CN103409489A - Preparation method for fish collagen antioxidant peptide - Google Patents
Preparation method for fish collagen antioxidant peptide Download PDFInfo
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- CN103409489A CN103409489A CN2013103549444A CN201310354944A CN103409489A CN 103409489 A CN103409489 A CN 103409489A CN 2013103549444 A CN2013103549444 A CN 2013103549444A CN 201310354944 A CN201310354944 A CN 201310354944A CN 103409489 A CN103409489 A CN 103409489A
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Abstract
The invention provides a preparation method for fish collagen antioxidant peptide, which relates to a collagen. The preparation method comprises the following steps: with a fish-skin or fish scale as a raw material, soaking the raw material with an alkaline solution containing absolute ethyl alcohol, removing impurity proteins and fat, rinsing the raw material with clear water until the raw material is neutral, then soaking the raw material with an acidic solution and rinsing the raw material with clear water until the raw material is neutral; adding composite protease into the pretreated fish-skin or fish scale for enzymatic hydrolysis so as to obtain fish collagen enzymatic hydrolysate; heating the fish collagen enzymatic hydrolysate, carrying out enzyme deactivation, then filtering the fish collagen enzymatic hydrolysate to remove insoluble substances and removing amino acids and salts by using a nanofiltration membrane so as to obtain a fish collagen peptide solution; preparing a fish collagen antioxidant peptide solution by adding a hydrophobic adsorbent into the fish collagen peptide solution, standing the solution for adsorption, adding an organic solvent into the hydrophobic adsorbent after filtration and then carrying out filtering so as to obtain the fish collagen antioxidant peptide solution; and removing the organic solvent in the fish collagen antioxidant peptide solution through vacuum heating evaporation and carrying out spray drying or freeze drying so as to prepare the fish collagen antioxidant peptide with an antioxidant function.
Description
Technical field
The present invention relates to a kind of collagen protein, especially relate to utilize hydrophobic adsorbent to collagen protein enzymolysis liquid adsorb, the preparation of the method for wash-out, have the preparation method of a kind of collagen anti-oxidation peptide of good anti-oxidant function.
Background technology
Collagen protein is the dermis of skin important component part, but with advancing age, the renewal rate of skin collagen descends gradually, therefore needs timely replenishing collagen.Collagen peptide is a kind of hydrolytic collagen polypeptide of small molecules amount, and the collagen run off for skin can award timely reparation, and then improves the water retention capacity of skin, delay skin aging.On the other hand, research shows, in human body, excessive free radical can destroy lipid, protein and DNA and causes various damages, and the senescence process that accelerates body also brings out various diseases.Although natural and synthetized oxidation preventive agent can play the effect of removing free radical, can there be certain potential safety hazard in the use of synthetized oxidation preventive agent such as butylated hydroxy anisole (BHA).Along with the development of Chinese society, the quickening of rhythm of life and the raising of health care consciousness, natural, safe antioxidant has received increasing concern.And, along with people deepen continuously to the understanding of effective constituent in oceanic resources, the interest of the biologically active substance that is derived from aquatic animal is constantly increased.
Owing in human inner cell's film, containing a large amount of polybasic unsaturated fatty acids, the collagen peptide with good lipophilic hydrophobic structure will be brought into play better effect in vivo.
China Agricultural University has reported and has been derived from anti-oxidation peptide of collagen protein and uses thereof in Chinese patent CN101824071A, disclose a series of anti-oxidation peptides that are derived from collagen protein, and it has one of following aminoacid sequence: (1) Hyl-Cys; (2) Gln-Gly-Ala-Arg; (3) Leu-Gln-Gly-Met; (4) Leu-Gln-Gly-Met-Hyp; This anti-oxidation peptide can be synthetic by polypeptide instrument chemical process, also can be by by collagen hydrolysate, and the hydrolysate separation and purification that then will obtain and obtaining.The applicant provides a kind of extraction preparation method of small molecules collagen of fish skin peptide in Chinese patent CN102703555A, the fish-skin of fresh-water fishes of take is raw material, remove noncollagen protein, through degreasing, de-raw meat, the step such as grind, under acidic conditions, the collagen protein heating hydrolysis is processed, then adopt enzymolysis process to control the palliating degradation degree of collagen protein, adopt membrane separation process to obtain the target micromolecular collagen peptide and to the proteolytic enzyme recycling, then by the nanofiltration desalination, after gac binding resin decoloration deodorization, utilize spraying drying to obtain the small molecules collagen of fish skin Gly-His-Lys of colorless and odorless.But foregoing invention has all been ignored the extraction preparation of lipophilic hydrophobic structure collagen peptide.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of collagen anti-oxidation peptide with good anti-oxidant function.
The present invention includes following steps:
1) pre-treatment of raw material: take fish-skin or fish scale is raw material, soaks with the basic solution that contains dehydrated alcohol, remove after foreign protein and fat with the clear water rinsing to neutral, then after with acidic solution, soaking, with the clear water rinsing to neutral;
2) enzymolysis: add compound protease in pretreated fish-skin or fish scale, after enzymolysis, obtain the Isin glue collagen enzymolysis solution;
3) enzyme filters, goes out: the Isin glue collagen enzymolysis solution heating that will obtain, after the enzyme that goes out, filter, and remove insolubles, then utilize nanofiltration membrane to remove amino acid and salinity, obtain collagen peptide solution;
4) preparation of collagen anti-oxidation peptide solution: in collagen peptide solution, add hydrophobic adsorbent, standing adsorption, after filtration, add organic solvent in hydrophobic adsorbent, after filtration, obtains collagen anti-oxidation peptide solution;
5) preparation of collagen anti-oxidation peptide: utilize the organic solvent in heating under vacuum evaporative removal collagen anti-oxidation peptide solution, by spraying drying or lyophilize, be prepared into the collagen anti-oxidation peptide with anti-oxidant function, prepared collagen anti-oxidation peptide is Powdered.
In step 1) in, described fish-skin or fish scale can adopt a kind of fish-skin or the fish scale in fresh-water fishes, sea water fish; The concentration expressed in percentage by volume of described dehydrated alcohol can be 20%; The described add-on that contains the basic solution of dehydrated alcohol can be 2～5 times of raw material; The condition that described basic solution soaks can be: basic solution is 0.01～0.05M NaOH solution, and the temperature of immersion is 4～20 ℃, and the time of immersion is 12～24h; The add-on of described acidic solution can be 2～5 times of raw material; The condition that described acidic solution soaks can be: acidic solution is 0.05～0.20M HCl solution, and the temperature of immersion is 4～20 ℃, and the time of immersion is 1～3h.
In step 2) in, described compound protease can be selected from least two kinds in Collagenase, Sumizyme MP, trypsinase, papoid, bromeline, neutral protease etc.; The add-on of compound protease can be 0.1%～0.5% of raw materials quality by mass percentage; The condition of described enzymolysis can be in 40～60 ℃ of lower enzymolysis 2～6h.
In step 3) in, the temperature of described heating can be 90～100 ℃, and the time of heating can be 5～15min; Described filtration can be adopted Plate Filtration or centrifuging; The molecular weight cut-off of described nanofiltration membrane can be 200 dalton.
In step 4) in, described hydrophobic adsorbent can be selected from least a in gac, ion exchange resin, macroporous adsorbent resin etc.; The add-on of described hydrophobic adsorbent can be 1%～5% of collagen peptide solution by mass percentage; The time of described standing adsorption can be 30～90min; The composition of described organic solvent can be: the volume ratio of dehydrated alcohol/acetic acid/water is 50/ (0.5～2.5)/(49.5～47.5); The add-on of described organic solvent can be 2～5 times of hydrophobic adsorbent in mass ratio.
In step 5) in, the temperature of described heating under vacuum evaporation can be 50～80 ℃.
The present invention be take fish-skin or fish scale and is raw material, remove noncollagen protein, adopt compound protease to carry out enzymolysis, after enzymolysis solution is removed amino acid and salt by nanofiltration membrane, utilize the preparation methods such as hydrophobic adsorbent adsorbs, organic solvent wash-out, then the means such as organic solvent, drying of removing by heating evaporation prepare collagen peptide.In collagen peptide prepared by the present invention, hydrophobic amino acid content is high, and molecular weight is concentrated and is distributed in 300～2000Da, has good anti-oxidant function, can be widely used in the industries relevant to HUMAN HEALTH such as protective foods, biological medicine, makeup.
In human inner cell's film, contain a large amount of polybasic unsaturated fatty acids, easily oxidized.Antioxidant can be for the chain reaction of oil-control autoxidation.Yet the research of at present relevant collagen peptide mainly concentrates on the extraction of wetting ability collagen peptide, the collagen peptide of preparation is not owing to being soluble in grease, and range of application is subject to certain restrictions.The present invention utilizes hydrophobic adsorbent to adsorb the Isin glue collagen enzymolysis solution; the organic solvents such as recycling alcohol, acetic acid carry out the collagen peptide that wash-out is prepared into will have good lipophilic hydrophobic structure; can be inserted in the microbial film of unsaturated fatty acids existence the effect of performance anti-oxidation protection.Treatment condition gentleness of the present invention, can reclaim the hydrophobicity collagen peptide in the decoloration process of collagen peptide, effectively utilizes collagen protein enzymolysis thing, reduces production costs.Therefore the present invention has the following advantages:
1, the collagen peptide for preparing of the present invention has good anti-oxidant function.
2, the collagen peptide for preparing of the present invention contains a large amount of hydrophobic amino acids, will have good oleophylic function.
3, the molecular weight of the collagen peptide for preparing of the present invention is mainly concentrated and is distributed in 300～3000Da, is conducive to the absorption of human body utilization.
4, the preparation technology of the present invention hydrophobicity collagen peptide that can run off for reclaiming the collagen peptide decolorization, environmental contamination reduction, reduce the production cost of collagen peptide.
5, the present invention utilizes fish-skin, fish scale etc. to prepare the collagen peptide that has good anti-oxidant function, contains a large amount of hydrophobic groupings, the collagen that not only can run off for supplementing skin, can also remove interior free yl, will on the industry relevant to HUMAN HEALTH such as medicine, the cosmetics of super quality, protective foods, have a good application prospect.
The accompanying drawing explanation
Fig. 1 is the high performance liquid phase collection of illustrative plates of the collagen anti-oxidation peptide molecular weight distribution of embodiment 1 preparation.
Fig. 2 is the high performance liquid phase collection of illustrative plates of the collagen anti-oxidation peptide molecular weight distribution of embodiment 2 preparations.
Fig. 3 is the high performance liquid phase collection of illustrative plates of the collagen anti-oxidation peptide molecular weight distribution of embodiment 3 preparations.
Fig. 4 is the high performance liquid phase collection of illustrative plates of the collagen anti-oxidation peptide molecular weight distribution of embodiment 4 preparations.
Embodiment
The present invention is further illustrated in connection with accompanying drawing for following examples.
Embodiment 1
The 0.01M NaOH solution that contains 20% (v/v) dehydrated alcohol that adds 20L in 10kg tilapia fish scale, under 20 ℃, soak 24h, after utilizing the tap water rinsing clean, add the 0.05M HCl solution of 20L to soak 3h under 20 ℃, extremely neutral with the tap water rinsing, utilize the fish scale after the separate type high-density paste mill will be processed to grind, the compound protease (25g Collagenase and 25g papoid) that adds 50g, at 40 ℃ of lower enzymolysis 2h, 100 ℃ of heating 15min enzymes that go out, filter and remove insolubles, utilizing molecular weight cut-off is after 200 daltonian nanofiltration membrane are removed amino acid and salinity, acquisition Brix is 12% collagen protein peptide solution 20L, through being cooled to room temperature, add the 1000g macroporous adsorbent resin, after standing 30min, filter, in the macroporous adsorbent resin obtained, add 2000ml to contain the machine solvent aqueous solution of 50% (v/v) alcohol and 2.5% (v/v) acetic acid, at room temperature stir 15min, filter and obtain collagen peptide solution, utilize Rotary Evaporators to remove organic solvent under 50 ℃ of heating under vacuum, spraying drying obtains the collagen peptide powder of 220g left and right.The high performance liquid phase collection of illustrative plates of the collagen anti-oxidation peptide molecular weight distribution of embodiment 1 preparation is referring to Fig. 1.
Embodiment 2
The 0.01M NaOH solution that contains 20% (v/v) dehydrated alcohol that adds 30L in 10kg large yellow croaker fish scale, under 20 ℃, soak 18h, after utilizing the tap water rinsing clean, add the 0.05M HCl solution of 30L to soak 2h under 20 ℃, extremely neutral with the tap water rinsing, utilize the fish scale after the separate type high-density paste mill will be processed to grind, the compound protease (20g Sumizyme MP and 20g neutral protease) that adds 40g, at 45 ℃ of lower enzymolysis 4h, 100 ℃ of heating 15min enzymes that go out, filter and remove insolubles, utilizing molecular weight cut-off is after 200 daltonian nanofiltration membrane are removed amino acid and salinity, acquisition Brix is 13% collagen protein peptide solution 18L, through being cooled to room temperature, add 700g ion exchange resin, after standing 45min, filter, in the gac obtained, add 2100ml to contain the aqueous solutions of organic solvent of 50% (v/v) alcohol and 1.5% (v/v) acetic acid, at room temperature stir 20min, filter and obtain collagen peptide solution, utilize Rotary Evaporators to remove organic solvent under 60 ℃ of heating under vacuum, spraying drying obtains the collagen peptide powder of 230g left and right.The high performance liquid phase collection of illustrative plates of the collagen anti-oxidation peptide molecular weight distribution of embodiment 2 preparations is referring to Fig. 2.
Embodiment 3
The 0.01M NaOH solution that contains 20% (v/v) dehydrated alcohol that adds 40L in 10kg shark fish-skin, under 20 ℃, soak 15h, after utilizing the tap water rinsing clean, add the 0.05M HCl solution of 40L to soak 2h under 20 ℃, extremely neutral with the tap water rinsing, utilize the fish-skin after the separate type high-density paste mill will be processed to grind, the compound protease (10g trypsinase and 10g papoid) that adds 20g, at 50 ℃ of lower enzymolysis 5h, 100 ℃ of heating 10min enzymes that go out, filter and remove insolubles, utilizing molecular weight cut-off is after 200 daltonian nanofiltration membrane are removed amino acid and salinity, acquisition Brix is 15% collagen protein peptide solution 16L, through being cooled to room temperature, add the 320g gac, after standing 60min, filter, in the gac obtained, add 1000ml to contain the aqueous solutions of organic solvent of 50% (v/v) alcohol and 1.0% (v/v) acetic acid, at room temperature stir 25min, filter and obtain collagen peptide solution, utilize Rotary Evaporators to remove organic solvent under 70 ℃ of heating under vacuum, lyophilize obtains the collagen peptide powder of 320g left and right.The high performance liquid phase collection of illustrative plates of the collagen anti-oxidation peptide molecular weight distribution of embodiment 3 preparations is referring to Fig. 3.
Embodiment 4
The 0.01M NaOH solution that contains 20% (v/v) dehydrated alcohol that adds 50L in the 10kg tilapia fishskin, under 20 ℃, soak 12h, after utilizing the tap water rinsing clean, add the 0.05M HCl solution of 50L to soak 1h under 20 ℃, extremely neutral with the tap water rinsing, utilize the fish-skin after the separate type high-density paste mill will be processed to grind, the compound protease (5g trypsinase and 5g bromeline) that adds 10g, at 60 ℃ of lower enzymolysis 6h, 100 ℃ of heating 5min enzymes that go out, filter and remove insolubles, utilizing molecular weight cut-off is after 200 daltonian nanofiltration membrane are removed amino acid and salinity, acquisition Brix is 15% collagen protein peptide solution 15L, through being cooled to room temperature, add the 150g gac, after standing 90min, filter, in the gac obtained, add 750ml to contain the aqueous solutions of organic solvent of 50% (v/v) alcohol and 0.5% (v/v) acetic acid, at room temperature stir 30min, filter and obtain collagen peptide solution, utilize Rotary Evaporators to remove organic solvent under 80 ℃ of heating under vacuum, lyophilize obtains the collagen peptide powder of 300g left and right.The high performance liquid phase collection of illustrative plates of the collagen anti-oxidation peptide molecular weight distribution of embodiment 4 preparations is referring to Fig. 4.
The present invention utilizes high performance liquid chromatograph to measure the molecular weight distribution of the collagen peptide of the present invention's production, and result is as shown in Fig. 1～4.As can be known by Fig. 1～4, the molecular weight of collagen anti-oxidation peptide prepared by the present invention mainly is distributed in 300～2000 dalton, and (embodiment 2 is 1150Da and 390Da wherein to utilize the molecular weight of collagen peptide prepared by macroporous resin (embodiment 1) to concentrate on 470 dalton (Da) near zone; Embodiment 3 is 1800Da and 460Da; Embodiment 4 be 2000Da, 1230 and 400Da).It is reported, compare with amino acid and protein polypeptide, lower than 2000 daltonian oligopeptides, not only be easy to the absorption of human body metabolism, and have good biological activity.DPPH free radical and the Scavenging action to hydroxyl free radical of collagen anti-oxidation peptide to preparation measured, if shown in result table 1.As shown in Table 1, although the DPPH radical scavenging activity of the collagen peptide of embodiment 1～4 preparation also has a certain distance with gsh, but hydroxy radical qiao is removed ability near gsh, shows and utilizes collagen peptide prepared by the present invention to have good resistance of oxidation.Utilize amino acidanalyser to analyze (table 2) to the amino acid composition of collagen anti-oxidation peptide, found that, hydrophobic amino acid ratio in the collagen anti-oxidation peptide of preparation can reach 40.3%～58.6%, apparently higher than 30% left and right of Isin glue collagen enzymolysis solution.And some document think glycine between polarity and nonpolar between, in biology, generally also it is classified as nonpolar.Therefore in the collagen anti-oxidation peptide for preparing of the present invention, the hydrophobic amino acid ratio can be up to more than 70%, to have good lipophilic hydrophobic structure, anti-oxidation peptide can be strengthened with the interaction with the hydrophobicity polyunsaturated fatty acid in vivo, and then suppress the lipid peroxidation chain reaction, therefore can be widely used in the industries such as protective foods, biological medicine, makeup.
In sum, the present invention is to utilizing compound protease to carry out enzymolysis through pretreated fish-skin or fish scale, after enzymolysis solution is removed amino acid and salt by nanofiltration membrane, utilize the preparation methods such as hydrophobic adsorbent adsorbs, organic solvent wash-out, then the means such as organic solvent, drying of removing by heating evaporation prepare collagen peptide.Technique of the present invention can be carried out combination with conventional collagen peptide production technique, decoloration process, the hydrophobicity collagen peptide run off in the decoloration process of efficient recovery collagen peptide, and environmental contamination reduction, save production cost; The small molecules collagen peptide of preparation has good anti-oxidant function, enlarges the range of application of collagen peptide.
It should be noted that: the fish-skin that the present invention is used or fish scale can be a kind of in fresh-water fishes or sea water fish.
Table 1 be the collagen anti-oxidation peptide antioxidant property (half-inhibition concentration, IC50)
The amino acid composition analysis of table 2 collagen anti-oxidation peptide (individual/1000 amino-acid residues)
Annotate: * is hydrophobic amino acid.
Claims (10)
1. the preparation method of a collagen anti-oxidation peptide is characterized in that comprising the following steps:
1) pre-treatment of raw material: take fish-skin or fish scale is raw material, soaks with the basic solution that contains dehydrated alcohol, remove after foreign protein and fat with the clear water rinsing to neutral, then after with acidic solution, soaking, with the clear water rinsing to neutral;
2) enzymolysis: add compound protease in pretreated fish-skin or fish scale, after enzymolysis, obtain the Isin glue collagen enzymolysis solution;
3) enzyme filters, goes out: the Isin glue collagen enzymolysis solution heating that will obtain, after the enzyme that goes out, filter, and remove insolubles, then utilize nanofiltration membrane to remove amino acid and salinity, obtain collagen peptide solution;
4) preparation of collagen anti-oxidation peptide solution: in collagen peptide solution, add hydrophobic adsorbent, standing adsorption, after filtration, add organic solvent in hydrophobic adsorbent, after filtration, obtains collagen anti-oxidation peptide solution;
5) preparation of collagen anti-oxidation peptide: utilize the organic solvent in heating under vacuum evaporative removal collagen anti-oxidation peptide solution, by spraying drying or lyophilize, be prepared into the collagen anti-oxidation peptide with anti-oxidant function, prepared collagen anti-oxidation peptide is Powdered.
2. a kind of preparation method of collagen anti-oxidation peptide as claimed in claim 1, is characterized in that in step 1) in, described fish-skin or fish scale adopt a kind of fish-skin or the fish scale in fresh-water fishes, sea water fish; The concentration expressed in percentage by volume of described dehydrated alcohol can be 20%.
3. a kind of preparation method of collagen anti-oxidation peptide as claimed in claim 1, is characterized in that in step 1) in, the described add-on that contains the basic solution of dehydrated alcohol is 2～5 times of raw material; The condition that described basic solution soaks can be: basic solution is 0.01～0.05M NaOH solution, and the temperature of immersion is 4～20 ℃, and the time of immersion is 12～24h.
4. a kind of preparation method of collagen anti-oxidation peptide as claimed in claim 1, is characterized in that in step 1) in, the add-on of described acidic solution is 2～5 times of raw material; The condition that described acidic solution soaks can be: acidic solution is 0.05～0.20MHCl solution, and the temperature of immersion is 4～20 ℃, and the time of immersion is 1～3h.
5. a kind of preparation method of collagen anti-oxidation peptide as claimed in claim 1, it is characterized in that in step 2) in, described compound protease is selected from least two kinds in Collagenase, Sumizyme MP, trypsinase, papoid, bromeline, neutral protease etc.; The add-on of compound protease can be 0.1%～0.5% of raw materials quality by mass percentage; The condition of described enzymolysis can be in 40～60 ℃ of lower enzymolysis 2～6h.
6. a kind of preparation method of collagen anti-oxidation peptide as claimed in claim 1, is characterized in that in step 3) in, the temperature of described heating is 90～100 ℃, the time of heating is 5～15min.
7. a kind of preparation method of collagen anti-oxidation peptide as claimed in claim 1, is characterized in that in step 3) in, Plate Filtration or centrifuging are adopted in described filtration; The molecular weight cut-off of described nanofiltration membrane can be 200 dalton.
8. a kind of preparation method of collagen anti-oxidation peptide as claimed in claim 1, is characterized in that in step 4) in, described hydrophobic adsorbent is selected from least a in gac, ion exchange resin, macroporous adsorbent resin; The add-on of described hydrophobic adsorbent can be 1%～5% of collagen peptide solution by mass percentage.
9. a kind of preparation method of collagen anti-oxidation peptide as claimed in claim 1, is characterized in that in step 4) in, the time of described standing adsorption is 30～90min; The composition of described organic solvent can be: the volume ratio of dehydrated alcohol/acetic acid/water is 50/ (0.5～2.5)/(49.5～47.5); The add-on of described organic solvent can be 2～5 times of hydrophobic adsorbent in mass ratio.
10. a kind of preparation method of collagen anti-oxidation peptide as claimed in claim 1, is characterized in that in step 5) in, the temperature of described heating under vacuum evaporation is 50～80 ℃.
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