose group, middle dose group and high dose group, every group
20.
3.2 rat feeding patterns
Low calcium control group is with low calcium forage feed（Low calcium feed formula：Casein 19.4%, cornstarch 39.4%, soybean oil
10%, maltodextrin 13.6%, sucrose 8.7%, cellulose 5%, mixed vitamin 1%, DL- METHIONINE 0.1%, choline tartrate
0.25%, tert-butylhydroquinone 0.002%, mineral mixture 2.5%, calcium 0.1%）.
Low, middle and high dose groups rat feed low calcium feed on the basis of, the daily basic, normal, high dosage calcium of gavage it is compound
Calcium powder.
Given low reference：800 mg（60 kg of body weight of being grown up）It is converted into 13.3 mg/（kg·d）, basic, normal, high dose
Amount is 2,5,10 times of human dose.Correspond to rat oral gavage calcium dosage be 26.6,66.5,133mg/（kg·d）（Contained with calcium
Amount and rat body weight gauge）.Each group rat is fed under identical environment, ad lib, claims 1 body weight weekly.Each group rat
It is fed under identical environment, ad lib, claims 1 body weight weekly.
3.3 rats take in evaluation of the compound calcium powder to growth and calcium uptake effect
During raising, experimental animal does not occur disease and death.Experiment initial stage each group rat weight, height no significant difference.
After feeding 3 weeks, compound each dosage Growth in Rats of calcium powder is all right.Compound each dosage group rat weight of calcium powder is all remarkably higher than
Low calcium control group.Low calcium control rats growth indexes are significantly lower than other dosage groups, and the intensely dark pool of rat hair color, tired at this time
It is idle to be slow in action.Specific such as influence of the 1 compound calcium powder of table to Growth in Rats.
Influence of the 1 compound calcium powder of table to Growth in Rats
Claims (4)
1. the method for preparing the compound calcium powder of high-quality ocean source amino acid, which is characterized in that include the following steps：
（1）Aquatic product leftovers clean：Aquatic product leftovers are cleaned 2-3 times with clear water, are then dried；
（2）It is broken：The aquatic product leftovers of drying are subjected to break process, obtain 10-30 mesh powders；
（3）Desalination：By step（2）The product powder of acquisition is with 1:The hydrochloric acid solution of a concentration of 0.5-1mol/L of 3-5 mass ratioes
It is impregnated, impregnates 20-30min, soaking process assisting ultrasonic；
（4）Preliminary acidolysis：The powder of 100 parts by weight is put into the water of 3-5 times of weight, while 10-15 parts by weight are added
Organic acid, boil 30min, be cooled to 30-35 DEG C, maintain 3-5h；
（5）Microbial fermentation is degraded：Raw material after preliminary acidolysis is warming up to 35-40 DEG C, bacillus licheniformis, saccharomycete is added
It with 0.03-0.06 parts of Bacillus subtilis strain, fully mixes thoroughly, ferments 1-2 days；
（6）Amino acid tentatively compounds：1-2 times of citric acid-sodium citrate buffer and 1-3 is added in the material that fermentation is obtained
The compound aqueous acid of amino acid again, is warming up to 40-60 DEG C, while ultrasonication 1-2h；
（7）Enzymolysis:Addition alkali protease, cathepsin and lysozyme in the material after amino acid tentatively compounds, three kinds
The weight of enzyme is respectively 1.5-3%, 0.5-2% and 0.05-0.5% of weight of material；Temperature maintains 30-40 DEG C, holds time
Then 2-5h is warming up to 80-90 DEG C of enzyme deactivation activity, is then centrifuged for, collect supernatant；
（8）The secondary compounding of amino acid：By obtained supernatant be added 3-5 times citric acid-sodium citrate buffer and 3-5 times
The compound aqueous acid of amino acid, be warming up to 40-70 DEG C, while ultrasonication 2-3h；
（9）It is dry：By step（8）Material using be concentrated in vacuo drying, absolute pressure 0.06-0.2MPa, temperature 95-
It is 100 DEG C, 1-2 hours dry；
（10）Ultramicro grinding：It is ground into the particle of 200 mesh, then screening packaging.
2. the preparation method of the compound calcium powder of ocean source according to claim 1 amino acid, which is characterized in that aquatic products are got a foothold
Material is selected from shrimp shell, shrimp head, fish-bone, crab shell etc..
3. the preparation method of the compound calcium powder of ocean source according to claim 1 amino acid, which is characterized in that（4）Preliminary acid
Organic acid in solution is selected from the Compound-acid of citric acid, tartaric acid, malic acid, three kinds of sour weight ratio 5:2-3:1.
4. the preparation method of the compound calcium powder of ocean source according to claim 1 amino acid, which is characterized in that step（6）With
Step（8）Compound-acid in middle amino acid compounding includes tryptophan, phenylalanine, ASPARTIC ACID and glycine, four kinds
The weight ratio of acid is 1:2-5:3-7:The mass percent of 3-4, Ammonia In Aqueous Solution base acid are 20-35%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109820200A (en) * | 2019-03-19 | 2019-05-31 | 湖南文理学院 | A kind of preparation method of amino acid chelated calcium type shrimp paste |
| CN111466499A (en) * | 2020-05-06 | 2020-07-31 | 青岛卓越海洋集团有限公司 | Application of chlorella in preparation of fish culture feed |
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|---|---|---|---|---|
| CN101220383B (en) * | 2008-01-18 | 2010-06-02 | 中国水产科学研究院南海水产研究所 | Method for producing calcium amino acid |
| CN107095309A (en) * | 2017-04-27 | 2017-08-29 | 温州科技职业学院 | Marine organisms composite calcium powder, preparation method thereof |
| CN107095198A (en) * | 2017-04-27 | 2017-08-29 | 温州科技职业学院 | The quick method for preparing biological compound calcium powder |
| CN107485030A (en) * | 2017-07-31 | 2017-12-19 | 浦江县昂宝生物技术有限公司 | A kind of low value fish-bone polypeptide chelate calcium |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220383B (en) * | 2008-01-18 | 2010-06-02 | 中国水产科学研究院南海水产研究所 | Method for producing calcium amino acid |
| CN107095309A (en) * | 2017-04-27 | 2017-08-29 | 温州科技职业学院 | Marine organisms composite calcium powder, preparation method thereof |
| CN107095198A (en) * | 2017-04-27 | 2017-08-29 | 温州科技职业学院 | The quick method for preparing biological compound calcium powder |
| CN107485030A (en) * | 2017-07-31 | 2017-12-19 | 浦江县昂宝生物技术有限公司 | A kind of low value fish-bone polypeptide chelate calcium |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109820200A (en) * | 2019-03-19 | 2019-05-31 | 湖南文理学院 | A kind of preparation method of amino acid chelated calcium type shrimp paste |
| CN111466499A (en) * | 2020-05-06 | 2020-07-31 | 青岛卓越海洋集团有限公司 | Application of chlorella in preparation of fish culture feed |
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