CN107286352B - Extract the method for simultaneously separate active ingredients simultaneously from fish scale - Google Patents
Extract the method for simultaneously separate active ingredients simultaneously from fish scale Download PDFInfo
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- CN107286352B CN107286352B CN201710462868.7A CN201710462868A CN107286352B CN 107286352 B CN107286352 B CN 107286352B CN 201710462868 A CN201710462868 A CN 201710462868A CN 107286352 B CN107286352 B CN 107286352B
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- 241000251468 Actinopterygii Species 0.000 title claims abstract description 115
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000004480 active ingredient Substances 0.000 title claims abstract description 9
- 239000000284 extract Substances 0.000 title claims description 34
- 102000008186 Collagen Human genes 0.000 claims abstract description 116
- 108010035532 Collagen Proteins 0.000 claims abstract description 116
- 229920001436 collagen Polymers 0.000 claims abstract description 116
- UYTPUPDQBNUYGX-UHFFFAOYSA-N guanine Chemical compound O=C1NC(N)=NC2=C1N=CN2 UYTPUPDQBNUYGX-UHFFFAOYSA-N 0.000 claims abstract description 116
- 108090000765 processed proteins & peptides Proteins 0.000 claims abstract description 47
- 238000000605 extraction Methods 0.000 claims abstract description 25
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 59
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 42
- 239000000243 solution Substances 0.000 claims description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 40
- 239000002244 precipitate Substances 0.000 claims description 38
- 239000000843 powder Substances 0.000 claims description 34
- 239000007788 liquid Substances 0.000 claims description 33
- 238000001914 filtration Methods 0.000 claims description 30
- 238000000926 separation method Methods 0.000 claims description 30
- 239000000706 filtrate Substances 0.000 claims description 28
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- 239000002253 acid Substances 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 13
- 238000002390 rotary evaporation Methods 0.000 claims description 12
- 108091003079 Bovine Serum Albumin Proteins 0.000 claims description 11
- 239000012141 concentrate Substances 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
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 10
- 238000004108 freeze drying Methods 0.000 claims description 9
- 241000283690 Bos taurus Species 0.000 claims description 8
- KDCGOANMDULRCW-UHFFFAOYSA-N 7H-purine Chemical compound N1=CNC2=NC=NC2=C1 KDCGOANMDULRCW-UHFFFAOYSA-N 0.000 claims description 6
- 230000008014 freezing Effects 0.000 claims description 6
- 238000007710 freezing Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000012670 alkaline solution Substances 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
- 239000013505 freshwater Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 102000004196 processed proteins & peptides Human genes 0.000 claims description 3
- 238000005202 decontamination Methods 0.000 claims description 2
- 230000003588 decontaminative effect Effects 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000005457 optimization Methods 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 12
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000007812 deficiency Effects 0.000 abstract description 2
- 238000011160 research Methods 0.000 description 8
- 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
- 239000000470 constituent Substances 0.000 description 6
- 241000252230 Ctenopharyngodon idella Species 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000004833 fish glue Substances 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000002699 waste material Substances 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
- 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
- 239000003814 drug Substances 0.000 description 2
- 235000014103 egg white Nutrition 0.000 description 2
- 210000000969 egg white Anatomy 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
- 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
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 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
- 101710109488 Salt stress-induced protein Proteins 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
- 239000000908 ammonium hydroxide Substances 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
- 239000003795 chemical substances by application Substances 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
- 238000004140 cleaning Methods 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
- 235000013601 eggs Nutrition 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 239000012467 final product Substances 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
- 239000004615 ingredient Substances 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
- 239000012263 liquid product 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
- 102000039446 nucleic acids Human genes 0.000 description 1
- 108020004707 nucleic acids Proteins 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
- 108010048734 sclerotin Proteins 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
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 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 method that the invention discloses a kind of to extract simultaneously separate active ingredients simultaneously from fish scale, using fish scale as raw material, guanine, collagen peptide and collagen in fish scale is extracted simultaneously, the concentration and acidity and temperature for controlling extracting solution again, successively separate collagen, guanine and collagen peptide；The method of the present invention is using fish scale as raw material, onestep extraction simultaneously separates collagen, collagen peptide and guanine, and simple process takes full advantage of fish scale natural resources, the technological deficiency of the single extraction in current technology is overcome, there is apparent social value and economic benefit.
Description
Technical field
The present invention relates to biological extractive techniques, belong to fish sideline production deep process technology field, and especially one kind is same from fish scale
When extract and separation guanine, collagen peptide and collagen method.
Background technique
Fish scale (scale) is the sclerotin scale that the collagen of fish skin corium generates, and 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.Existing research table
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 the study found that fish scale contain it is more
Lecithin plays the role of enhancing memory, delays and prolong cell ageing；Contain a large amount of collagen in fish scale, can rise a variety of
Biological function, such as promote wound healing, hemostasis, antigenicity is lower, can promote the formation of bone, enhancing skin metabolism etc..
Fish scale collagen and other collagen ratios, protein easily decompose, are easy to be digested, absorb.It is a variety of contained in fish scale
Unsaturated fatty acid can be helped to transmit and chyle fat in the form of protein-bonded in blood, reduce cholesterol in blood vessel
It is deposited on wall, having prevents 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 gastric 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. and main medicine intermediate, it can be used for synthesizing a series of the anti-of high-efficiency low-toxicities
Bleb medicine.
China is that maximum freshwater fish culturing is national in the world.The leftover bits and pieces generated during processing of aquatic products every year
(such as fish-skin, fish-bone, crab shell, fish scale) reaches 2,500,000 tons or more [exploitation prospect [J] of Zhang Junjie, Zeng Qingxiao fish scale
Processing 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 collagen
Scape [J] aquatic science and technology information, 2007,34 (5): 210-212].How fish scale resource is utilized, so that it is turned waste into wealth, be in recent years
To be engaged in the hot spot of fishery process deeply industry research.To the deep processing and utilization of these fish scale wastes, has a large amount of research report
Road.Research is concentrated mainly on fish scale extraction 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 coupling reaction prepares fish scale collagen
The technical research of peptide, Jiangsu University's master thesis, 2014] and extract guanine or pearl essence or fish scale essence (fish
Silver) [Zeng Xiaodan, Zhang Yingjiao, Xia Chen, Wang Zipeng, Cao Yang grass carp scales extract the technique and quality research [J] of guanine,
Modern agriculture science and technology, 2012,1:15-16；A kind of method that pearl essence is extracted from fish scale of CN1033827A；
A kind of method 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 sum up are as follows: first fish scale cleans, cleans and dries 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 [chu knows gorgeous, Xiong Guangquan, Li Xin, Geng Shengrong, Yu Wei, Jiang Hongyou, Liao Tao grass carp scales
Preparation and analysis [J] food research and development of collagen peptide, 2014,35(7): 36-39;Zhang Huijie Hydrolyzed Collagen
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 thermal method glue handles the fish glue from scale obtained with acid solution and is referred to as acid-processed gelatin, is then referred to as with the fish glue from scale that base extraction obtains
Alkaline process glue, the fish glue from scale for taking protease to obtain are referred to as enzyme process glue or collagen peptide, and 103773828 A of CN is from fish scale
The method for extracting collagen；A kind of preparation method of acid-soluble fish scale collagen of 104892750 A of CN；
A kind of preparation method of fish scale collagen of CN101418328A；103773830 B one kind of CN extracts collagen egg from fish scale
White method；A kind of method that collagen is extracted from fish scale of 105063154 A of CN；103773830 B one kind of CN from
The method of 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 to there is Zeng Xiaodan et al. to mention from grass carp scales
Take the guanine [technique and quality research of Zeng Xiaodan, Zhang Yingjiao, Xia Chen, Wang Zipeng, Cao Yang grass carp scales extraction guanine
[J], modern agriculture science and technology, 2012,1:15-16], [CN1033827A one kind mentions two China's patent of invention from fish scale
The method for taking pearl essence；A kind of method that pearl essence is extracted from fish scale of CN201410730562.1].Previous literature method is
At 98 DEG C of temperature, surfactant is added and under the conditions of concentration is the hydrochloric acid of 5.0 moL/L in the fish scale that will have been pre-processed
Grass carp scales are extracted into 2.0 h, obtain quiescent crystallization after filtrate, and hydrochloric acid bird to obtain the final product after crystallization refine again with hydrochloric acid solution
Purine.Latter two patents method used surfactant in subsequent processing and had a significant impact to human body and environment four
Chlorination carbon.
Technology contents disclosed above be only to the collagen or collagen peptide or guanine of fish scale institute respectively into
Capable independent extraction.That is when extracting collagen or collagen peptide, guanine is not extracted；Extracting bird
When purine, collagen or collagen peptide are not extracted, when especially doing calcium remover with acid, have part collagen
It is dissolved in acid and loses.It is thus described above and method there is the wastes to loss and resource with important available ingredient
The problem of, and also have no so far in the industry with regard to how using fish scale while to extract the collagen of high value added product, collagen egg
White peptide and guanine and propose effective technical solution.Therefore, one kind is researched and developed from fish scale while being extracted active constituent and its being divided
From method, to improve production efficiency, reduce the wasting of resources it is very necessary.
Summary of the invention
The purpose of the present invention is: propose it is a kind of from fish scale and meanwhile extract and separate active ingredients method, from fish scale
Onestep extraction simultaneously isolates collagen, collagen peptide and guanine product with important physiological action, to realize fish scale
Efficient utilization.
The technical solution of the invention is as follows: using fish scale as raw material, by guanine, collagen peptide and the collagen in fish scale
Albumen extracts simultaneously, then controls the concentration and acidity and temperature of extracting solution, successively by collagen, guanine and collagen egg
White peptide is separated；Specific step is as follows: to cleaning with deimpurity fish scale after freeze-drying, being ground into Filamentous fish scale；
It after Filamentous fish scale is mixed according to certain solid-to-liquid ratio with Extraction solvent, is placed in Vltrasonic device, ultrasonic power, temperature in setting
It is extracted under degree and ultrasonic time, insoluble matter is removed in centrifuge separation, obtains mixed containing guanine, collagen peptide and collagen
Close extracting solution；Mixed extract is placed in rotary evaporating device and is concentrated to give concentrate；Concentrate is placed in quiet under low temperature
It sets to after there is precipitating and clear liquid, precipitate A and clear liquid B is obtained by filtration；Precipitate A freezes after being washed with deionized to no chloride ion
Dry white object C；After clear liquid B is adjusted to certain pH value by alkaline solution, stand certain time at low temperature, filtering and
White precipitate D and clear solution E are obtained after being washed with deionized to no chloride ion, white precipitate D is frozen into white powder
Shape D；Clear solution E continues after being adjusted to certain pH value with alkaline solution, concentration, stands certain time, filtering point at low temperature
From must precipitate F and filtrate G, precipitating F is washed, after freeze-drying is colourless object F, and it is dry that filtrate G is concentrated rear directly freezed
White powder G；White object C, white powder D it is infrared completely the same and not soluble in water with the infrared figure of standard bovine albumin,
It is soluble in hydrochloric acid, it was demonstrated that two kinds of objects are collagen；Colourless object F's is infrared almost the same with standard guanine, not soluble in water, card
Bright is impure guanine；White powder G is highly soluble in water, is also highly soluble in acid, infrared figure and the clear collagen of 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, clean and decontamination the fish scale refers to: the fish scale that market is purchased is washed with water to no color
With wash water solution without muddy object, other any processing are not done, are directly freeze-dried, Filamentous fish scale is ground into.
Wherein, the selection of Extraction solvent is such as to be gone with two kinds of standard sample guanines and collagen in different solvents
Ionized water, ammonium hydroxide, 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 the preferred solvent that hydrochloric acid solution is while extracting.
Wherein, the extraction process of mixed extract is: Filamentous fish scale is dense according to mass number and 0.050~0.82 mol/L
After the hydrochloric acid solution volume of degree is mixed according to 1g:10 ~ 19mL ratio, 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 centrifuge separation, obtains mixed containing guanine, collagen peptide and collagen
Close extracting solution.
Wherein, mixed extract is obtained under the extraction conditions using Uniform Design method；To collagen and
The recovery rate of collagen peptide is by photometry to the hydroxyl dried meat ammonia for representing collagen and collagen peptide in mixed extract
What acid was measured and calculated；Recovery rate to guanine is by high performance liquid chromatography to the guanine in mixed extract
It is detected and is calculated；The relationship of extraction conditions and recovery rate is fitted by 2003 software of Excel, has been obtained time
Return analysis equation, with this equation of partial differentiation solution, the extraction conditions optimized are as follows: the quality of Filamentous 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 300C。
Wherein, concentration process is: 6000 r/min of mixed extract is centrifuged 20min, obtains filtrate, filtrate is dense through rotary evaporation
Contract to obtain concentrate.
Wherein, the separation of collagen is: concentrate is placed in 00C~10 0It after C is stood overnight, is separated by filtration, is precipitated
A and clear liquid B；Precipitate A is freeze-dried to obtain white object C in freeze dryer after being washed with deionized to no chloride ion；Clear liquid B is used
After the sodium hydroxide adjusting pH value of 0.5 ~ 1mol/L is 6.0 ~ 6.5, also in 00C~10 0After C stand at low temperature is stayed overnight, pass through
Quantitative filter paper filtering and deionized water washing, obtain white precipitate D and clear solution E, white precipitate D is frozen into white powder
Shape D；White object C, white powder D it is infrared completely the same and not soluble in water with the infrared figure of standard bovine albumin, be soluble in
Hydrochloric acid, it was demonstrated that two kinds of objects are collagen.
Wherein, the separation of guanine is: by quantitative filter paper filter after white precipitate D resulting clear solution E with 0.05 ~
0.2mol/L sodium hydroxide adjusts pH value to be concentrated, 0 after 7.0-7.50C~10 0C stand at low temperature is overnight to there is clear liquid and heavy
It forms sediment, is separated by filtration to obtain precipitating F and filtrate G, precipitating F is colourless object F through water washing, after freeze-drying；The infrared and mark of colourless object F
Quasi- guanine is almost the same, not soluble in water, it was demonstrated that is impure guanine.
Wherein, the separation of collagen peptide is: it is separated by filtration to precipitate the filtrate G after F, rotary evaporation is steamed to anhydrous,
White powder G is lyophilized to obtain in freeze drier after freezing in low temperature refrigerator again；White powder G is highly soluble in water, also easily
It is dissolved in acid, infrared figure is consistent with the clear collagen of standard bovine, is marked as the water soluble collagen peptide containing salt.
The invention has the following advantages that
(1) present invention passes through simple washed with impurities step with fish scale, directly carries out the extraction of active constituent in fish scale simultaneously
And separation, it simplifies current existing patented technology or document fish scale makees raw material and extracts collagen or collagen peptide needs
The step of adding calcium remover to remove calcium, so that extraction process is easy.
(2) use certain density hydrochloric acid as extractant, while playing the role of a variety of: can dissolve collagen and
Guanine, can also be by part collagen acidolysis at collagen peptide, but also is acting on production subsequently through with sodium hydroxide
Salt plays the role of the effect for collagen being salted out and being removed calcium in fish scale.
(3) existing to be extracted in invention or the technical literature of collagen or collagen peptide using fish scale, in extraction process
In be only extracted fish scale single active ingredient, other useful components lose；The present invention is compared with these existing technologies, in fish scale
Collagen, collagen peptide and one step of guanine effective component is extracted and basic separation, take full advantage of fish scale
Natural resources overcomes the technological deficiency of single extraction.
Detailed description of the invention
Fig. 1 is process flow chart of the invention；Wherein: (1) being extraction optimization technological process figure；It (2) is to extract and separate
Process flow chart；
Fig. 2 is the white object C and standard bovine albumin infrared scan figure extracted；
Fig. 3 is the white object D extracted and the infrared scan figure of standard bovine albumin；
Fig. 4 is the colourless object F and guanine standard specimen infrared scan figure extracted；
Fig. 5 is the white object G extracted and the infrared scan figure of standard bovine albumin.
Specific embodiment
The present invention is specifically described below by embodiment.It must be noted that the embodiment provided, is only pair
Further explanation of the invention, should not be understood as limiting the scope of the invention, and the professional in the field can basis
The contents of the present invention make the modifications and adaptations of certain non-intrinsically safes.
Embodiment 1: extracting according to following steps and separates the active constituent in fish scale
(1) pretreatment of fish scale: the fish scale that market is purchased is washed with water to no color and wash water solution without muddiness
Object does not do other any processing, is directly freeze-dried, is ground into Filamentous fish scale；
(2) acquisition of mixed extract: 50.0g filiform fish scale is molten according to the hydrochloric acid of mass number and 0.050mol/L concentration
After liquid product is according to the mixing of 1g:10mL ratio, it is placed in Vltrasonic device, power 35%, 20 minutes time and temperature 300C is mentioned
It takes；Insoluble matter is removed in centrifuge separation, obtains the mixed extract containing guanine, collagen peptide and collagen；
(3) be concentrated: 6000 r/min of mixed extract is centrifuged 20min, obtains filtrate, filtrate is concentrated to give concentration through rotary evaporation
Liquid；
(4) separation of collagen: concentrate is placed in 00It after C is stood overnight, is separated by filtration, obtains precipitate A and clear liquid B；
Precipitate A is freeze-dried to obtain white object C 6.8g in freeze dryer after being washed with deionized to no chloride ion；Clear liquid B is used
After the sodium hydroxide adjusting pH value of 0.5mol/L is 6.0, also in 00After C stand at low temperature is stayed overnight, pass through quantitative filter paper mistake
Filter and deionized water washing, obtain white precipitate D and clear solution E, white precipitate D is frozen into white powder D 4.6g；
White object C, white powder D it is infrared completely the same and not soluble in water with the infrared figure of standard bovine albumin, be soluble in salt
Acid, it was demonstrated that two kinds of objects are collagen；
(5) separation of guanine: pass through resulting clear solution E 0.05mol/L after quantitative filter paper filtering white precipitate D
After sodium hydroxide adjusting pH value is 7.0, concentration, 00C stand at low temperature is separated by filtration to obtain precipitating F overnight to having clear liquid and precipitating
With filtrate G, precipitating F is colourless object F 0.24g through water washing, after freeze-drying；Colourless object F's is infrared infrared with standard guanine
It is almost the same, it is not soluble in water, it was demonstrated that be impure guanine；
(6) separation of collagen peptide: being separated by filtration to precipitate the filtrate G after F, and rotary evaporation is steamed to anhydrous, then
White powder G 5.2g is lyophilized to obtain in freeze drier after freezing in low temperature refrigerator；White powder G is highly soluble in water, also easily
It is dissolved in acid, the infrared figure of white powder G is consistent with the standard bovine infrared figure of clear collagen, is marked as the water-soluble glue containing salt
Former protein peptides.
Embodiment 2: extracting according to following steps and separates the active constituent in fish scale
(1) pretreatment of fish scale: the fish scale that market is purchased is washed with water to no color and wash water solution without muddiness
Object does not do other any processing, is directly freeze-dried, is ground into Filamentous fish scale；
(2) 50.0g filiform fish scale the acquisition of mixed extract: is pressed to the hydrochloric acid solution of mass number and 0.45mol/L concentration
After volume is mixed according to 1g:14.5mL ratio, it is placed in Vltrasonic device, power 53%, 30 minutes time and temperature 300C is mentioned
It takes；Insoluble matter is removed in centrifuge separation, obtains the mixed extract containing guanine, collagen peptide and collagen；
(3) be concentrated: 6000 r/min of mixed extract is centrifuged 20min, obtains filtrate, filtrate is concentrated to give concentration through rotary evaporation
Liquid；
(4) separation of collagen: concentrate is placed in 50It after C is stood overnight, is separated by filtration, obtains precipitate A and clear liquid B；
Precipitate A is freeze-dried to obtain white object C 13.8g in freeze dryer after being washed with deionized to no chloride ion；Clear liquid B is used
After the sodium hydroxide adjusting pH value of 0.75mol/L is 6.3, also in 50After C stand at low temperature is stayed overnight, pass through quantitative filter paper mistake
Filter and deionized water washing, obtain white precipitate D and clear solution E, white precipitate D is frozen into white powder D 11.1g；
White object C, white powder D it is infrared completely the same and not soluble in water with the infrared figure of standard bovine albumin, be soluble in salt
Acid, it was demonstrated that two kinds of objects are collagen；
(5) separation of guanine: pass through 0.13 mol/ of resulting clear solution E after quantitative filter paper filtering white precipitate D
After L sodium hydroxide adjusting pH value is 7.5, concentration, 50C stand at low temperature is separated by filtration to obtain precipitating F overnight to having clear liquid and precipitating
With filtrate G, precipitating F is colourless object F 0.28g through water washing, after freeze-drying；Colourless object F's is infrared basic with standard guanine
Unanimously, not soluble in water, it was demonstrated that be impure guanine；
(6) separation of collagen peptide: being separated by filtration to precipitate the filtrate G after F, and rotary evaporation is steamed to anhydrous, then
White powder G 8.6g is lyophilized to obtain in freeze drier after freezing in low temperature refrigerator；White powder G is highly soluble in water, also pole
It is soluble 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: extracting according to following steps and separates the active constituent in fish scale
(1) pretreatment of fish scale: the fish scale that market is purchased is washed with water to no color and wash water solution without muddiness
Object does not do other any processing, is directly freeze-dried, is ground into Filamentous fish scale；
(2) 50.0g filiform fish scale the acquisition of mixed extract: is pressed to the hydrochloric acid solution of mass number and 0.82 mol/L concentration
After volume is mixed according to 1g:19mL ratio, it is placed in Vltrasonic device, power 71%, 40 minutes time and temperature 300C is extracted；
Insoluble matter is removed in centrifuge separation, obtains the mixed extract containing guanine, collagen peptide and collagen；
(3) be concentrated: 6000 r/min of mixed extract is centrifuged 20min, obtains filtrate, filtrate is concentrated to give concentration through rotary evaporation
Liquid；
(4) separation of collagen: concentrate is placed in 100It after C is stood overnight, is separated by filtration, obtains precipitate A and clear liquid
B；Precipitate A is freeze-dried to obtain white object C 15.6g in freeze dryer after being washed with deionized to no chloride ion；Clear liquid B is used
After the sodium hydroxide adjusting pH value of 1mol/L is 6.5, also in 100After C stand at low temperature is stayed overnight, filtered by quantitative filter paper
And deionized water washing, white precipitate D and clear solution E are obtained, white precipitate D is frozen into white powder D 12.1g；It is white
Color object C, the infrared figure of white powder D and the infrared figure of standard bovine albumin are completely the same and not soluble in water, are soluble in salt
Acid, it was demonstrated that two kinds of objects are collagen；
(5) separation of guanine: pass through resulting clear solution E 0.2mol/L after quantitative filter paper filtering white precipitate D
After sodium hydroxide adjusting pH value is 7.5, concentration, 100C stand at low temperature is separated by filtration to obtain precipitating overnight to having clear liquid and precipitating
F and filtrate G, precipitating F is colourless object F 0.33g through water washing, after freeze-drying；The infrared figure and standard guanine of colourless object F
Infrared figure is almost the same, not soluble in water, it was demonstrated that is impure guanine；
(6) separation of collagen peptide: being separated by filtration to precipitate the filtrate G after F, and rotary evaporation is steamed to anhydrous, then
White powder G 9.2g is lyophilized to obtain in freeze drier after freezing in low temperature refrigerator；White powder G is highly soluble in water, also easily
It is dissolved in acid, the infrared figure of white powder G is consistent with the standard bovine infrared figure of clear collagen, is marked as the water-soluble collagen containing salt
Protein peptides.
Embodiment 4: extracting according to following steps and separates the active constituent in fish scale
(1) pretreatment of fish scale: the fish scale that market is purchased is washed with water to no color and wash water solution without muddiness
Object does not do other any processing, is directly freeze-dried, is ground into Filamentous fish scale；
(2) 50.0g filiform fish scale the acquisition of mixed extract: is pressed to the hydrochloric acid solution of mass number and 0.33mol/L concentration
After volume is mixed according to 1g:16.6mL ratio, it is placed in Vltrasonic device, power 57%, 28 minutes time and temperature 300C is mentioned
It takes；Insoluble matter is removed in centrifuge separation, obtains the mixed extract containing guanine, collagen peptide and collagen；
(3) be concentrated: 6000 r/min of mixed extract is centrifuged 20min, obtains filtrate, filtrate is concentrated to give concentration through rotary evaporation
Liquid；
(4) separation of collagen: concentrate is placed in 50It after C is stood overnight, is separated by filtration, obtains precipitate A and clear liquid B；
Precipitate A is freeze-dried to obtain white object C 17.1g in freeze dryer after being washed with deionized to no chloride ion；Clear liquid B 1mol/
After the sodium hydroxide adjusting pH value of L is 6.0, also in 50C stand at low temperature overnight after, by quantitative filter paper filter and go from
Sub- water washing, obtains white precipitate D and clear solution E, and white precipitate D is frozen into white powder D 12.5g；White object C,
White powder D's is infrared completely the same and not soluble in water with the infrared figure of standard bovine albumin, is soluble in hydrochloric acid, it was demonstrated that two
Kind object is collagen；
(5) separation of guanine: pass through resulting clear solution E 0.05mol/L after quantitative filter paper filtering white precipitate D
After sodium hydroxide adjusting pH value is 7.5, concentration, 100C stand at low temperature is separated by filtration to obtain precipitating overnight to having clear liquid and precipitating
F and filtrate G, precipitating F is colourless object F 0.42g through water washing, after freeze-drying；The infrared and standard guanyl- of colourless object F
This is consistent, not soluble in water, it was demonstrated that is impure guanine；
(6) separation of collagen peptide: being separated by filtration to precipitate the filtrate G after F, and rotary evaporation is steamed to anhydrous, then
White powder G 10.5g is lyophilized to obtain in freeze drier after freezing in low temperature refrigerator；White powder G is highly soluble in water, also pole
It is soluble 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, technical solution according to the present invention and given specific embodiment and relevant detection data card
Real, the present invention reaches expected goal of the invention.
Claims (4)
1. the method for extracting simultaneously separate active ingredients simultaneously from fish scale, using fish scale as raw material, by guanine, the collagen in fish scale
Protein peptides and collagen extract simultaneously, then control the concentration and acidity and temperature of extracting solution, successively by collagen, bird
Purine and collagen peptide are separated；It is characterized in that it specific step is as follows: to clean and deimpurity fish scale through being subcooled
Be lyophilized it is dry after, be ground into Filamentous fish scale；After Filamentous fish scale is mixed according to certain solid-to-liquid ratio with Extraction solvent, it is placed in ultrasonic dress
In setting, extracted under the ultrasonic power of setting, temperature and ultrasonic time, centrifuge separation remove insoluble matter, obtain containing guanine,
The mixed extract of collagen peptide and collagen；Mixed extract is placed in rotary evaporating device be concentrated to give it is dense
Contracting liquid；Concentrate, which is placed under low temperature, to be stood to after there is precipitating and clear liquid, and precipitate A and clear liquid B is obtained by filtration；Precipitate A spend from
White object C is freeze-dried to obtain after sub- water washing to no chloride ion；After clear liquid B is adjusted to certain pH value by alkaline solution,
Certain time is stood under low temperature, white precipitate D and clear solution E are obtained after filtering and be washed with deionized to no chloride ion,
White precipitate D is frozen into white powder D；Clear solution E continues after being adjusted to certain pH value with alkaline solution, concentration,
Stand certain time under low temperature, be separated by filtration to obtain precipitating F and filtrate G, precipitating F it is washed, freeze-drying after be colourless object F, filter
Liquid G be concentrated rear directly freezed it is dry white powder G；The infrared and standard bovine albumin of white object C, white powder D
Infrared figure is completely the same, and not soluble in water, is soluble in hydrochloric acid, it was demonstrated that two kinds of objects are collagen；The infrared and standard of colourless object F
Guanine is almost the same, not soluble in water, it was demonstrated that is 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；
The extraction process of the mixed extract is: by Filamentous fish scale according to mass number and 0.050~0.82 mol/L concentration
Hydrochloric acid solution volume according to 1g:10 ~ 19mL ratio mix after, be placed in Vltrasonic device, power 35~71%, 20 ~ 40 minutes time and
30 DEG C of temperature extract；Insoluble matter is removed in centrifuge separation, obtains the mixing containing guanine, collagen peptide and collagen and mentions
Take liquid；
The concentration process is: 6000 r/min of mixed extract is centrifuged 20min, obtains filtrate, filtrate is concentrated through rotary evaporation
Obtain concentrate；
The separation of the collagen is: concentrate be placed in 0 DEG C ~ 10 DEG C stand overnight after, be separated by filtration, obtain precipitate A
With clear liquid B；Precipitate A is freeze-dried to obtain white object C in freeze dryer after being washed with deionized to no chloride ion；Clear liquid B is with 0.5
After the sodium hydroxide adjusting pH value of ~ 1mol/L is 6.0 ~ 6.5, after being stayed overnight also in 0 DEG C ~ 10 DEG C stand at low temperature, pass through
Quantitative filter paper filtering and deionized water washing, obtain white precipitate D and clear solution E, white precipitate D is frozen into white powder
Shape D；White object C, white powder D it is infrared completely the same and not soluble in water with the infrared figure of standard bovine albumin, be soluble in
Hydrochloric acid, it was demonstrated that two kinds of objects are collagen；
The separation of the guanine is: by quantitative filter paper filter after white precipitate D resulting clear solution E with 0.05 ~
0.2mol/L sodium hydroxide adjusts concentration after pH value is 7.0-7.5, in 0 DEG C ~ 10 DEG C stand at low temperature overnight to there is clear liquid and heavy
It forms sediment, is separated by filtration to obtain precipitating F and filtrate G, precipitating F is colourless object F through water washing, after freeze-drying；The infrared and mark of colourless object F
Quasi- guanine is almost the same, not soluble in water, it was demonstrated that is impure guanine；
The separation of the collagen peptide is: being separated by filtration to precipitate the filtrate G after F, rotary evaporation is steamed to anhydrous, then low
White powder G is lyophilized to obtain in freeze drier after freezing in temperature refrigerator；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 be ocean fish, the fish scale of fresh-water fishes or two kinds of fish scales mixture.
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
Object does not do other any processing, is directly freeze-dried, is ground into Filamentous 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
The extraction process for closing the optimization of extracting solution is: Filamentous fish scale quality is 1g:16.6mL, HCl concentration with hydrochloric acid volume ratio
0.33mol/L, ultrasonic power 57%, extraction time 28min, Extracting temperature are 30 DEG C.
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Citations (4)
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| JPH04173087A (en) * | 1990-11-05 | 1992-06-19 | Yuukishitsu Hiryo Seibutsu Kassei Riyou Gijutsu Kenkyu Kumiai | New microorganism |
| CN103540635A (en) * | 2013-09-23 | 2014-01-29 | 石狮海星食品有限公司 | Preparation process of fish scale collagen protein |
| 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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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04173087A (en) * | 1990-11-05 | 1992-06-19 | Yuukishitsu Hiryo Seibutsu Kassei Riyou Gijutsu Kenkyu Kumiai | New microorganism |
| CN103540635A (en) * | 2013-09-23 | 2014-01-29 | 石狮海星食品有限公司 | Preparation process of fish scale collagen protein |
| 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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