CN103540142A - Edible squid skin gelatin composite film and preparation method thereof - Google Patents
Edible squid skin gelatin composite film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an edible squid skin gelatin composite film and a preparation method of the edible squid skin gelatin composite film. The preparation method is characterized by comprising the steps of sequentially soaking the cleaned squid skin by alkali and acid, extracting the gelatin by hot water, and carrying out enzymolysis on part of the gelatin to obtain gelatin peptide with low molecular weight; adding gelatin, chitosan, glycerin and the gelatin peptide with low molecular weight into a 0.15-0.25wt% acetic acid solution, wherein the mass of the gelatin is 2-4% of that of the acetic acid solution, mass of the chitosan is 1.5-2.5% of that of the acetic acid solution, mass of the glycerin is 0.05-0.15% of that of the acetic acid solution, and the mass of the gelatin peptide with low molecular weight is 0.2-0.4% of that of the acetic acid solution; evenly mixing the mixed solution in the water bath with 40-60 DEG C, and carrying out heat preservation for 4-6h; carrying out vacuum degassing to form a uniform transparent film liquid; pouring the film liquid onto a perspex sheet, and evenly spreading the film liquid by a film coater; standing still for 2-4h at the temperature of 40-60 DEG C, and then standing still overnight under the conditions of room temperature and the relative humidity of 40-60%; stripping the film from the perspex sheet to obtain the product. The edible squid skin gelatin composite film and a preparation method of the edible squid skin gelatin composite film have the advantages that the composite film integrates the functions of nutrition, antioxidation, antibiosis and the like, and the preparation method is simple and easy to operate.
Description
Technical field
The present invention relates to food packaging film processing technique field, especially relate to a kind of squid skin gelatin edible composite film and preparation method thereof.
Background technology
Chemosynthesis plastic wrapping is difficult for decomposing rots, and causes serious " white pollution ", and this has become current global the difficult problem of environmental protection.Along with the raising of people to Food Quality and preservation term requirement, and the enhancing of environmental consciousness, exploitation edible packaging has become the study hotspot in food product pack field.Edible composite film refers to that take edible natural material (as polysaccharide, protein, lipid etc.) is raw material, add the materials such as softening agent, linking agent, the film with porous network structure forming by differing molecular interphase interaction, can be by preventing that the migration of gas, steam and solute etc. from keeping the quality of food, extends shelf time.Gelatin good film-forming property, biodegradable, containing multiple human body essential amino acid, be of high nutritive value, the consumption in food is unrestricted, thereby gelatin is made edible film and had superiority.
Gelatin (gelatin) be the side-chain radical on collagen molecules surface and water molecules with hydrogen bonded, expand, a kind of albumen superpolymer of formation, has been widely used in the industries such as food, medicine, chemical industry.The raw material of commodity gelatin is mainly from reticular tissue such as the bone of pig and ox and skins, and the reasons such as the pathophorous outburst of the animalities such as mad cow disease and foot and mouth disease and religious belief make people be devoted to find new safer raw material gelatin.Aquatic products gelatin perhaps can be used as a kind of new commodity replacing gelatin.Squid is the important processing variety of China, and squid skin is rich in gelatin, and work in-process accounts for fish-skin that squid weighs 5% left and right often directly as fish meal Raw material processing or go out of use, and economic benefit is not high.At present, any report of the correlative study about squid skin gelatin edible composite film and preparation method thereof is not also disclosed both at home and abroad.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of anti-oxidant, antibiotic and nutritious squid skin gelatin edible composite film and preparation method thereof that has.
The present invention solves the problems of the technologies described above adopted technical scheme:
1, a kind of squid skin gelatin edible composite film, the squid skin cleaning up is smashed to pieces, successively by alkali, acid soak, hot water extraction gelatin, and enzymolysis part of gelatin obtains low molecular weight gelatine peptide, in acetum, add gelatin, chitosan, glycerine and gelatin peptide and obtain film liquid, by film liquid heating, after vacuum outgas, film and obtain.
Described squid skin is smashed rear use 2～3%NaOH solution soaking to pieces, and distilled water is washed till neutrality, then soaks with 0.2% hydrochloric acid soln, and distilled water is washed till neutrality.
Described gelatin is joined in distilled water by the solid-liquid ratio of 1:10～15 by squid skin, in 40～60 ℃ of heating 22～26h, and cooled and filtered, glue is concentrated, dry to be obtained.
The gelatin solution that described gelatin peptide is 4～6% by mass concentration, adds proteolytic enzyme, in 50～60 ℃ of temperature, under the condition of pH 6～7, after enzymolysis 1.5～2h, after enzymolysis solution is concentrated, is dried, obtains; Wherein the addition of proteolytic enzyme is every gram of gelatin 6000～8000u.
Gelatin, 1.5～2.5% chitosan, 0.05～0.15% glycerine and 0.2～0.4% low molecular weight gelatine peptide that described film liquid adds acetum quality 2～4% in 0.15～0.25wt% acetum obtain.
Described painting membrane process is: film liquid is poured on poly (methyl methacrylate) plate, with coating device, evenly spread out, after 40～60 ℃ of placement 2～4h, under room temperature, relative humidity 40～60% conditions, place and spend the night, from sheet glass, stripping obtains squid skin gelatin edible composite film.
2, a preparation method for squid skin gelatin edible composite film, comprises the following steps:
(1) squid skin pre-treatment
Squid skin flowing water is thawed, and clear water is cleaned, and smashs rear use 2～3wt%NaOH solution soaking 4～8h to pieces, and distilled water is washed till neutrality; With 0.2wt% hydrochloric acid soln, soak after squid skin 4～8h, distilled water is washed till neutrality again;
(2) gelatin extraction
The squid skin that step (1) is obtained joins in distilled water by the solid-liquid ratio of 1:10～15, in 40～60 ℃ of heating 22～26h, and cooled and filtered, concentrated, the dry gelatin that obtains of glue;
(3) preparation of gelatin peptide
Gelatin that step (2) is obtained is water-soluble, and to be configured to mass concentration be 4～6% gelatin solution, adds proteolytic enzyme, in 50～60 ℃ of temperature, under the condition of pH 6～7, after enzymolysis 1.5～2h, enzymolysis solution is concentrated, dry after, obtain low molecular weight gelatine peptide;
(4) preparation of film liquid
In the acetum that is 0.15～0.25% by massfraction, add gelatin, 1.5～2.5% chitosan, 0.05～0.15% glycerine and 0.2～0.4% the low molecular weight gelatine peptide of acetum quality 2～4%, even in 40～60 ℃ of stirred in water bath, insulation 4～6h, vacuum outgas, the film liquid of formation transparent and homogeneous;
(5) preparation of gelatin edible composite film
Film liquid is poured on poly (methyl methacrylate) plate, with coating device, evenly spreads out, after 40～60 ℃ of placement 2～4h, under room temperature, relative humidity 40～60% conditions, place and spend the night, stripping from sheet glass, obtains squid skin gelatin edible composite film.
The mass volume ratio of the squid skin described in step (1) and described NaOH solution is 1:8～12, and the mass volume ratio of described squid skin and described hydrochloric acid soln is 1:8～12.
The addition of the proteolytic enzyme described in step (3) is every gram of gelatin 6000～8000u.
Compared with prior art, the invention has the advantages that:
(1) gelatin extracting is carried out under the enzymatic hydrolysis condition of optimization of the present invention to enzymolysis, obtain molecular size range suitable, the low molecular weight gelatine peptide with high-efficiency antioxidant effect, wherein the molecular weight of 90% above gelatin peptide is between 1400-10000, this gelatin peptide is to DPPH(1, 1-phenylbenzene-2-trinitrophenyl-hydrazine) clearance rate of free radical can reach more than 90%, in film liquid, add this gelatin peptide with antioxygenation, the gelatin film tool resistance of oxidation making, to the clearance rate of DPPH free radical, can reach more than 78%, can suppress the especially lipid oxidation of fat-containing food of food, when the higher flesh of fish of lipid content is filmed or is packed, edible composite film has delayed the lipid oxidation of the flesh of fish, extended effective period of food quality,
(2) film fluid component chitosan has obvious anti-microbial effect, and the gelatin-compounded film making has antibacterial;
(3) because the gelatin in film fluid component, gelatin peptide are all by the protein of Amino acid profile or peptide, after being eaten, the film of making can provide each seed amino acid for human body, gelatin peptide molecular weight is low simultaneously, more hold easily absorbed by the body, therefore, the gelatin-compounded film making is as packaging material for food time, has nutrition, the function such as antibiotic, anti-oxidant, becomes a kind of multifunctional composite film;
(4) in the present invention, gelatin plays the effect of film forming, and glycerine provides booster action as edible softening agent for gelatin film forming.Gelatin mainly relies on the effect such as hydrogen bond to form three-dimensional net structure, and system is through dehydration and film forming, but the film that only relies on gelatin molecule to be cross-linked with each other to form is more crisp, snappiness is not enough.For reducing the fragility of gelatin film, improve its snappiness, can in gelatin film forming liquid, add softening agent, plasticizer molecule is by affecting the formation of gelatin molecule interchain hydrogen bond, and by moisture absorption in gelatin network, improve the mobility of gelatin film network structure, increase the snappiness of film.Both mix in ratio of the present invention, make the plasticity-of film and snappiness reach best;
(5) squid skin is rich in gelatin, take squid skin gelatin as matrix development packing film, exploitation integrate the edible composite membrane of nutrition, the function such as anti-oxidant, antibiotic, can reduce the discharge of aquatic products processing waste, environmental pollution and food-safety problem that reduction plastic packaging film brings.
In sum, a kind of squid skin gelatin of the present invention edible composite film, the edible packing film that the squid skin gelatin of take is developed as matrix, collection nutrition, anti-oxidant, antibiotic etc. act as one, its preparation method is simple, easy to operate, for the higher value application of squid skin provides a new way, provides theoretical foundation for the development and application of novel package material.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
A kind of squid skin gelatin of the present invention edible composite film, comprise the squid skin cleaning up, squid skin is soaked respectively by alkali lye and acid solution successively, distilled water is washed till the distilled water that adds 12 times of volumes after neutrality, after heating certain hour, concentrated, the dry gelatin that obtains of glue; Above-mentioned gelatin is configured to 5% concentration with distilled water, and enzymolysis obtains gelatin peptide; In acetum, add respectively gelatin, chitosan, glycerine and gelatin peptide and obtain film liquid, by the heating of film liquid, after vacuum outgas, film and obtain gelatin-compounded film, its concrete preparation method is as follows:
(1) squid skin flowing water thaws, clear water is cleaned, smash the rear 2.5wt%NaOH solution (the mass volume ratio 1:10 w/v of squid skin and NaOH solution) of first using to pieces and soak 6h, with distilled water, be washed till neutrality, use 0.2wt% hydrochloric acid soln (the mass volume ratio 1:10 w/v of squid skin and hydrochloric acid soln) to soak 6h, distilled water is washed till neutrality again;
(2) squid skin of above-mentioned pre-treatment is joined in distilled water to 50 ℃ of heating 24h, cooled and filtered, concentrated, the dry gelatin that obtains of glue by the solid-liquid ratio of 1:12;
(3) above-mentioned gelatin is dissolved in to distilled water and is configured to 5% concentration, add proteolytic enzyme (addition 7000u/g), in 55 ℃, under the condition of pH 6.5, after enzymolysis 1.8h, after enzymolysis solution is concentrated, is dried, obtain low molecular weight gelatine peptide;
(4) in the acetum that is 0.20% by massfraction, add gelatin, 2% chitosan, 0.1% glycerine and 0.3% the low molecular weight gelatine peptide of acetum quality 3%, even in 50 ℃ of stirred in water bath, insulation 5h, vacuum outgas, the film liquid of formation transparent and homogeneous; Get film liquid imitation crab meat rod is filmed, under 4 ℃ of conditions, preserve, its total number of bacterial colony rate of growth is starkly lower than the control group of not filming, and the quality guaranteed period extends about 4d;
(5) film liquid is poured on poly (methyl methacrylate) plate, with coating device, evenly spreads out, after 50 ℃ of placement 3h, under room temperature, relative humidity 50% condition, place and spend the night, from sheet glass, peel, obtain gelatin-compounded film, can be used for food fresh keeping packing.Utilize this film packing mackerel meat, under 4 ℃ of conditions, preserve, the peroxide value of control group mackerel meat reaches peak value 1.98mg/100g at 6d, and the peroxide value of edible film packing mackerel meat reaches peak value 1.42mg/100g at 9d, and edible composite film has delayed the lipid oxidation of the flesh of fish.
Embodiment 2
With embodiment 1, its difference is:
(1) squid skin cleans up and smashs rear 2.0wt%NaOH solution (1:8 w/v) the immersion 8h that first uses to pieces, and distilled water is washed till neutrality, then uses 0.2wt% hydrochloric acid soln (1:8w/v) to soak 8h, and distilled water is washed till neutrality;
(2) squid skin is joined in distilled water to 40 ℃ of heating 26h by the solid-liquid ratio of 1:10;
(3) above-mentioned gelatin is dissolved in to distilled water and is configured to 4% concentration, add proteolytic enzyme (addition 6000u/g), in 50 ℃, under the condition of pH 6.0, enzymolysis 2h;
(4) in the acetum that is 0.15% by massfraction, add gelatin, 1.5% chitosan, 0.05% glycerine and 0.2% the low molecular weight gelatine peptide of acetum quality 2%, even in 40 ℃ of stirred in water bath, insulation 6h; Get film liquid imitation crab meat rod is filmed, under 4 ℃ of conditions, preserve, its total number of bacterial colony rate of growth is lower than the control group of not filming, and the quality guaranteed period extends about 3d;
(5) film liquid is placed after 4h in 40 ℃, under relative humidity 40% condition, placed and spend the night.Utilize institute's masking packing mackerel meat, under 4 ℃ of conditions, preserve, the peroxide value of control group mackerel meat reaches peak value 1.98mg/100g at 6d, and the peroxide value of edible film packing mackerel meat reaches peak value 1.46mg/100g at 8d, and edible composite film has delayed the lipid oxidation of the flesh of fish.
Embodiment 3
With embodiment 1, its difference is:
(1) squid skin cleans up and smashs 3wt%NaOH solution (1:12 w/v) immersion 4h for rear priority to pieces, and distilled water is washed till neutrality, then uses 0.2wt% hydrochloric acid soln (1:12w/v) to soak 4h, and distilled water is washed till neutrality;
(2) squid skin is joined in distilled water to 60 ℃ of heating 22h by the solid-liquid ratio of 1:15;
(3) above-mentioned gelatin is dissolved in to distilled water and is configured to 6% concentration, add proteolytic enzyme (addition 8000u/g), in 60 ℃, under the condition of pH 8.0, enzymolysis 1.5h;
(4) in the acetum that is 0.25% by massfraction, add gelatin, 2.5% chitosan, 0.15% glycerine and 0.4% the low molecular weight gelatine peptide of acetum quality 4%, even in 60 ℃ of stirred in water bath, insulation 4h; Get film liquid imitation crab meat rod is filmed, under 4 ℃ of conditions, preserve, its total number of bacterial colony rate of growth is lower than the control group of not filming, and the quality guaranteed period extends about 4d;
(5) film liquid is placed after 2h in 60 ℃, under relative humidity 60% condition, placed and spend the night.Utilize institute's masking packing mackerel meat, under 4 ℃ of conditions, preserve, the peroxide value of control group mackerel meat reaches peak value 1.98mg/100g at 6d, and the peroxide value of edible film packing mackerel meat reaches peak value 1.31mg/100g at 9d, and edible composite film has delayed the lipid oxidation of the flesh of fish.
Certainly, above-mentioned explanation is not limitation of the present invention, and the present invention is also not limited to above-mentioned giving an example.Those skilled in the art are in essential scope of the present invention, and the variation of making, remodeling, interpolation or replacement, also should belong to protection scope of the present invention.
Claims (9)
1. a squid skin gelatin edible composite film, it is characterized in that: the squid skin cleaning up is smashed to pieces successively by alkali, acid soak, hot water extraction gelatin, and enzymolysis part of gelatin obtains low molecular weight gelatine peptide, in acetum, add gelatin, chitosan, glycerine and gelatin peptide and obtain film liquid, by film liquid heating, after vacuum outgas, film and obtain.
2. a kind of squid skin gelatin multifunctional composite film according to claim 1, is characterized in that: described squid skin is smashed rear 2～3%NaOH solution soaking of first using to pieces, with distilled water, is washed till neutrality, then soaks with 0.2% hydrochloric acid soln, and distilled water is washed till neutrality.
3. a kind of squid skin gelatin multifunctional composite film according to claim 1, it is characterized in that: described gelatin is joined in distilled water by the solid-liquid ratio of 1:10～15 by squid skin, in 40～60 ℃ of heating 22～26h, cooled and filtered, glue is concentrated, dry to be obtained.
4. a kind of squid skin gelatin multifunctional composite film according to claim 3, it is characterized in that: the gelatin solution that described gelatin peptide is 4～6% by mass concentration, add proteolytic enzyme, in 50～60 ℃ of temperature, under the condition of pH 6～7, after enzymolysis 1.5～2h, after being concentrated, be dried, enzymolysis solution obtains; Wherein the addition of proteolytic enzyme is every gram of gelatin 6000～8000u.
5. a kind of squid skin gelatin multifunctional composite film according to claim 1, is characterized in that: gelatin, 1.5～2.5% chitosan, 0.05～0.15% glycerine and 0.2～0.4% low molecular weight gelatine peptide that described film liquid adds acetum quality 2～4% in 0.15～0.25wt% acetum obtain.
6. a kind of squid skin gelatin multifunctional composite film according to claim 5, it is characterized in that described painting membrane process is: film liquid is poured on poly (methyl methacrylate) plate, with coating device, evenly spread out, in 40～60 ℃, place after 2～4h, under room temperature, relative humidity 40～60% conditions, place and spend the night, from sheet glass, stripping obtains squid skin gelatin multifunctional composite film.
7. according to a preparation method for the squid skin gelatin edible composite film described in any one in claim 1-6, it is characterized in that comprising the following steps:
(1) squid skin pre-treatment
Squid skin flowing water is thawed, and clear water is cleaned, and smashs rear use 2～3wt%NaOH solution soaking 4～8h to pieces, and distilled water is washed till neutrality; With 0.2wt% hydrochloric acid soln, soak after squid skin 4～8h, distilled water is washed till neutrality again;
(2) gelatin extraction
The squid skin that step (1) is obtained joins in distilled water by the solid-liquid ratio of 1:10～15, in 40～60 ℃ of heating 22～26h, and cooled and filtered, concentrated, the dry gelatin that obtains of glue;
(3) preparation of gelatin peptide
Gelatin that step (2) is obtained is water-soluble, and to be configured to mass concentration be 4～6% gelatin solution, adds proteolytic enzyme, in 50～60 ℃ of temperature, under the condition of pH 6～7, after enzymolysis 1.5～2h, enzymolysis solution is concentrated, dry after, obtain low molecular weight gelatine peptide;
(4) preparation of film liquid
In the acetum that is 0.15～0.25% by massfraction, add gelatin, 1.5～2.5% chitosan, 0.05～0.15% glycerine and 0.2～0.4% the low molecular weight gelatine peptide of acetum quality 2～4%, even in 40～60 ℃ of stirred in water bath, insulation 4～6h, vacuum outgas, the film liquid of formation transparent and homogeneous;
(5) preparation of gelatin edible composite film
Film liquid is poured on poly (methyl methacrylate) plate, with coating device, evenly spreads out, after 40～60 ℃ of placement 2～4h, under room temperature, relative humidity 40～60% conditions, place and spend the night, stripping from sheet glass, obtains squid skin gelatin edible composite film.
8. the preparation method of a kind of squid skin gelatin edible composite film according to claim 7, it is characterized in that: the mass volume ratio of the squid skin described in step (1) and described NaOH solution is 1:8～12, and the mass volume ratio of described squid skin and described hydrochloric acid soln is 1:8～12.
9. the preparation method of a kind of squid skin gelatin edible composite film according to claim 7, is characterized in that: the addition of the proteolytic enzyme described in step (3) is every gram of gelatin 6000～8000u.
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