CN102276858A - Preparation method of edible collagen composite membrane - Google Patents
Preparation method of edible collagen composite membrane Download PDFInfo
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- CN102276858A CN102276858A CN 201110222564 CN201110222564A CN102276858A CN 102276858 A CN102276858 A CN 102276858A CN 201110222564 CN201110222564 CN 201110222564 CN 201110222564 A CN201110222564 A CN 201110222564A CN 102276858 A CN102276858 A CN 102276858A
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Abstract
The invention discloses a preparation method of an edible collagen composite membrane. The preparation method comprises the following steps of: dissolving collagen into distilled water to prepare collagen aqueous solution and dissolving chitosan and derivatives thereof into dilute acetic acid solution to prepare dilute solution, wherein the fish skin collagen, the chitosan and the derivatives thereof serve as main raw materials; compounding the two kinds of solution; adding a plasticizer; and performing membrane forming to prepare the edible collagen composite membrane. The edible collagen composite membrane has excellent biocompatibility, degradability and a good freshness-retaining function; and the main raw materials and auxiliary materials are edible substances and the sources of the materials are sufficient.
Description
Technical field
The present invention relates to a kind of method for preparing the collagen protein composite membrane, more specifically relate to a kind of preparation method of edibility collagen protein composite membrane.
Background technology
China is aquatic products big country, and aquatic resources are abundant.2009, China's fishery products total amount just reached 5,120 ten thousand tons, and the fishery products ultimate production will reach 5,350 ten thousand tons in 2010, increase by 4.6% on a year-on-year basis.But China's processing of aquatic products is still based on roughing at present, and the ratio of intensive processing product is not high.Fish produce tankage such as a large amount of fish-skins, fish-bone, fish scale in the course of processing, account for 40% ~ 55% of raw material fish.Contain rich in protein and various trace elements in the fish-skin, its protein mainly is macromolecular collagen protein and mucopolysaccharide composition, and collagen protein accounts for about 80% of crude protein.As seen, fish-skin is the good source of collagen protein.Yet these fish-skin wastes are used for producing cheap feed substantially aborning, or directly as refuse treatment, cause the wasting of resources and environmental pollution.Therefore, making full use of the aquatic products processing tankage, is the task of top priority and the development trend of fishery products tankage research.In addition, the employed material major part of food product pack all is plastics, but its serious consequence is to use the back to abandon degraded difficulty in environment, has caused " white pollution ", has brought serious harm to ecotope.Therefore, utilize the fish disposal from fishery product processing to produce the collagen protein composite membrane, to reducing aquatic products processing enterprise discharging wastes, reduce the use of plastic wrapping in food, the protection environment all has good effect.
Edible packing membrane (Edible Packaging Films, be called for short PEF) be (as protein with the edible natural material, polysaccharide etc.) be raw material, add glycerine, edibility softening agent such as sorbyl alcohol, make it after drying, to form a kind of have certain physical strength, the film of compact structure by certain treatment process.Can divide by its raw material sources protein-based, polyose, polyester and composite edible packing film, wherein the research of compound PEF and application are current development trends.Protein self has good film forming ability and nutritive value, and wherein collagen protein is an animal protein most widely used in the edible packing membrane, but the raw materials for production of collagen protein are skin and the bone of pig, ox basically.Owing to the fear of mad cow disease, Schweineseuche and religion reason etc., extracting collagen protein from hydrocoles becomes necessary in recent years.The collagen protein that people such as Limpisophon K. extract by the hot-water process from the shark skin waste adds glycerine and has prepared collagen film as softening agent, has good photoresistance, peroxidation has good provide protection to food.Jongjareonrak A. etc. have obtained collagen protein by hot-water process's extraction from big red silk fish fish-skin, add glycerine as softening agent, have prepared the edible packaging mould material of collagen protein.But itself there is the deficiency of gas barrier property, mechanical property and water resistance in single collagen film, and their application is restricted.Chitin is that the nature store content is only second to cellulosic natural polymeric material, chitosan be chitin take off the acetyl product, it has good film-forming properties, adds antibiotic, the fresh-keeping function of chitosan uniqueness, thereby is a kind of good material as edible packing membrane.So the collagen protein chitosan complex film of the compound preparation of collagen protein and chitosan can be good at improving the deficiency that single collagen film itself exists, and can increase the fresh-keeping function of film again.But it is less relatively about compound collagen protein chitosan film report at home and abroad.
Summary of the invention
The invention provides a kind of preparation method of edibility collagen protein composite membrane, these method raw material sources are extensive, and technology is simple, and cost is low, and the composite membrane of preparation is functional and have fresh-keeping function preferably, but widespread use.
The preparation method of a kind of edibility collagen protein composite membrane provided by the invention, it is a main raw material with collagen of fish skin and chitosan and derivative thereof, collagen of fish skin is dissolved in distilled water makes collagen solution, chitosan and derivative thereof are dissolved in dilute acetic acid make dilute solution, compound with collagen solution then, and the adding softening agent, make the composite edible collagen film at last.Described collagen of fish skin is to extract to obtain from fish processing fent fish-skin, its technical matters comprises removes fish processing fent fish-skin noncollagen protein, degreasing, takes off step such as raw meat, obtains collagen of fish skin through superheated water lixiviate, centrifugation, freeze-drying again.
Technical scheme of the present invention is as follows:
A kind of preparation method of edibility collagen protein composite membrane, this film is a main raw material with collagen of fish skin and chitosan and derivative thereof, with the softening agent is ancillary component, collagen of fish skin is dissolved in distilled water makes the collagen protein aqueous solution, chitosan and derivative thereof are dissolved in dilute acetic acid make the chitosan dilute solution, solution combined with two kinds then, and add softening agent, last film forming is made edibility collagen protein composite membrane.
The extraction of described collagen of fish skin is as follows: the waste fish-skin is scaled, and shreds cleanly, stir to soak 12～24h in basic solution, then, is washed till neutrality with clear water; In acidic solution, stir again and soak 2～8h, be washed till neutrality with clear water; After the hot water lixiviate, adopt centrifugation to remove insoluble substance, freeze-drying obtains the collagen of fish skin powder.Described basic solution is for containing H
2O
2The Na0H aqueous solution, NaOH concentration is 0.01M～0.2M, H
2O
2Mass concentration is 1%～5%.Described acidic solution is acetic acid or the aqueous citric acid solution of 0.05M～O.5M.Described waste fish-skin soaking temperature in basic solution is 4～20 ℃.Described hot water extraction temperature is 30～60 ℃, and extraction time is 6～12h.
Described chitosan and derivative thereof are selected from chitosan, O-cm-chitosan, N-cm-chitosan and N, O-cm-chitosan.
Described softening agent is a glycerine.Described plasticizer dosage accounts for 25%～50% of collagen of fish skin and chitosan and derivative gross weight thereof.
The collagen protein aqueous solution that the described collagen protein aqueous solution is weight ratio 2%～6%.
The preparation of described chitosan dilute solution is that to add volume ratio in chitosan and derivative thereof be in 1%～5% the dilute acetic acid, is 0.5%～5% chitosan and derivative dilute solution thereof through fully stirring, making weight ratio.
The present invention prepares the collagen protein composite membrane and has following advantage:
1. the main raw material and the auxiliary material of preparation edibility collagen protein composite membrane are the edibility material, nutritious as collagen of fish skin, contain multiple essential amino acid, chitosan and derivative source abundance thereof are extensively inexpensive, all nontoxic to human body, also can be human body nutritive ingredient and certain physiological hygiene function are provided.
2. this film has excellent biological compatibility.
3. this film is biodegradable, so waste does not cause environmental pollution.
4. no fierce chemical reacting condition in the membrane prepare process, no obnoxious flavour and liquid produce, and is safe.
5. the membrane prepare technical process is simple, and facility investment is few, and cost is low, so good market prospects.
Embodiment
Method of the present invention comprises following processing step:
(1) extraction of collagen of fish skin: the waste fish-skin is scaled, shred clean, with 10～20 times of raw materials heavy contain 1%～5% H
2O
20.01M～0.2M NaOH aqueous solution stir to soak 12～24h at 4～20 ℃, then, be washed till neutrality with clear water; At room temperature stir with acetic acid of the heavy 0.05M of 10～20 times of raw materials～O.5M or aqueous citric acid solution and to soak 2～8h, then, be washed till neutrality with clear water; Then, lixiviate 6～12h in 30～60 ℃ of heavy hot water of 5～10 times of raw materials.Then, adopt centrifugation to remove insoluble substance, freeze-drying obtains the collagen of fish skin powder.
(2) preparation of film-casting liquid: collagen protein is dissolved in the distilled water, under 30 ℃～60 ℃, stirs, make weight ratio and be 2%～6% the collagen protein aqueous solution; Chitosan and derivative thereof be dissolved in 1%～5% the dilute acetic acid, under 30 ℃～60 ℃, stir, make weight ratio and be 0.5%～5% chitosan dilute solution.The collagen protein aqueous solution and chitosan dilute solution is compound, add and account for the glycerine of collagen protein and chitosan and derivative weight 25%～50% thereof as softening agent, continue to stir 30min～60min, then, utilize the deaeration machine to carry out being prepared into the edible film film-casting liquid after the deaeration.Wherein 3:1～1:3 is compound by volume for the collagen of fish skin aqueous solution and chitosan dilute solution.
(3) preparation of collagen protein composite membrane: the 6ml film-casting liquid that modulates evenly is poured in the silicone resin frame of 12cm * 8cm * 1cm, in 22 ℃ of baking ovens, dry 24h, then, can obtain edibility collagen protein composite membrane after peeling off from silicone resin.
Below being several specific examples of the present invention, be to further describe of the present invention, but the present invention is not limited only to this.
Embodiment 1
1, the extraction of collagen protein: get 250g silver carp waste fish-skin and shred, clean, at 20 ℃ of 0.01M NaOH-1%H with 2.5L
2O
2Solution stirring is soaked 12h, is washed till neutrality with clear water; Then, at room temperature the 0.05M aqueous acetic acid with 2.5L stirs immersion 2h, then, is washed till neutrality with clear water; Use the hot water lixiviate 12h of 30 ℃ of 2.5L again, then, insoluble substance is removed in 18 000 * g centrifugation, and freeze-drying obtains collagen of fish skin.
2, the preparation of film-casting liquid: the 2.0g collagen of fish skin is dissolved in the 100ml distilled water, under 30 ℃, stirs, make weight ratio and be 2% the collagen protein aqueous solution; The 0.5g chitosan is dissolved in the dilute acetic acid of 100ml 1%, under 30 ℃, stirs, make weight ratio and be 0.5% chitosan dilute solution.3:1 is compound by volume with the collagen of fish skin aqueous solution and chitosan dilute solution, and add account for collagen of fish skin and chitosan gross weight 25% glycerine as softening agent, continue to stir 30min; Then, utilize the deaeration machine to carry out being prepared into the edible film film-casting liquid after the deaeration.
3, the preparation of collagen protein composite membrane: the 6ml film-casting liquid that modulates evenly is poured in the silicone resin frame of 12cm * 8cm * 1cm, in 22 ℃ of baking ovens, dry 24h, then, can obtain edibility collagen protein chitosan complex film after peeling off from silicone resin.
Embodiment 2
1, the extraction of collagen protein: get 500g grass carp waste fish-skin and shred, clean, use 7.5L 0.05M NaOH-1%H down at 10 ℃
2O
2Solution stirring is soaked 18h, is washed till neutrality with clear water; Then, at room temperature be washed till neutrality with clear water behind the 0.2M aqueous citric acid solution immersion 4h with 7.5L; Use the hot water lixiviate 10h of 45 ℃ of 5L again, then, insoluble substance is removed in 18 000 * g centrifugation, and freeze-drying obtains collagen of fish skin.
2, the preparation of film-casting liquid: the 3.0g collagen of fish skin is dissolved in the 100ml distilled water, under 45 ℃, stirs, make weight ratio and be 4% the collagen protein aqueous solution; The 2.0g chitosan is dissolved in the dilute acetic acid of 100ml 3%, under 45 ℃, stirs, make weight ratio and be 2% chitosan dilute solution.1:1 is compound by volume with the collagen of fish skin aqueous solution and chitosan solution, and add account for collagen of fish skin and chitosan gross weight 30% glycerine as softening agent, continue to stir 30min; Then, utilize the deaeration machine to carry out being prepared into the edible film film-casting liquid after the deaeration.
3, the preparation of collagen protein composite membrane: the preparation method is identical with example 1.
Embodiment 3
1, the extraction of collagen protein: get 1kg grass carp waste fish-skin and shred, clean, under 15 ℃, be used in the 0.1M NaOH-3%H of 10L
2O
2Solution stirring is soaked 24h, is washed till neutrality with clear water; Then, at room temperature be washed till neutrality with clear water behind the 0.5M aqueous acetic acid immersion 4h with 5L; Use the hot water lixiviate 8h of 50 ℃ of 5L again, then, insoluble substance is removed in 18 000 * g centrifugation, and freeze-drying obtains collagen of fish skin.
2, the preparation of film-casting liquid: the 3.0g collagen of fish skin is dissolved in the 100ml distilled water, under 50 ℃, stirs, make weight ratio and be 3% the collagen protein aqueous solution; (substitution value=0.25-0.9) is dissolved in 3% the dilute acetic acid, stirs under 50 ℃, makes weight ratio and be 4% O-cm-chitosan dilute solution with 4.0g O-cm-chitosan.1:3 is compound by volume with collagen of fish skin solution and O-cm-chitosan dilute solution, and add account for collagen of fish skin and O-cm-chitosan gross weight 40% glycerine as softening agent, continue to stir 45min; Then, utilize the deaeration machine to carry out being prepared into the edible film film-casting liquid after the deaeration.
3, the preparation of collagen protein composite membrane: the preparation method is identical with example 1.
Embodiment 4
1, the extraction of collagen protein: get 2kg silver carp waste fish-skin and shred, clean, at 4 ℃ of 0.2M NaOH-5%H that use 15L down
2O
2Solution stirring is soaked 24h, is washed till neutrality with clear water; Then, at room temperature be washed till neutrality with clear water behind the 0.1M aqueous acetic acid immersion 6h with 10L; Use the hot water lixiviate 12h of 60 ℃ of 10L again, then, insoluble substance is removed in 18 000 * g centrifugation, and freeze-drying obtains collagen of fish skin.
2, the preparation of film-casting liquid: the 6.0g collagen of fish skin is dissolved in the 100ml distilled water, under 60 ℃, stirs, make weight ratio and be 6% the collagen protein aqueous solution; With 5.0g N, the O-cm-chitosan is dissolved in the dilute acetic acid of 100ml 5%, stirs under 60 ℃, makes weight ratio and be 5% N, O-cm-chitosan dilute solution.With collagen solution and N, 1:1 is compound by volume for O-cm-chitosan dilute solution, and adding accounts for collagen of fish skin and N, the glycerine of O-cm-chitosan gross weight 50% is as softening agent, continue to stir 60min, then, utilize the deaeration machine to carry out being prepared into the edible film film-casting liquid after the deaeration.
3, the preparation of collagen protein composite membrane: the preparation method is identical with example 1.
Claims (10)
1. the preparation method of an edibility collagen protein composite membrane, this film is a main raw material with collagen of fish skin and chitosan and derivative thereof, with the softening agent is ancillary component, it is characterized in that: collagen of fish skin is dissolved in distilled water makes the collagen protein aqueous solution, chitosan and derivative thereof are dissolved in dilute acetic acid make the chitosan dilute solution, solution combined with two kinds then, and add softening agent, last film forming is made edibility collagen protein composite membrane.
2. method according to claim 1 is characterized in that: the extraction of described collagen of fish skin is as follows: the waste fish-skin is scaled, and shreds cleanly, stir to soak 12～24h in basic solution, then, is washed till neutrality with clear water; In acidic solution, stir again and soak 2～8h, be washed till neutrality with clear water; After the hot water lixiviate, adopt centrifugation to remove insoluble substance, freeze-drying obtains the collagen of fish skin powder.
3. method according to claim 2 is characterized in that: described basic solution is for containing H
2O
2The Na0H aqueous solution, NaOH concentration is 0.01M～0.2M, H
2O
2Mass concentration is 1%～5%.
4. method according to claim 2 is characterized in that: described acidic solution is acetic acid or the aqueous citric acid solution of 0.05M～O.5M.
5. method according to claim 2 is characterized in that: described waste fish-skin soaking temperature in basic solution is 4～20 ℃.
6. method according to claim 2 is characterized in that: described hot water extraction temperature is 30～60 ℃, and extraction time is 6～12h.
7. method according to claim 1 is characterized in that: described chitosan and derivative thereof are selected from chitosan, O-cm-chitosan, N-cm-chitosan and N, O-cm-chitosan.
8. method according to claim 1 is characterized in that: described softening agent is a glycerine.
9. method according to claim 1 is characterized in that: the collagen protein aqueous solution that the described collagen protein aqueous solution is weight ratio 2%～6%.
10. method according to claim 1, it is characterized in that: the preparation of described chitosan dilute solution is that to add volume ratio in chitosan and derivative thereof be in 1%～5% the dilute acetic acid, through fully stirring, making weight ratio is 0.5%～5% chitosan and derivative dilute solution thereof.
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Cited By (14)
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| CN102643554A (en) * | 2012-05-08 | 2012-08-22 | 福州大学 | Edible fishskin collagen antibiosis membrane and preparing method thereof |
| CN102763843A (en) * | 2012-07-05 | 2012-11-07 | 昆明豪原特自控有限公司 | Biological nutrient |
| CN103030979A (en) * | 2012-12-27 | 2013-04-10 | 福建省博特生物科技有限公司 | Collagen antibacterial membrane containing cinnamon essential oil and preparation method of collagen antibacterial membrane |
| CN104387779A (en) * | 2014-11-05 | 2015-03-04 | 福州大学 | Antioxidative collagen film containing active plant extract nanoliposome |
| CN104877155A (en) * | 2015-05-21 | 2015-09-02 | 浙江海洋学院 | Method for preparing gelatin-ZnO nano composite film from tuna heads |
| CN105029512A (en) * | 2015-07-24 | 2015-11-11 | 四川大学 | Preparation method of fish skin collagen jelly |
| CN105541998A (en) * | 2015-12-10 | 2016-05-04 | 中国海洋大学 | Glycosylation method for improving emulsification stability of collagen |
| CN105961608A (en) * | 2016-03-23 | 2016-09-28 | 马鞍山市黄池食品（集团）有限公司 | Fresh dried bean curd for calming nerves and harmonizing stomach and preparation method thereof |
| CN106632665A (en) * | 2016-11-03 | 2017-05-10 | 合肥工业大学 | Method for extracting collagen from freshwater fish skin by lactic acid |
| CN106973988A (en) * | 2017-05-14 | 2017-07-25 | 郭迎庆 | A kind of preparation method for applying membranous type edible fruit antistaling agent |
| CN107141518A (en) * | 2017-06-07 | 2017-09-08 | 安徽中盛食用油科技有限公司 | A kind of edibility antibacterial film for wrapping up tea-seed oil and preparation method thereof |
| CN107254182A (en) * | 2017-06-15 | 2017-10-17 | 深圳先进技术研究院 | Edible film is into film liquid and preparation method thereof and edible film and preparation method thereof |
| CN110511437A (en) * | 2019-07-25 | 2019-11-29 | 安徽新翔包装材料有限公司 | A kind of Biodegradable environment protection type packaging material for food |
| CN115260605A (en) * | 2021-04-30 | 2022-11-01 | 北京服装学院 | Process for manufacturing textile by using fish skin |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643554A (en) * | 2012-05-08 | 2012-08-22 | 福州大学 | Edible fishskin collagen antibiosis membrane and preparing method thereof |
| CN102643554B (en) * | 2012-05-08 | 2013-12-04 | 福州大学 | Edible fishskin collagen antibiosis membrane and preparing method thereof |
| CN102763843A (en) * | 2012-07-05 | 2012-11-07 | 昆明豪原特自控有限公司 | Biological nutrient |
| CN103030979A (en) * | 2012-12-27 | 2013-04-10 | 福建省博特生物科技有限公司 | Collagen antibacterial membrane containing cinnamon essential oil and preparation method of collagen antibacterial membrane |
| CN104387779A (en) * | 2014-11-05 | 2015-03-04 | 福州大学 | Antioxidative collagen film containing active plant extract nanoliposome |
| CN104877155A (en) * | 2015-05-21 | 2015-09-02 | 浙江海洋学院 | Method for preparing gelatin-ZnO nano composite film from tuna heads |
| CN105029512A (en) * | 2015-07-24 | 2015-11-11 | 四川大学 | Preparation method of fish skin collagen jelly |
| CN105541998A (en) * | 2015-12-10 | 2016-05-04 | 中国海洋大学 | Glycosylation method for improving emulsification stability of collagen |
| CN105961608A (en) * | 2016-03-23 | 2016-09-28 | 马鞍山市黄池食品（集团）有限公司 | Fresh dried bean curd for calming nerves and harmonizing stomach and preparation method thereof |
| CN106632665A (en) * | 2016-11-03 | 2017-05-10 | 合肥工业大学 | Method for extracting collagen from freshwater fish skin by lactic acid |
| CN106973988A (en) * | 2017-05-14 | 2017-07-25 | 郭迎庆 | A kind of preparation method for applying membranous type edible fruit antistaling agent |
| CN107141518A (en) * | 2017-06-07 | 2017-09-08 | 安徽中盛食用油科技有限公司 | A kind of edibility antibacterial film for wrapping up tea-seed oil and preparation method thereof |
| CN107254182A (en) * | 2017-06-15 | 2017-10-17 | 深圳先进技术研究院 | Edible film is into film liquid and preparation method thereof and edible film and preparation method thereof |
| CN110511437A (en) * | 2019-07-25 | 2019-11-29 | 安徽新翔包装材料有限公司 | A kind of Biodegradable environment protection type packaging material for food |
| CN115260605A (en) * | 2021-04-30 | 2022-11-01 | 北京服装学院 | Process for manufacturing textile by using fish skin |
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Application publication date: 20111214 |