CN107286352A - The method for extracting simultaneously separate active ingredients simultaneously from fish scale - Google Patents
The method for extracting simultaneously separate active ingredients simultaneously from fish scale Download PDFInfo
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- CN107286352A CN107286352A CN201710462868.7A CN201710462868A CN107286352A CN 107286352 A CN107286352 A CN 107286352A CN 201710462868 A CN201710462868 A CN 201710462868A CN 107286352 A CN107286352 A CN 107286352A
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- fish scale
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- 241000251468 Actinopterygii Species 0.000 title claims abstract description 120
- 238000000034 method Methods 0.000 title claims abstract description 46
- 239000004480 active ingredient Substances 0.000 title claims abstract description 14
- UYTPUPDQBNUYGX-UHFFFAOYSA-N guanine Chemical compound O=C1NC(N)=NC2=C1N=CN2 UYTPUPDQBNUYGX-UHFFFAOYSA-N 0.000 claims abstract description 117
- 102000008186 Collagen Human genes 0.000 claims abstract description 115
- 108010035532 Collagen Proteins 0.000 claims abstract description 115
- 229920001436 collagen Polymers 0.000 claims abstract description 114
- 108090000765 processed proteins & peptides Proteins 0.000 claims abstract description 47
- 239000000284 extract Substances 0.000 claims abstract description 36
- 238000000605 extraction Methods 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 54
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 48
- 239000000243 solution Substances 0.000 claims description 43
- 239000002244 precipitate Substances 0.000 claims description 39
- 238000001914 filtration Methods 0.000 claims description 31
- 239000000843 powder Substances 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 29
- 239000000706 filtrate Substances 0.000 claims description 27
- 238000000926 separation method Methods 0.000 claims description 21
- 239000012141 concentrate Substances 0.000 claims description 17
- 238000001556 precipitation Methods 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 12
- 108091003079 Bovine Serum Albumin Proteins 0.000 claims description 11
- QYSGYZVSCZSLHT-UHFFFAOYSA-N octafluoropropane Chemical compound FC(F)(F)C(F)(F)C(F)(F)F QYSGYZVSCZSLHT-UHFFFAOYSA-N 0.000 claims description 11
- 241000370738 Chlorion Species 0.000 claims description 10
- 230000033228 biological regulation Effects 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 238000004108 freeze drying Methods 0.000 claims description 9
- KDCGOANMDULRCW-UHFFFAOYSA-N 7H-purine Chemical compound N1=CNC2=NC=NC2=C1 KDCGOANMDULRCW-UHFFFAOYSA-N 0.000 claims description 8
- 241000283690 Bos taurus Species 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 238000002390 rotary evaporation Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 239000003292 glue Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000013505 freshwater Substances 0.000 claims description 3
- 102000004169 proteins and genes Human genes 0.000 claims description 3
- 108090000623 proteins and genes Proteins 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000005202 decontamination Methods 0.000 claims description 2
- 230000003588 decontaminative effect Effects 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 2
- 238000005457 optimization Methods 0.000 claims description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 2
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 2
- 102000004196 processed proteins & peptides Human genes 0.000 claims 2
- 150000004679 hydroxides Chemical class 0.000 claims 1
- 210000002966 serum Anatomy 0.000 claims 1
- 238000004781 supercooling Methods 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 13
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000007812 deficiency Effects 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 20
- 230000000694 effects Effects 0.000 description 8
- 238000011160 research Methods 0.000 description 8
- 235000011121 sodium hydroxide Nutrition 0.000 description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 6
- 239000011575 calcium Substances 0.000 description 6
- 229910052791 calcium Inorganic materials 0.000 description 6
- 241000252230 Ctenopharyngodon idella Species 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000004833 fish glue Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- QCVGEOXPDFCNHA-UHFFFAOYSA-N 5,5-dimethyl-2,4-dioxo-1,3-oxazolidine-3-carboxamide Chemical compound CC1(C)OC(=O)N(C(N)=O)C1=O QCVGEOXPDFCNHA-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 102000002322 Egg Proteins Human genes 0.000 description 2
- 108010000912 Egg Proteins Proteins 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 235000014103 egg white Nutrition 0.000 description 2
- 210000000969 egg white Anatomy 0.000 description 2
- 235000013601 eggs Nutrition 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 2
- 239000005416 organic matter 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
- -1 purine Class compound Chemical class 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 description 1
- 206010000830 Acute leukaemia Diseases 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 108091005804 Peptidases Proteins 0.000 description 1
- 239000004365 Protease Substances 0.000 description 1
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 1
- 101710093813 Scale keratin Proteins 0.000 description 1
- 208000034189 Sclerosis Diseases 0.000 description 1
- 241000238371 Sepiidae Species 0.000 description 1
- 208000005718 Stomach Neoplasms Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 125000002015 acyclic group Chemical group 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000003466 anti-cipated effect Effects 0.000 description 1
- 230000036436 anti-hiv Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 210000001367 artery Anatomy 0.000 description 1
- 230000008827 biological function Effects 0.000 description 1
- 208000002352 blister Diseases 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 230000037396 body weight Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000032677 cell aging Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 210000001268 chyle Anatomy 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 235000015177 dried meat Nutrition 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 230000005714 functional activity Effects 0.000 description 1
- 206010017758 gastric cancer Diseases 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 208000019622 heart disease Diseases 0.000 description 1
- 230000023597 hemostasis Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 235000010445 lecithin Nutrition 0.000 description 1
- 229940067606 lecithin Drugs 0.000 description 1
- 239000000787 lecithin Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 108020004707 nucleic acids Proteins 0.000 description 1
- 102000039446 nucleic acids Human genes 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 108010048734 sclerotin Proteins 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 201000011549 stomach cancer Diseases 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000004260 weight control Methods 0.000 description 1
- 230000029663 wound healing Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H1/00—Macromolecular products derived from proteins
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D473/00—Heterocyclic compounds containing purine ring systems
- C07D473/02—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6
- C07D473/18—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 one oxygen and one nitrogen atom, e.g. guanine
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/78—Connective tissue peptides, e.g. collagen, elastin, laminin, fibronectin, vitronectin or cold insoluble globulin [CIG]
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Biophysics (AREA)
- Gastroenterology & Hepatology (AREA)
- Genetics & Genomics (AREA)
- Zoology (AREA)
- Molecular Biology (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Toxicology (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymers & Plastics (AREA)
- Peptides Or Proteins (AREA)
Abstract
The invention discloses a kind of method for extracting simultaneously separate active ingredients simultaneously from fish scale, using fish scale as raw material, guanine in fish scale, collagen peptide and collagen are extracted simultaneously, the concentration and acidity and temperature of extract solution are controlled again, are successively separated collagen, guanine and collagen peptide；The inventive method is using fish scale as raw material, onestep extraction simultaneously separates collagen, collagen peptide and guanine, and technique is easy, takes full advantage of fish scale natural resources, the technological deficiency of the single extraction in current technology is overcome, with obvious social value and economic benefit.
Description
Technical field
The present invention relates to biological extractive technique, belong to fish sideline production deep process technology field, particularly one kind is same from fish scale
When extract and separation guanine, the method for collagen peptide and collagen.
Background technology
Fish scale（scale）It is the sclerotin scale of the collagen generation of fish skin corium, accounts for the 1% ~ 5% of fish body weight.Fish scale
In appearance as petal, and edge is in small curling, and white gloss slightly has a fish like smell, and quality is hard and soft.Table is studied
Bright, organic matter accounts for 41% ~ 55% in fish scale, and inorganic matter accounts for 38% ~ 46%, and water content is 16.4%~17.8%.Content of organics
Most is protein, wherein being accounted for the 90% of fish scale organic matter based on collagen and fish scale keratin again, also being contained purine
Class compound.Inorganic matter is based on hydroxyapatite.
Fish scale shows good effect in nutrition and medical domain.Nutritionist's research finds that fish scale contains more
Lecithin, plays the role of enhancing memory, delays and prolong cell ageing；Contain substantial amounts of collagen in fish scale, can rise a variety of
Biological function, such as promotes wound healing, hemostasis, and antigenicity is relatively low, can promote the formation of bone, enhancing skin metabolism etc..
Fish scale collagen and other collagen ratios, its protein easily decompose, are easily digested, absorb.It is a variety of contained by fish scale
Unrighted acid, can help to transmit and chyle fat in protein-bonded form, reduce cholesterol in blood vessel in blood
Deposited on wall, with preventing a variety of effects such as artery sclerosis, preventing hypertension and heart disease.Therefore, fish scale is special health care
Food.The 6- extracted from fish scale is dredged for guanine, clinical treatment acute leukemia, and effective percentage is 70%~75%；And to stomach cancer,
Lymphadenoma also has special effect.
Contain more guanine in fish scale, guanine can be extracted from birds droppings or fish scale.Guanine and its derivative
With important biomolecule activity, such as antitumor, antiviral [Kim A., Hong H.J.Synthesis and anti-HIV study
of novel acyclic guanine derivatives[J]. Nucleosides Nucleotides Nucleic
Acids, 2008,27（2）：121-130] etc., it is also main medicine intermediate, available for synthesizing a series of the anti-of high-efficiency low-toxicities
Bleb medicine.
China is freshwater fish culturing country maximum in the world.The annual leftover bits and pieces produced during processing of aquatic products
(such as fish-skin, fish-bone, crab shell, fish scale) reaches more than 2,500,000 tons, and [person of outstanding talent once celebrates exploitation prospect [J] of filial piety fish scales
Process technology, 2004, (5)：74-75], wherein fish scale is up to 35 ~ 450,000 tons [before the preparation and development and application of He Lan scale collagens
Scape [J] aquatic science and technology information, 2007,34 (5)：210-212].How fish scale resource is utilized, it is turned waste into wealth, be in recent years
To be engaged in the focus of fishery process deeply industry research.To the deep processing and utilization of these fish scale discarded objects, existing substantial amounts of research report
Road.Research is concentrated mainly on fish scale extracts collagen, anti-oxidation peptide, [Zeng Li, Li Li, Wang Jiabin wait water to blood pressure lowering peptide
Produce collagen peptide functional activity and its Study on Preparation progress [J] Oceanography Institute Of Zhejiang journal, 2013,32 (2)：163-
168], with each fish scale hydroxyapatite of fish scale system etc., [Hao person of outstanding talent's ultrasound pretreatment enzyme membrane coupled reaction prepares fish scale collagen
The technical research of peptide, Jiangsu University's master thesis, 2014] and extraction guanine or pearl essence or fish scale essence (fish
Silver) [Zeng Xiaodan, Zhang Yingjiao, Xia Chen, Wang Zipeng, Cao Yang grass carp scales extract technique and the quality research [J] of guanine,
Modern agriculture science and technology, 2012,1:15-16；A kind of methods that pearl essence is extracted from fish scale of CN1033827A；
A kind of methods that pearl essence is extracted from fish scale of CN201410730562.1] etc..
The method that collagen is extracted from fish scale, general technology path can be attributed to：First by fish scale removal of impurities, clean and dry in the air
It is dry, then calcium is removed with calcium remover, the suitable extractant of reselection and equipment extract collagen and separation.According to the extraction of selection
Agent is different, and obtained collagen is different, and [zu knows gorgeous, Xiong Guangquan, Li Xin, Geng Shengrong, Yu Wei, Jiang Hongyou, Liao Tao grass carp scales
Preparation and analysis [J] food research and developments of collagen peptide, 2014,35（7）：36-39;Zhang Huijie Hydrolyzed Collagens
The research of molecular weight control technology, University Of Science and Technology Of Tianjin's Master's thesis, 2014,2-3].The fish glue from scale quilt obtained with hot water treatment
Referred to as hot method glue, the fish glue from scale obtained is handled with acid solution and is referred to as acid-processed gelatin, the fish glue from scale obtained with base extraction is then referred to as
Alkaline process glue, the fish glue from scale for taking protease to obtain is referred to as enzyme process glue or collagen peptide, and the A of CN 103773828 are from fish scale
The method for extracting collagen；A kind of preparation methods of acid-soluble fish scale collagen of the A of CN 104892750；
A kind of preparation methods of fish scale collagen of CN101418328A；The B of CN 103773830 one kind extracts collagen egg from fish scale
White method；A kind of methods that collagen is extracted from fish scale of the A of CN 105063154；The B of CN 103773830 it is a kind of from
The method that collagen is extracted in fish scale；Lei Jing, Li Hesheng, Zhang Liyuan, Sun Nannan, the extraction of cuttlefish collagen and knot
Structure characterizes [J], research and development of natural products, 2012,24:575-580] etc..
The method that guanine is extracted from fish scale, is studied less at present.It is rarely seen have once Xiao Dan et al. carried from grass carp scales
Taking guanine, [Zeng Xiaodan, Zhang Yingjiao, Xia Chen, Wang Zipeng, Cao Yang grass carp scales extract technique and the quality research of guanine
[J], modern agriculture science and technology, 2012,1:15-16], two China's patent of invention [CN1033827A one kind is carried from fish scale
The method for taking pearl essence；A kind of methods that pearl essence is extracted from fish scale of CN201410730562.1].Previous literature method is
By the fish scale anticipated, at 98 DEG C of temperature, surfactant is added and under the conditions of concentration is 5.0 moL/L hydrochloric acid
Grass carp scales are extracted into 2.0 h, quiescent crystallization after filtrate is obtained, and produce hydrochloric acid bird after crystallization is refined again with hydrochloric acid solution
Purine.Latter two patents method has used surfactant and have a significant impact to human body and environment four in subsequent treatment
Chlorination carbon.
Technology contents disclosed above are only that the collagen or collagen peptide or guanine of fish scale are entered respectively
Capable independent extraction.That is when extracting collagen or collagen peptide, guanine is not extracted；Extracting bird
During purine, collagen or collagen peptide are not extracted, when especially doing calcium remover with acid, existing part collagen
It is dissolved in acid and loses.Thus it is described above and method there is the waste to loss and resource with important available composition
The problem of, and also have no so far in the industry with regard to how using fish scale while extracting the collagen of high value added product, collagen egg
White peptide and guanine and propose effective technical scheme.Therefore, one kind is researched and developed to extract active component simultaneously from fish scale and its divide
From method, to improve production efficiency, reduce the wasting of resources it is very necessary.
The content of the invention
The purpose of the present invention is：A kind of method for extracting simultaneously separate active ingredients simultaneously from fish scale is proposed, from fish scale
Onestep extraction simultaneously isolates the collagen with important physiological action, collagen peptide and guanine product, to realize fish scale
Efficient utilization.
The present invention technical solution be：Using fish scale as raw material, by the guanine in fish scale, collagen peptide and collagen
Albumen is extracted simultaneously, then controls the concentration and acidity and temperature of extract solution, successively by collagen, guanine and collagen egg
White peptide is separated；Comprise the following steps that:To cleaning with deimpurity fish scale after freeze-drying, thread fish scale is ground into；
After thread fish scale is mixed according to certain solid-to-liquid ratio with Extraction solvent, it is placed in Vltrasonic device, ultrasonic power, temperature in setting
Extracted under degree and ultrasonic time, insoluble matter is removed in centrifugation, obtain mixed containing guanine, collagen peptide and collagen
Close extract solution；Mixed extract is placed in rotary evaporating device and carries out being concentrated to give concentrate；Concentrate is placed in quiet under low temperature
Put to occurring after precipitation and clear liquid, be filtrated to get precipitate A and clear liquid B；Precipitate A is washed with deionized to without freezing after chlorion
Dry white thing C；Clear liquid B is adjusted to certain pH value by alkaline solution, certain time is stood at low temperature, filtering and
It is washed with deionized to after without chlorion and obtains white precipitate D and settled solution E, white precipitate D is frozen into white powder
Shape D；Settled solution E continuation is adjusted to certain pH value with alkaline solution, concentration, and certain time is stood at low temperature, filtering point
From that must precipitate F and filtrate G, precipitation F is scrubbed, after freeze-drying be colourless thing F, and it is dry that filtrate G is concentrated rear directly freezed
White powder G；White thing C, white powder D it is infrared completely the same and water insoluble with the infrared figure of standard bovine albumin,
It is soluble in hydrochloric acid, it was demonstrated that two kinds of things are collagen；Colourless thing F's is infrared basically identical with standard guanine, water insoluble, card
Bright is impure guanine；White powder G is highly soluble in water, is also highly soluble in acid, the infrared clear collagen of figure and standard bovine
Unanimously, it is marked as the water-soluble collagen peptide containing salt.
Wherein, fish scale used is the mixture of ocean fish, the fish scale of fresh-water fishes or two kinds of fish scales.
Wherein, the fish scale of described clean and decontamination refers to：The fish scale that market is purchased, is washed with water to no color
With wash water solution without muddy thing, other any processing are not done, is directly freeze-dried, is ground into thread fish scale.
Wherein, the selection of Extraction solvent is, in different solvents, such as to go with two kinds of standard sample guanines and collagen
Ionized water, ammoniacal liquor, sodium hydroxide solution, hydrochloric acid solution carry out solubility test respectively；Wherein hydrochloric acid solution can dissolve two kinds of marks
Quasi- sample（Guanine and collagen）；Therefore hydrochloric acid solution is the preferred solvent of extraction simultaneously.
Wherein, the extraction process of mixed extract is：Thread fish scale is dense according to mass number and 0.050~0.82 mol/L
The hydrochloric acid solution volume of degree is according to 1g:After 10 ~ 19mL is than mixing, it is placed in Vltrasonic device, 20 ~ 40 points of power 35~71%, time
Clock and temperature 300C is extracted；Insoluble matter is removed in centrifugation, obtains mixed containing guanine, collagen peptide and collagen
Close extract solution.
Wherein, mixed extract is obtained under the extraction conditions using Uniform Design method；To collagen and
The recovery rate of collagen peptide is to representing the hydroxyl dried meat ammonia of collagen and collagen peptide in mixed extract by photometry
What acid was measured and calculated；Recovery rate to guanine is to the guanine in mixed extract by high performance liquid chromatography
Detected and calculated；Relation to extraction conditions and recovery rate is fitted by the softwares of Excel 2003, has been drawn time
Return analysis equation, with this equation of partial differentiation solution, the extraction conditions optimized are：The quality of thread fish scale and the body of hydrochloric acid
Product is than being 1g：16.6mL, HCl concentration 0.33mol/L, ultrasonic power 57%, extraction time 28min, Extracting temperature is 300C。
Wherein, concentration process is：The r/min of mixed extract 6000 centrifuges 20min, obtains filtrate, and the rotated evaporation of filtrate is dense
Contract to obtain concentrate.
Wherein, the separation of collagen is：Concentrate is placed in 00C~10 0After C is stood overnight, it is separated by filtration, is precipitated
A and clear liquid B；Precipitate A is washed with deionized to after without chlorion is freeze-dried to obtain white thing C in freeze dryer；Clear liquid B is used
0.5 ~ 1mol/L sodium hydroxide regulation pH value be 6.0 ~ 6.5 after, also in 00C~10 0After C stand at low temperature is stayed overnight, pass through
Quantitative filter paper is filtered and deionized water washing, obtains white precipitate D and settled solution E, white precipitate D is frozen into white powder
Shape D；White thing C, white powder D it is infrared completely the same and water insoluble with the infrared figure of standard bovine albumin, be soluble in
Hydrochloric acid, it was demonstrated that two kinds of things are collagen.
Wherein, the separation of guanine is：Settled solution E as obtained by filtering after white precipitate D quantitative filter paper with 0.05 ~
0.2mol/L sodium hydroxides adjust pH value after 7.0-7.5, to concentrate, 00C~10 0C stand at low temperature is overnight to having clear liquid and heavy
Form sediment, F and filtrate G must be precipitated by being separated by filtration, precipitation F is colourless thing F through water washing, after freeze-drying；Colourless thing F infrared and mark
Quasi- guanine is basically identical, water insoluble, it was demonstrated that be impure guanine.
Wherein, the separation of collagen peptide is：The filtrate G after F must be precipitated by being separated by filtration, and rotary evaporation is steamed to anhydrous,
White powder G is freezed to obtain after being frozen again in low temperature refrigerator in freeze drier；White powder G is highly soluble in water, also easily
Acid is dissolved in, infrared figure is consistent with the clear collagen of standard bovine, is marked as the water-soluble collagen peptide containing salt.
The present invention has advantages below：
（One）The present invention passes through simple ion step with fish scale, directly carries out the extraction of active component and dividing in fish scale simultaneously
From simplifying current existing patented technology or document fish scale make raw material and extract collagen or collagen peptide to need plus remove
The step of calcium agent removes calcium so that extraction process is easy.
（Two）Using certain density hydrochloric acid as extractant, while serving a variety of effects：Can dissolve collagen and
Guanine, can also be by part collagen acidolysis into collagen peptide, but also is acting on production subsequently through with sodium hydroxide
Salt, serves the effect for salting out collagen and the effect for removing calcium in fish scale.
（Three）Existing utilization fish scale is extracted in collagen or the invention of collagen peptide or technical literature, in extraction process
In be only extracted fish scale single-activity composition, other useful components are lost；It is of the invention compared with these existing technologies, in fish scale
Collagen, collagen peptide and the step of guanine active ingredient one are extracted and basic separation, take full advantage of fish scale
Natural resources, overcomes the technological deficiency of single extraction.
Brief description of the drawings
Fig. 1 is process chart of the invention；Wherein：（1）To extract optimization technological process figure；（2）To extract with separating
Process chart；
Fig. 2 is the white thing C and standard bovine albumin infrared scan figure extracted；
Fig. 3 is the white thing D extracted and the infrared scan figure of standard bovine albumin；
Fig. 4 is the colourless thing F and guanine standard specimen infrared scan figure extracted；
Fig. 5 is the white thing G extracted and the infrared scan figure of standard bovine albumin.
Embodiment
The present invention is specifically described below by embodiment.It must be noted that the embodiment provided, only it is pair
The present invention's further illustrates, it is impossible to be interpreted as limiting the scope of the invention, the professional in the field can basis
Present disclosure makes the modifications and adaptations of some non-intrinsically safes.
Embodiment 1：Extracted according to following steps and separate the active component in fish scale
（1）The pretreatment of fish scale：The fish scale that market is purchased, is washed with water to no color and wash water solution without muddy thing,
Other any processing are not done, are directly freeze-dried, are ground into thread fish scale；
（2）The acquisition of mixed extract：By hydrochloric acid solution body of the thread fish scales of 50.0g according to mass number and 0.050mol/L concentration
Product is according to 1g:After 10mL is than mixing, it is placed in Vltrasonic device, power 35%, 20 minutes time and temperature 300C is extracted；From
The heart separates insoluble matter, obtains the mixed extract containing guanine, collagen peptide and collagen；
（3）Concentration：The r/min of mixed extract 6000 centrifuges 20min, obtains filtrate, filtrate is rotated to be concentrated by evaporation to obtain concentrate；
（4）The separation of collagen：Concentrate is placed in 00After C is stood overnight, it is separated by filtration, obtains precipitate A and clear liquid B；Precipitation
A is washed with deionized to after without chlorion is freeze-dried to obtain white thing C 6.8g in freeze dryer；Clear liquid B 0.5mol/L
Sodium hydroxide regulation pH value be 6.0 after, also in 00After C stand at low temperature is stayed overnight, pass through quantitative filter paper filtering and deionization
Water washing, obtains white precipitate D and settled solution E, and white precipitate D is frozen into white powder D 4.6g；It is white thing C, white
The powdered D's of color is infrared completely the same and water insoluble with the infrared figure of standard bovine albumin, is soluble in hydrochloric acid, it was demonstrated that two kinds
Thing is collagen；
（5）The separation of guanine：Settled solution E 0.05mol/L hydrogen-oxygens as obtained by filtering after white precipitate D quantitative filter paper
Change sodium regulation pH value be 7.0 after, concentration, 00C stand at low temperature is overnight to having clear liquid and precipitation, and F and filter must be precipitated by being separated by filtration
Liquid G, precipitation F is colourless thing F 0.24g through water washing, after freeze-drying；Colourless thing F infrared and standard guanine is infrared basic
Unanimously, it is water insoluble, it was demonstrated that to be impure guanine；
（6）The separation of collagen peptide：The filtrate G after F must be precipitated by being separated by filtration, and rotary evaporation is steamed to anhydrous, then in low temperature
White powder G 5.2g are freezed to obtain after being frozen in refrigerator in freeze drier；White powder G is highly soluble in water, is also highly soluble in
Acid, white powder G infrared figure is consistent with the infrared figure of the clear collagen of standard bovine, is marked as the water-soluble collagen egg containing salt
White peptide.
Embodiment 2：Extracted according to following steps and separate the active component in fish scale
（1）The pretreatment of fish scale：The fish scale that market is purchased, is washed with water to no color and wash water solution without muddy thing,
Other any processing are not done, are directly freeze-dried, are ground into thread fish scale；
（2）The acquisition of mixed extract：By hydrochloric acid solution volume of the thread fish scales of 50.0g by mass number and 0.45mol/L concentration
According to 1g:After 14.5mL is than mixing, it is placed in Vltrasonic device, power 53%, 30 minutes time and temperature 300C is extracted；From
The heart separates insoluble matter, obtains the mixed extract containing guanine, collagen peptide and collagen；
（3）Concentration：The r/min of mixed extract 6000 centrifuges 20min, obtains filtrate, filtrate is rotated to be concentrated by evaporation to obtain concentrate；
（4）The separation of collagen：Concentrate is placed in 50After C is stood overnight, it is separated by filtration, obtains precipitate A and clear liquid B；Precipitate A
It is washed with deionized to after without chlorion and white thing C 13.8g is freeze-dried to obtain in freeze dryer；Clear liquid B 0.75mol/L
Sodium hydroxide regulation pH value be 6.3 after, also in 50After C stand at low temperature is stayed overnight, pass through quantitative filter paper filtering and deionization
Water washing, obtains white precipitate D and settled solution E, and white precipitate D is frozen into white powder D 11.1g；It is white thing C, white
The powdered D's of color is infrared completely the same and water insoluble with the infrared figure of standard bovine albumin, is soluble in hydrochloric acid, it was demonstrated that two kinds
Thing is collagen；
（5）The separation of guanine：Settled solution E as obtained by filtering after white precipitate D quantitative filter paper is with 0.13 mol/L hydrogen
Sodium oxide molybdena regulation pH value be 7.5 after, concentration, 50C stand at low temperature overnight to having clear liquid and precipitation, be separated by filtration must precipitate F and
Filtrate G, precipitation F is colourless thing F 0.28g through water washing, after freeze-drying；Colourless thing F infrared and standard guanine basic one
Cause, it is water insoluble, it was demonstrated that to be impure guanine；
（6）The separation of collagen peptide：The filtrate G after F must be precipitated by being separated by filtration, and rotary evaporation is steamed to anhydrous, then in low temperature
White powder G 8.6g are freezed to obtain after being frozen in refrigerator in freeze drier；White powder G is highly soluble in water, also easily molten
In acid, infrared figure is consistent with the clear collagen of standard bovine, is marked as the water-soluble collagen peptide containing salt.
Embodiment 3：Extracted according to following steps and separate the active component in fish scale
（1）The pretreatment of fish scale：The fish scale that market is purchased, is washed with water to no color and wash water solution without muddy thing,
Other any processing are not done, are directly freeze-dried, are ground into thread fish scale；
（2）The acquisition of mixed extract：By hydrochloric acid solution volume of the thread fish scales of 50.0g by mass number and 0.82 mol/L concentration
According to 1g:After 19mL is than mixing, it is placed in Vltrasonic device, power 71%, 40 minutes time and temperature 300C is extracted；Centrifugation
Insoluble matter is separated, the mixed extract containing guanine, collagen peptide and collagen is obtained；
（3）Concentration：The r/min of mixed extract 6000 centrifuges 20min, obtains filtrate, filtrate is rotated to be concentrated by evaporation to obtain concentrate；
（4）The separation of collagen：Concentrate is placed in 100After C is stood overnight, it is separated by filtration, obtains precipitate A and clear liquid B；It is heavy
Shallow lake A is washed with deionized to after without chlorion is freeze-dried to obtain white thing C 15.6g in freeze dryer；Clear liquid B 1mol/L
Sodium hydroxide regulation pH value be 6.5 after, also in 100After C stand at low temperature is stayed overnight, by quantitative filter paper filter and go from
Sub- water washing, obtains white precipitate D and settled solution E, and white precipitate D is frozen into white powder D 12.1g；White thing C,
White powder D infrared figure and the infrared figure of standard bovine albumin are completely the same and water insoluble, are soluble in hydrochloric acid, it was demonstrated that
Two kinds of things are collagen；
（5）The separation of guanine：Settled solution E 0.2mol/L hydrogen-oxygens as obtained by filtering after white precipitate D quantitative filter paper
Change sodium regulation pH value be 7.5 after, concentration, 100C stand at low temperature overnight to having clear liquid and precipitation, be separated by filtration must precipitate F and
Filtrate G, precipitation F is colourless thing F 0.33g through water washing, after freeze-drying；Colourless thing F infrared figure and standard guanine is infrared
Figure is basically identical, water insoluble, it was demonstrated that be impure guanine；
（6）The separation of collagen peptide：The filtrate G after F must be precipitated by being separated by filtration, and rotary evaporation is steamed to anhydrous, then in low temperature
White powder G 9.2g are freezed to obtain after being frozen in refrigerator in freeze drier；White powder G is highly soluble in water, is also highly soluble in
Acid, the infrared figures of white powder G are consistent with the infrared figure of the clear collagen of standard bovine, are marked as the water-soluble collagen containing salt
Peptide.
Embodiment 4：Extracted according to following steps and separate the active component in fish scale
（1）The pretreatment of fish scale：The fish scale that market is purchased, is washed with water to no color and wash water solution without muddy thing,
Other any processing are not done, are directly freeze-dried, are ground into thread fish scale；
（2）The acquisition of mixed extract：By hydrochloric acid solution volume of the thread fish scales of 50.0g by mass number and 0.33mol/L concentration
According to 1g:After 16.6mL is than mixing, it is placed in Vltrasonic device, power 57%, 28 minutes time and temperature 300C is extracted；From
The heart separates insoluble matter, obtains the mixed extract containing guanine, collagen peptide and collagen；
（3）Concentration：The r/min of mixed extract 6000 centrifuges 20min, obtains filtrate, filtrate is rotated to be concentrated by evaporation to obtain concentrate；
（4）The separation of collagen：Concentrate is placed in 50After C is stood overnight, it is separated by filtration, obtains precipitate A and clear liquid B；Precipitate A
It is washed with deionized to after without chlorion and white thing C 17.1g is freeze-dried to obtain in freeze dryer；Clear liquid B is with 1mol/L's
Sodium hydroxide regulation pH value be 6.0 after, also in 50After C stand at low temperature is stayed overnight, pass through quantitative filter paper filtering and deionized water
Washing, obtains white precipitate D and settled solution E, white precipitate D is frozen into white powder D 12.5g；White thing C, white
Powdered D's is infrared completely the same and water insoluble with the infrared figure of standard bovine albumin, is soluble in hydrochloric acid, it was demonstrated that two kinds of things
For collagen；
（5）The separation of guanine：Settled solution E 0.05mol/L hydrogen-oxygens as obtained by filtering after white precipitate D quantitative filter paper
Change sodium regulation pH value be 7.5 after, concentration, 100C stand at low temperature overnight to having clear liquid and precipitation, be separated by filtration must precipitate F and
Filtrate G, precipitation F is colourless thing F 0.42g through water washing, after freeze-drying；Colourless thing F infrared and standard guanine basic one
Cause, it is water insoluble, it was demonstrated that to be impure guanine；
（6）The separation of collagen peptide：The filtrate G after F must be precipitated by being separated by filtration, and rotary evaporation is steamed to anhydrous, then in low temperature
White powder G 10.5g are freezed to obtain after being frozen in refrigerator in freeze drier；White powder G is highly soluble in water, also easily molten
In acid, infrared figure is consistent with the clear collagen of standard bovine, is marked as the water-soluble collagen peptide containing salt.
To sum up, technique according to the invention solution and given specific embodiment and related detection data card
Real, the present invention reaches expected goal of the invention.
Claims (9)
1. the method for simultaneously separate active ingredients is extracted simultaneously from fish scale, using fish scale as raw material, by the guanine in fish scale, collagen
Protein peptides and collagen are extracted simultaneously, then control the concentration and acidity and temperature of extract solution, successively by collagen, bird
Purine and collagen peptide are separated；It is characterized in that it is comprised the following steps that:To cleaning with deimpurity fish scale through supercooling
It is lyophilized it is dry after, be ground into thread fish scale；After thread fish scale is mixed according to certain solid-to-liquid ratio with Extraction solvent, ultrasonic dress is placed in
In putting, extracted under the ultrasonic power of setting, temperature and ultrasonic time, centrifugation remove insoluble matter, obtain containing guanine,
The mixed extract of collagen peptide and collagen；By mixed extract be placed in rotary evaporating device carry out be concentrated to give it is dense
Contracting liquid；Concentrate is placed under low temperature and stood to occurring after precipitation and clear liquid, is filtrated to get precipitate A and clear liquid B；Precipitate A spend from
Sub- water washing is to without being freeze-dried to obtain white thing C after chlorion；Clear liquid B is adjusted to certain pH value by alkaline solution,
Certain time is stood under low temperature, filters and is washed with deionized to after without chlorion and obtain white precipitate D and settled solution E,
White precipitate D is frozen into white powder D；Settled solution E continuation is adjusted to certain pH value with alkaline solution, concentration,
Stand certain time under low temperature, F and filtrate G must be precipitated by being separated by filtration, precipitation F it is scrubbed, freeze-drying after be colourless thing F, filter
Liquid G be concentrated rear directly freezed it is dry white powder G；White thing C, white powder D infrared and standard bovine albumin
Infrared figure is completely the same, and water insoluble, is soluble in hydrochloric acid, it was demonstrated that two kinds of things are collagen；Colourless thing F infrared and standard
Guanine is basically identical, water insoluble, it was demonstrated that be impure guanine；White powder G is highly soluble in water, is also highly soluble in acid,
Infrared figure is consistent with the clear collagen of standard bovine, is marked as the water-soluble collagen peptide containing salt.
2. the method according to claim 1 for extracting simultaneously separate active ingredients simultaneously from fish scale, it is characterized in that：Used
Fish scale is the mixture of ocean fish, the fish scale of fresh-water fishes or two kinds of fish scales.
3. the method according to claim 1 for extracting simultaneously separate active ingredients simultaneously from fish scale, it is characterized in that described
Clean and the fish scale of decontamination refers to：The fish scale that market is purchased, is washed with water to no color and wash water solution without muddiness
Thing, other any processing are not done, is directly freeze-dried, is ground into thread fish scale.
4. the method according to claim 1 for extracting simultaneously separate active ingredients simultaneously from fish scale, it is characterized in that described mixed
Closing the extraction process of extract solution is：By hydrochloric acid solution body of the thread fish scale according to mass number and 0.050~0.82 mol/L concentration
Product is according to 1g:After 10 ~ 19mL is than mixing, it is placed in Vltrasonic device, power 35~71%, 20 ~ 40 minutes time and temperature 300C
Extracted；Insoluble matter is removed in centrifugation, obtains the mixed extract containing guanine, collagen peptide and collagen.
5. the method according to claim 4 for extracting simultaneously separate active ingredients simultaneously from fish scale, it is characterized in that described mixed
Closing the extraction process of the optimization of extract solution is：Thread fish scale quality is 1g with hydrochloric acid volume ratio：16.6mL, HCl concentration
0.33mol/L, ultrasonic power 57%, extraction time 28min, Extracting temperature is 300C。
6. the method according to claim 1 for extracting simultaneously separate active ingredients simultaneously from fish scale, it is characterized in that described
Concentration process is：The r/min of mixed extract 6000 centrifuges 20min, obtains filtrate, filtrate is rotated to be concentrated by evaporation to obtain concentrate.
7. the method according to claim 1 for extracting simultaneously separate active ingredients simultaneously from fish scale, it is characterized in that the glue
The separation of former albumen is：Concentrate is placed in 00C~10 0After C is stood overnight, it is separated by filtration, obtains precipitate A and clear liquid B；Precipitate A
It is washed with deionized to after without chlorion and white thing C is freeze-dried to obtain in freeze dryer；0.5 ~ 1mol/L of clear liquid B hydrogen
Sodium oxide molybdena regulation pH value be 6.0 ~ 6.5 after, also in 00C~10 0After C stand at low temperature is stayed overnight, by quantitative filter paper filtering and
Deionized water is washed, and obtains white precipitate D and settled solution E, white precipitate D is frozen into white powder D；It is white thing C, white
The powdered D's of color is infrared completely the same and water insoluble with the infrared figure of standard bovine albumin, is soluble in hydrochloric acid, it was demonstrated that two kinds
Thing is collagen.
8. the method according to claim 1 for extracting simultaneously separate active ingredients simultaneously from fish scale, it is characterized in that the bird
The separation of purine is：Settled solution E 0.05 ~ 0.2mol/L hydroxides as obtained by filtering after white precipitate D quantitative filter paper
Sodium adjusts pH value after 7.0-7.5, to concentrate, 00C~10 0C stand at low temperature is overnight to having clear liquid and precipitation, and being separated by filtration to sink
Shallow lake F and filtrate G, precipitation F is colourless thing F through water washing, after freeze-drying；Colourless thing F infrared and standard guanine basic one
Cause, it is water insoluble, it was demonstrated that to be impure guanine.
9. the method according to claim 1 for extracting simultaneously separate active ingredients simultaneously from fish scale, it is characterized in that the glue
The separation of former protein peptides is：The filtrate G after F must be precipitated by being separated by filtration, and rotary evaporation is steamed to anhydrous, then be tied in low temperature refrigerator
White powder G is freezed to obtain after ice in freeze drier；White powder G is highly soluble in water, is also highly soluble in acid, infrared figure and mark
Quasi- cow's serum collagen is consistent, is marked as the water-soluble collagen peptide containing salt.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110396093A (en) * | 2019-08-13 | 2019-11-01 | 广州怡和生物科技有限公司 | A kind of preparation method of guanine |
| CN114920825A (en) * | 2022-05-09 | 2022-08-19 | 自然资源部第三海洋研究所 | Rapid preparation method of fish collagen small peptide chelated calcium |
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| CN104324367A (en) * | 2014-10-20 | 2015-02-04 | 广西壮族自治区花红药业股份有限公司 | Novel application of fish scale extract in preparation of medicine for treating and/or preventing leukoderma |
| CN106119330A (en) * | 2016-08-09 | 2016-11-16 | 中国计量大学 | A kind of preparation method of fish scale collagen range of hydrolysed peptides |
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| JPH04173087A (en) * | 1990-11-05 | 1992-06-19 | Yuukishitsu Hiryo Seibutsu Kassei Riyou Gijutsu Kenkyu Kumiai | New microorganism |
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| CN110396093A (en) * | 2019-08-13 | 2019-11-01 | 广州怡和生物科技有限公司 | A kind of preparation method of guanine |
| CN114920825A (en) * | 2022-05-09 | 2022-08-19 | 自然资源部第三海洋研究所 | Rapid preparation method of fish collagen small peptide chelated calcium |
| CN114920825B (en) * | 2022-05-09 | 2024-03-22 | 自然资源部第三海洋研究所 | Rapid preparation method of fish collagen small peptide chelated calcium |
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Effective date of registration: 20200515 Address after: 510000 floor 1 and 2, building e, No. 9, Liangyuan North Road, Zhongluotan Town, Baiyun District, Guangzhou City, Guangdong Province Patentee after: Guangzhou Xiyan Biotechnology Co.,Ltd. Address before: 510000 unit 2414-2416, building, No. five, No. 371, Tianhe District, Guangdong, China Patentee before: GUANGDONG GAOHANG INTELLECTUAL PROPERTY OPERATION Co.,Ltd. Effective date of registration: 20200515 Address after: 510000 unit 2414-2416, building, No. five, No. 371, Tianhe District, Guangdong, China Patentee after: GUANGDONG GAOHANG INTELLECTUAL PROPERTY OPERATION Co.,Ltd. Address before: 223300 Huaian Changjiang Road, Jiangsu, No. 111 Patentee before: HUAIYIN NORMAL University |