CN108014136B - Preparation and application of squid ink melanin-chelated calcium tablets - Google Patents
Preparation and application of squid ink melanin-chelated calcium tablets Download PDFInfo
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- CN108014136B CN108014136B CN201710858914.5A CN201710858914A CN108014136B CN 108014136 B CN108014136 B CN 108014136B CN 201710858914 A CN201710858914 A CN 201710858914A CN 108014136 B CN108014136 B CN 108014136B
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 239000011575 calcium Substances 0.000 title claims abstract description 72
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 71
- 241000238366 Cephalopoda Species 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- XUMBMVFBXHLACL-UHFFFAOYSA-N Melanin Chemical compound O=C1C(=O)C(C2=CNC3=C(C(C(=O)C4=C32)=O)C)=C2C4=CNC2=C1C XUMBMVFBXHLACL-UHFFFAOYSA-N 0.000 claims abstract description 92
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 42
- 229920001184 polypeptide Polymers 0.000 claims description 30
- 108090000765 processed proteins & peptides Proteins 0.000 claims description 30
- 102000004196 processed proteins & peptides Human genes 0.000 claims description 30
- 229910052742 iron Inorganic materials 0.000 claims description 21
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 15
- LJCWONGJFPCTTL-SSDOTTSWSA-N D-4-hydroxyphenylglycine Chemical compound [O-]C(=O)[C@H]([NH3+])C1=CC=C(O)C=C1 LJCWONGJFPCTTL-SSDOTTSWSA-N 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000002244 precipitate Substances 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- 239000008187 granular material Substances 0.000 claims description 10
- 239000007779 soft material Substances 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 230000003301 hydrolyzing effect Effects 0.000 claims description 9
- 235000019359 magnesium stearate Nutrition 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 8
- 239000000945 filler Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 108090000145 Bacillolysin Proteins 0.000 claims description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 5
- 108091005507 Neutral proteases Proteins 0.000 claims description 5
- 102000035092 Neutral proteases Human genes 0.000 claims description 5
- 239000004677 Nylon Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 229930003316 Vitamin D Natural products 0.000 claims description 5
- QYSXJUFSXHHAJI-XFEUOLMDSA-N Vitamin D3 Natural products C1(/[C@@H]2CC[C@@H]([C@]2(CCC1)C)[C@H](C)CCCC(C)C)=C/C=C1\C[C@@H](O)CCC1=C QYSXJUFSXHHAJI-XFEUOLMDSA-N 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 5
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 5
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 5
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 5
- 235000013372 meat Nutrition 0.000 claims description 5
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 5
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 5
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229920001778 nylon Polymers 0.000 claims description 5
- 239000000741 silica gel Substances 0.000 claims description 5
- 229910002027 silica gel Inorganic materials 0.000 claims description 5
- 235000019166 vitamin D Nutrition 0.000 claims description 5
- 239000011710 vitamin D Substances 0.000 claims description 5
- 150000003710 vitamin D derivatives Chemical class 0.000 claims description 5
- 229940046008 vitamin d Drugs 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 claims description 4
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 4
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 claims description 4
- 229920001353 Dextrin Polymers 0.000 claims description 4
- 239000004375 Dextrin Substances 0.000 claims description 4
- 239000004384 Neotame Substances 0.000 claims description 4
- 229930006000 Sucrose Natural products 0.000 claims description 4
- 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 claims description 4
- 210000001015 abdomen Anatomy 0.000 claims description 4
- 235000019425 dextrin Nutrition 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 229940041616 menthol Drugs 0.000 claims description 4
- HLIAVLHNDJUHFG-HOTGVXAUSA-N neotame Chemical compound CC(C)(C)CCN[C@@H](CC(O)=O)C(=O)N[C@H](C(=O)OC)CC1=CC=CC=C1 HLIAVLHNDJUHFG-HOTGVXAUSA-N 0.000 claims description 4
- 235000019412 neotame Nutrition 0.000 claims description 4
- 108010070257 neotame Proteins 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 102000004169 proteins and genes Human genes 0.000 claims description 4
- 108090000623 proteins and genes Proteins 0.000 claims description 4
- 239000000600 sorbitol Substances 0.000 claims description 4
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 3
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 3
- 229930195725 Mannitol Natural products 0.000 claims description 3
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 claims description 3
- 235000019700 dicalcium phosphate Nutrition 0.000 claims description 3
- 239000000594 mannitol Substances 0.000 claims description 3
- 235000010355 mannitol Nutrition 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- 229920002472 Starch Polymers 0.000 claims description 2
- 239000008101 lactose Substances 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 15
- 230000036039 immunity Effects 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 10
- 239000003963 antioxidant agent Substances 0.000 abstract description 9
- 230000003078 antioxidant effect Effects 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 6
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 6
- 230000000840 anti-viral effect Effects 0.000 abstract description 6
- 230000007760 free radical scavenging Effects 0.000 abstract description 6
- 210000004185 liver Anatomy 0.000 abstract description 6
- 229910052725 zinc Inorganic materials 0.000 abstract description 6
- 239000011701 zinc Substances 0.000 abstract description 6
- 239000003814 drug Substances 0.000 abstract description 5
- 239000008280 blood Substances 0.000 abstract description 4
- 210000004369 blood Anatomy 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract description 4
- 239000013589 supplement Substances 0.000 abstract description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 3
- 210000004556 brain Anatomy 0.000 abstract description 3
- 229910052802 copper Inorganic materials 0.000 abstract description 3
- 239000010949 copper Substances 0.000 abstract description 3
- 210000003734 kidney Anatomy 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 10
- 210000000988 bone and bone Anatomy 0.000 description 10
- 229910001424 calcium ion Inorganic materials 0.000 description 10
- 102000004190 Enzymes Human genes 0.000 description 9
- 108090000790 Enzymes Proteins 0.000 description 9
- 235000006708 antioxidants Nutrition 0.000 description 7
- 230000009920 chelation Effects 0.000 description 7
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 6
- 108010009736 Protein Hydrolysates Proteins 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 239000000049 pigment Substances 0.000 description 5
- 238000009776 industrial production Methods 0.000 description 4
- 231100000331 toxic Toxicity 0.000 description 4
- 230000002588 toxic effect Effects 0.000 description 4
- YCCILVSKPBXVIP-UHFFFAOYSA-N 2-(4-hydroxyphenyl)ethanol Chemical compound OCCC1=CC=C(O)C=C1 YCCILVSKPBXVIP-UHFFFAOYSA-N 0.000 description 3
- 108091005658 Basic proteases Proteins 0.000 description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 3
- 235000010323 ascorbic acid Nutrition 0.000 description 3
- 229960005070 ascorbic acid Drugs 0.000 description 3
- 239000011668 ascorbic acid Substances 0.000 description 3
- 239000001362 calcium malate Substances 0.000 description 3
- 229940016114 calcium malate Drugs 0.000 description 3
- 235000011038 calcium malates Nutrition 0.000 description 3
- QXDHJHQRJCJRAU-UHFFFAOYSA-N calcium;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical compound [Ca].OC(=O)CC(O)(C(O)=O)CC(O)=O QXDHJHQRJCJRAU-UHFFFAOYSA-N 0.000 description 3
- 239000013522 chelant Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000796 flavoring agent Substances 0.000 description 3
- 235000019634 flavors Nutrition 0.000 description 3
- 238000004108 freeze drying Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000000415 inactivating effect Effects 0.000 description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 229960004793 sucrose Drugs 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229920001222 biopolymer Polymers 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000004080 punching Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000010736 Chelating Activity Effects 0.000 description 1
- 229910001262 Ferralium Inorganic materials 0.000 description 1
- 208000003076 Osteolysis Diseases 0.000 description 1
- 102000003425 Tyrosinase Human genes 0.000 description 1
- 108060008724 Tyrosinase Proteins 0.000 description 1
- 229920001284 acidic polysaccharide Polymers 0.000 description 1
- 150000004805 acidic polysaccharides Chemical class 0.000 description 1
- 125000004442 acylamino group Chemical group 0.000 description 1
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- 210000001124 body fluid Anatomy 0.000 description 1
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- 230000037396 body weight Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
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- 208000029791 lytic metastatic bone lesion Diseases 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- 210000003205 muscle Anatomy 0.000 description 1
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- 231100000956 nontoxicity Toxicity 0.000 description 1
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
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- 239000002700 tablet coating Substances 0.000 description 1
- 238000009492 tablet coating Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
- A61K35/56—Materials from animals other than mammals
- A61K35/618—Molluscs, e.g. fresh-water molluscs, oysters, clams, squids, octopus, cuttlefish, snails or slugs
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/06—Aluminium, calcium or magnesium; Compounds thereof, e.g. clay
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/20—Pills, tablets, discs, rods
- A61K9/2004—Excipients; Inactive ingredients
- A61K9/2022—Organic macromolecular compounds
- A61K9/205—Polysaccharides, e.g. alginate, gums; Cyclodextrin
- A61K9/2059—Starch, including chemically or physically modified derivatives; Amylose; Amylopectin; Dextrin
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Epidemiology (AREA)
- Medicinal Chemistry (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Pharmacology & Pharmacy (AREA)
- Marine Sciences & Fisheries (AREA)
- Zoology (AREA)
- Inorganic Chemistry (AREA)
- Medicinal Preparation (AREA)
- Medicines That Contain Protein Lipid Enzymes And Other Medicines (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
The invention discloses a preparation method of a squid ink melanin chelated calcium tablet, which comprises the following steps: the squid melanin chelated calcium tablet can be swallowed or chewed or eaten, and is suitable for people of multiple ages to eat. The beneficial effects are that: the effective calcium component in the tablet has high content, and can be easily absorbed by human body, and melanin has antibacterial and antiviral activity, and also has strong antioxidant and free radical scavenging effects, and can enhance immunity of human body; the calcium tablet has good taste, good stability and strong disintegration effect, and can accelerate the dissolution of the medicine; the production process is feasible, the quality is controllable, and the method is suitable for industrial mass production; the tablet can supplement calcium, enhance immunity by regulating steady state of antioxidant system, has certain effect in removing lead from blood lead and liver lead, and can protect copper in liver, zinc in kidney and zinc in brain.
Description
Technical Field
The invention relates to the field of preparation and application of tablets, in particular to preparation and application of squid melanin-chelated calcium tablets.
Technical Field
Calcium is an essential element for living beings. Ca is useful in human body in muscle, nerve, body fluid and bone2+A bound protein. Calcium is the main inorganic component of human bone and teeth, and is also an essential element for neurotransmission, muscle contraction, blood coagulation, hormone release, milk secretion and the like. Calcium participates in metabolism and must be supplemented every day; the deficiency or excess of calcium in human body can affect growth and health. Calcium is the most abundant inorganic salt component in human body, and the total amount of calcium in healthy adult is about 1000-1300 g, and about 1.5% -2.0% of body weight, wherein 99% of calcium exists in bone salt form in bone and teeth, and the rest is distributed in soft tissue, and calcium in extracellular fluid only accounts for 0.1% of total calcium. Bone is the main site of calcium deposition, soIt is called "calcium pool". Bone calcium exists mainly in two forms of amorphous calcium hydrogen phosphate and crystalline hydroxyapatite, and its composition and physical and chemical properties change with physiological or pathological conditions of human body. More calcium hydrogen phosphate is contained in the new bone than the old bone, and the bone is gradually changed into hydroxyapatite in the process of maturing. The bone keeps dynamic balance of bone calcium and blood calcium through continuous osteogenesis and osteolysis.
The name biopolymer contained in squid ink is the only natural endogenous biopolymer known to protect organisms from radiation. Contains polypeptide fragment, acidic polysaccharide, tyrosinase, etc. Has the characteristics of scavenging free radicals and binding potential toxic ions (such as some transition metals), and has great application potential. The squid melanin belongs to natural melanin, contains functional groups such as hydroxyl, carboxyl, amino or acylamino and the like, and has better metal ion chelating activity.
The invention discloses a citric acid calcium malate drug tablet, which is prepared by directly tabletting raw material powder of citric acid calcium malate into a tablet, has the characteristics of high solubility, high absorption and utilization, no influence on iron absorption of a human body, safety, no toxicity and no damage on acid-base balance of gastrointestinal tracts, but has no sweet taste and poor mouthfeel because the tablet is only prepared from the citric acid calcium malate, and is easy to absorb moisture and deteriorate and has influence on quality because the tablet does not contain any coating material.
Disclosure of Invention
The method aims to provide preparation and application of the squid ink melanin-chelated calcium tablet, the squid ink melanin-chelated calcium is used as a tablet material, the tablet is high in stability and calcium absorption rate, and the tablet also has the effects of resisting oxidation and enhancing immunity.
Aiming at the problems mentioned in the background technology, the invention adopts the technical scheme that: preparation and application of squid ink melanin-chelated calcium tablets comprise: the preparation method comprises the following steps of obtaining melanin from ink, preparing polypeptide chelated iron, preparing polypeptide chelated calcium, preparing tablets and applying the tablets, and specifically comprises the following steps:
obtaining black pigment: cutting open the abdomen of the squid body, taking out an ink sac, cutting off a sac membrane, extruding ink, soaking with equal volume of pure water at 0-4 ℃ overnight, centrifuging for 10-25 minutes at 12000r/min at 11000-; the squid melanin extracted by the enzyme method has better hydrolysis effect, is simple and easy to operate, avoids using toxic organic solvent, is environment-friendly, and can be used for industrial production; the trace 4-hydroxyphenylethanol added in the enzymolysis process is beneficial to reducing the energy gradient between the basic state and the active state of the enzymolysis reaction, quickening the reaction progress, greatly improving the efficiency of the enzymolysis reaction and saving the time cost and the labor cost;
preparing polypeptide chelated iron, namely hydrolyzing squid protein, hydrolyzing according to the conditions of 4.1-4.5 parts of squid meat, 100 parts of distilled water, 120 parts of distilled water, 40-45 ℃, 4000U/g of neutral protease 2000-;
the preparation of the polypeptide chelated calcium comprises the steps of transferring 20-30 parts of 9-12 mmol/L calcium chloride solution into a glass reaction bottle, adding 0.018-0.023 part of squid ink melanin, 0.003-0.005 part of polypeptide chelated iron agent and 0.001-0.0015 part of D-4-hydroxyphenylglycine, adjusting the pH value of the solution to 3.8-4.5, filling nitrogen and placing in a dark place, oscillating and adsorbing for 8-10 hours by a shaking table at 50-55r/min, taking out and centrifuging, taking out the precipitate and drying to obtain the ink melanin chelated calcium;
preparation of tablets: respectively weighing 40-45 parts of jet black chelated calcium, 40-42 parts of microcrystalline cellulose, 10-15 parts of filler, 20-25 parts of calcium hydrophosphate, 10-15 parts of hydroxypropyl methyl cellulose, 1.5-2.0 parts of superfine silica gel powder and 0.2-0.3 part of vitamin D, uniformly mixing in a wet granulator, adding 10-15 parts of 50-55% ethanol to prepare a soft material, granulating the obtained soft material on a swing granulator by using a 20-24-mesh nylon screen, drying the obtained granules in a fluidized bed, finishing granules, adding 2-3 parts of magnesium stearate for total mixing, preparing the granules obtained by the total mixing into shallow concave round tablets with the diameter of 6-7mm by using a rotary tablet press and coating to obtain the jet black chelated calcium tablet; the effective calcium component in the tablet has high content, and can be easily absorbed by human body, and melanin has antibacterial and antiviral activity, and also has strong antioxidant and free radical scavenging effects, and can enhance immunity of human body; the calcium tablet has good taste, good stability and strong disintegration effect, and can accelerate the dissolution of the medicine; the production process is feasible, the quality is controllable, and the method is suitable for industrial mass production;
the application comprises the following steps: the chelated calcium tablet can be swallowed or chewed or eaten in a buccal manner, and is suitable for people of all ages to eat; the tablet can supplement calcium, enhance immunity by regulating steady state of antioxidant system, has certain effect in removing lead from blood lead and liver lead, and can protect copper in liver, zinc in kidney and zinc in brain.
Preferably, the filler is lactose or mannitol or a compressible starch; has fluidity, compressibility, self-lubricating property and adhesiveness, and has good disintegration effect and easy absorption by human body.
Preferably, the coating material is a mixture of 20-25 parts of cane sugar, 0.045-0.05 part of neotame, 0.5-0.6 part of menthol, 20-25 parts of sorbitol, 35-40 parts of dextrin and 1-1.2 parts of magnesium stearate; the tablet coating has good stability and is suitable for large-scale production.
Compared with the prior art, the invention has the advantages that: 1) the effective calcium component in the tablet has high content, and can be easily absorbed by human body, and melanin has antibacterial and antiviral activity, and also has strong antioxidant and free radical scavenging effects, and can enhance immunity of human body; the calcium tablet has good taste, good stability and strong disintegration effect, and can accelerate the dissolution of the medicine; the production process is feasible, the quality is controllable, and the method is suitable for industrial mass production; 2) The tablet can supplement calcium, enhance immunity by regulating steady state of antioxidant system, has certain effect in removing lead from blood lead and liver lead, and can protect copper in liver, zinc in kidney and zinc in brain.
Drawings
FIG. 1 is a graph showing the relationship between the calcium ion chelating ratio of squid melanin and the weight ratio of polypeptide chelating iron agent/D-4-hydroxyphenylglycine.
Detailed Description
The scheme of the invention is further illustrated by the following examples:
example 1:
preparation and application of squid ink melanin-chelated calcium tablets comprise the following steps:
1) soaking squid to obtain ink, soaking the squid in pure water with the same volume at 4 ℃ overnight, centrifuging for 10 minutes at 11000r/min, adding alkaline protease for hydrolysis, heating to inactivate enzyme, centrifuging for 10 minutes at 12000r/min, repeatedly washing with water, centrifuging to neutrality, taking precipitate, drying at 65 ℃ to obtain melanin, 2) adding neutral protease and flavor enzyme into squid meat for hydrolysis, inactivating, filtering to obtain hydrolysate, adding 1ml of 0.1 mol/L ferric chloride solution into 100ml of hydrolysate, adding 0.1g of ascorbic acid, adjusting the pH to 7, keeping the temperature at 20 ℃, magnetically stirring for 15 minutes, centrifuging to remove precipitate, concentrating, freeze-drying, placing in a drying dish at 0 ℃ for later use, 3) transferring 20ml of 9 mmol/L calcium chloride solution into a glass reaction bottle, adding 0.018 part of squid melanin, 0.003g of polypeptide chelate iron agent, adjusting the pH of the solution to 3.8, filling nitrogen, placing in a shaking table for 8 hours, taking out, drying, taking out the precipitate, and obtaining the squid melanin black pigment with high stability and being suitable for industrial production without side effects of other side effects;
4) respectively weighing 40 parts of melanin chelated calcium, 40 parts of microcrystalline cellulose, 10 parts of mannitol, 20 parts of calcium hydrophosphate, 10 parts of hydroxypropyl methyl cellulose, 1.5 parts of superfine silica gel powder and 0.2 part of vitamin D, uniformly mixing in a wet granulator, adding 10 parts of 50% ethanol to prepare a soft material, granulating the obtained soft material on a swing granulator by using a 20-mesh nylon screen, drying the obtained granules in a fluidized bed, finishing the granules, adding 2 parts of magnesium stearate, totally mixing, and coating the granules obtained by totally mixing by using a rotary tablet press to obtain shallow concave round punched tablets with the diameter of 6 mm; the tablet has high content of effective calcium, is easily absorbed by human body, and melanin has antibacterial and antiviral activity, strong antioxidant and free radical scavenging effects, and can enhance immunity of human body.
Example 2:
preparation and application of squid ink melanin-chelated calcium tablets comprise: the preparation, chelation, tablet preparation and application of the melanin and the polypeptide chelated iron are specifically characterized by comprising the following steps:
1) obtaining black pigment: cutting open the abdomen of the squid body, taking out an ink sac, cutting off a sac membrane, extruding ink, soaking with pure water with the same volume at 4 ℃ overnight, centrifuging at 12000r/min for 25 minutes, adjusting the pH to 7.5, adjusting the temperature to 55 ℃, adding 4500U/g of alkaline protease, adding 4-hydroxyphenylethanol with the weight of 0.5% of the ink, hydrolyzing for 2 hours, heating to inactivate enzyme, centrifuging at 14000r/min for 15 minutes, repeatedly washing with water, centrifuging to be neutral, and drying the precipitate at 75 ℃ to obtain melanin; the squid melanin extracted by the enzyme method has better hydrolysis effect, is simple and easy to operate, avoids using toxic organic solvent, is environment-friendly, and can be used for industrial production;
2) preparing polypeptide chelated iron, namely hydrolyzing 4.5 parts of squid meat, 120 parts of distilled water, 45 ℃, 4000U/g of neutral protease, 4000U/g of flavor enzyme and 7 of pH value for 2 hours, inactivating, filtering to obtain hydrolysate, adding 1.5 parts of 0.12 mol/L ferric chloride solution into 150 parts of hydrolysate, adding 0.12 part of ascorbic acid, adjusting the pH to 7.2 and the temperature to 23 ℃, carrying out magnetic stirring and chelation for 30 minutes, centrifuging to remove precipitate, concentrating, freeze-drying, preserving in a drying dish at 4 ℃ for later use, hydrolyzing squid protein to prepare polypeptide, and then preparing the polypeptide chelated iron agent for later use;
3) the preparation of the polypeptide chelated calcium comprises the steps of transferring 30 parts of 12 mmol/L calcium chloride solution into a glass reaction bottle, adding 0.023 part of squid melanin and 0.005 part of polypeptide chelated iron agent, adjusting the pH value of the solution to 4.5, filling nitrogen gas and placing the solution in a dark place, oscillating and adsorbing the solution for 10 hours by a shaking table at 55r/min, taking the solution out and centrifuging the solution, taking the precipitate and drying the precipitate to obtain the ink melanin chelated calcium;
4) preparation of tablets: respectively weighing 45 parts of jet black chelated calcium, 42 parts of microcrystalline cellulose, 15 parts of filler, 25 parts of calcium hydrophosphate, 15 parts of hydroxypropyl methyl cellulose, 2 parts of superfine silica gel powder and 0.3 part of vitamin D, uniformly mixing in a wet granulator, adding 15 parts of 55% ethanol to prepare a soft material, granulating the obtained soft material on a swing granulator by using a 24-mesh nylon screen, placing the obtained granules in a fluidized bed for drying, granulating, adding 3 parts of magnesium stearate for total mixing, and coating the particles obtained by total mixing by using a rotary tablet press to obtain a shallow concave circular punching tablet with the diameter of 7mm, wherein the coating material is a mixture of 20 parts of sucrose, 0.045 part of neotame, 0.5 part of menthol, 20 parts of sorbitol, 35 parts of dextrin and 1 part of magnesium stearate; the tablet has high content of effective calcium, is easily absorbed by human body, and melanin has antibacterial and antiviral activity, strong antioxidant and free radical scavenging effects, and can enhance immunity of human body.
Example 3:
preparation and application of squid ink melanin-chelated calcium tablets comprise: the preparation method comprises the following steps of obtaining melanin from ink, preparing polypeptide chelated iron, preparing polypeptide chelated calcium, preparing tablets and applying the tablets, and specifically comprises the following steps:
obtaining black pigment: cutting open the abdomen of the squid body, taking out an ink sac, cutting off a sac membrane, extruding ink, soaking with pure water with the same volume as 2 ℃ overnight, centrifuging at 12000r/min for 15 minutes, adjusting the pH to 7.4, adjusting the temperature to 52 ℃, adding 4200U/g of alkaline protease, adding 4-hydroxyphenylethanol with the weight of 0.7% of the ink, hydrolyzing for 3 hours, heating to inactivate enzyme, centrifuging at 14000r/min for 15 minutes, repeatedly washing with water, centrifuging to neutrality, and drying the precipitate at 70 ℃ to obtain melanin; the squid melanin extracted by the enzyme method has better hydrolysis effect, is simple and easy to operate, avoids using toxic organic solvent, is environment-friendly, and can be used for industrial production;
preparing polypeptide chelated iron, namely hydrolyzing 4.2 parts of squid meat, 100 parts of distilled water, 40 ℃, 3000U/g of neutral protease, 3000U/g of flavor enzyme and 7 of pH value for 2 hours, inactivating, filtering to obtain hydrolysate, adding 1 part of 0.12 mol/L ferric chloride solution into 120 parts of hydrolysate, adding 0.1 part of ascorbic acid, adjusting the pH to 7, performing magnetic stirring for chelation for 15 minutes, centrifuging to remove precipitates, concentrating, freeze-drying, and preserving in a drying dish at 3 ℃ for later use;
the preparation of the polypeptide chelated calcium comprises the steps of transferring 25 parts of 10 mmol/L calcium chloride solution into a glass reaction bottle, adding 0.020 part of squid melanin, 0.004 part of polypeptide chelated iron agent and 0.001 part of D-4-hydroxyphenylglycine, adjusting the pH value of the solution to 4.0, filling nitrogen and placing in a dark place, oscillating and adsorbing for 8 hours at 55r/min of a shaking table, taking out and centrifuging, taking out the precipitate and drying to obtain the black melanin chelated calcium;
preparation of tablets: respectively weighing 45 parts of jet black chelated calcium, 40 parts of microcrystalline cellulose, 15 parts of filler, 20 parts of calcium hydrophosphate, 15 parts of hydroxypropyl methyl cellulose, 2 parts of superfine silica gel powder and 0.3 part of vitamin D, uniformly mixing in a wet granulator, adding 12 parts of 50% ethanol to prepare a soft material, granulating the obtained soft material on a swinging granulator by using a 24-mesh nylon screen, placing the obtained granules in a fluidized bed for drying, granulating, adding 2 parts of magnesium stearate for total mixing, and coating the particles obtained by total mixing by using a rotary tablet press to obtain shallow concave circular punching tablets with the diameter of 7mm, wherein the coating material is a mixture of 22 parts of sucrose, 0.045 part of neotame, 0.5 part of menthol, 20 parts of sorbitol, 35 parts of dextrin and 1.2 parts of magnesium stearate; the effective calcium component in the tablet has high content, and can be easily absorbed by human body, and melanin has antibacterial and antiviral activity, and also has strong antioxidant and free radical scavenging effects, and can enhance immunity of human body; the calcium tablet has good taste, good stability and strong disintegration effect, and can accelerate the dissolution of the medicine; the production process is feasible, the quality is controllable, and the method is suitable for industrial mass production.
Example 4:
on the basis of example 3, without changing any data of example 3, the weight parts of the polypeptide chelating ferralium/D-4-hydroxyphenylglycine in the chelating step were set to 0.03/0.03, 0.04/0.02, 0.045/0.015, 0.04/0.01, 0.05/0.01, 0.03/0.005, 0.042/0.006, 0.04/0.005, 0.045/0.005, 0.05/0.005, i.e., the weight ratio of the two was 1:1, 2:1, … …, 9:1, 10: 1.
Measuring the content of calcium ions in the solution after the chelation step in the examples 1 to 4 by using a spectrophotometry method, so as to obtain the chelation rate of the squid melanin chelated calcium, and arranging the chelation rates in the examples 1 to 3 into the values shown in the table 1:
TABLE 1 chelating ratio of calcium chelate from squid ink melanin in examples 1-3
| Example 1 | Example 2 | Example 3 | |
| Rate of chelation | 60.5％ | 58.6％ | 68.5％ |
From table 1, it can be seen that by controlling a proper chelating condition, the chelating rate of squid ink melanin to calcium ions is very high, and can reach 55% -70%, the higher chelating rate improves the utilization efficiency of squid ink, increases the amount of calcium ions absorbed by squid ink melanin, and improves the calcium content of squid ink melanin chelated calcium tablets, and particularly, after D-4-hydroxyphenylglycine is added in the chelating reaction of example 3, the chelating rate of squid ink melanin is improved by nearly 10% compared with examples 1-2 without D-4-hydroxyphenylglycine, which shows that the addition of D-4-hydroxyphenylglycine improves the absorption effect of squid ink melanin to calcium ions based on a certain unknown intrinsic mechanism.
The chelating rate of the polypeptide iron chelate agent and D-4-hydroxyphenylglycine in example 4 was measured in different weight parts, and the relationship between the chelating rate and the weight ratio is shown in FIG. 1.
As can be seen from fig. 1, there is a correlation between the chelating rate of squid melanin to calcium ions and the weight ratio of the polypeptide iron chelate to D-4-hydroxyphenylglycine, and the correlation exhibits a non-linear correlation; as can be seen from figure 1, when the weight ratio of the polypeptide chelated iron agent to the D-4-hydroxyphenylglycine is within the interval of 3:1-10:1, the chelated rate of the squid ink melanin to the calcium ions is higher than 60%, particularly, when the weight ratio of the polypeptide chelated iron agent to the D-4-hydroxyphenylglycine is 3:1 or within the interval of 7:1-8:1, the chelated rate of the squid ink melanin to the calcium ions reaches more than 80%, which may be because the D-4-hydroxyphenylglycine acts on the polypeptide chelated iron agent to release certain unknown substances to change the chelated internal environment, thereby improving the adsorption capacity of the squid ink melanin to the calcium ions and improving the chelated rate thereof, the internal mechanism thereof is not clear, the higher chelated rate of the squid ink melanin to the calcium ions is helpful for improving the content of calcium in the tablet, meanwhile, the utilization value of the black pigment of the squid ink is enhanced.
Conventional operations in the operation steps of the present invention are well known to those skilled in the art and will not be described herein.
The embodiments described above are intended to illustrate the technical solutions of the present invention in detail, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modification, supplement or similar substitution made within the scope of the principles of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A preparation method of squid ink melanin chelated calcium tablets comprises the steps of obtaining squid melanin, preparing polypeptide chelated iron, preparing polypeptide chelated calcium and preparing tablets, and is characterized in that the polypeptide chelated iron is prepared by the steps of hydrolyzing squid protein, hydrolyzing according to the conditions that squid meat is 4.1-4.5 parts, distilled water is 100 parts, the temperature is 40-45 ℃, neutral protease 2000-;
the preparation method of the polypeptide chelated calcium comprises the steps of moving 20-30 parts of 9-12 mmol/L calcium chloride solution into a glass reaction bottle, adding 0.018-0.023 part of squid melanin, 0.003-0.005 part of polypeptide chelated iron agent and 0.001-0.0015 part of D-4-hydroxyphenylglycine, adjusting the pH value of the solution to 3.8-4.5, filling nitrogen and placing in a dark place, oscillating and adsorbing for 8-10 hours by a shaking table at 50-55r/min, taking out and centrifuging, taking out and drying precipitates to obtain the melanin chelated calcium.
2. The preparation of the squid melanin-chelated calcium tablet according to claim 1, wherein: the step of obtaining the melanin of the ink comprises the following steps: cutting open the abdomen of the squid body, taking out the ink sac, cutting off the sac membrane, extruding out the ink, soaking in pure water with the same volume at 0-4 ℃ overnight, centrifuging at 12000r/min for 10-25 minutes at 11000-.
3. The preparation of the squid melanin-chelated calcium tablet according to claim 1, wherein: the preparation steps of the tablet are as follows: respectively weighing 40-45 parts of jet black chelated calcium, 40-42 parts of microcrystalline cellulose, 10-15 parts of filler, 20-25 parts of calcium hydrogen phosphate, 10-15 parts of hydroxypropyl methyl cellulose, 1.5-2 parts of superfine silica gel powder and 0.2-0.3 part of vitamin D, uniformly mixing in a wet granulator, adding 10-15 parts of 50-55% ethanol to prepare a soft material, granulating the obtained soft material on a swing granulator by using a 20-24 mesh nylon screen, drying the obtained granules in a fluidized bed, granulating, adding 2-3 parts of magnesium stearate for total mixing, preparing the granules obtained by total mixing into shallow concave round punched tablets with the diameter of 6-7mm by using a rotary tablet press, and coating to obtain the jet black chelated calcium tablet.
4. The preparation method of the squid melanin-chelated calcium tablet according to claim 3, wherein the steps of: the filling agents in the preparation step of the tablet are as follows: lactose or mannitol or a compressible starch.
5. The preparation method of the squid melanin-chelated calcium tablet according to claim 3, wherein the steps of: the coating material in the tablet preparation step is a mixture of 20-25 parts of sucrose, 0.045-0.05 part of neotame, 0.5-0.6 part of menthol, 20-25 parts of sorbitol, 35-40 parts of dextrin and 1-1.2 parts of magnesium stearate.
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