CN109135302A - Isinglass/compound the edible film of oxidized starch dual network, preparation method and its application - Google Patents
Isinglass/compound the edible film of oxidized starch dual network, preparation method and its application Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/38—Packaging materials of special type or form
- B65D65/46—Applications of disintegrable, dissolvable or edible materials
- B65D65/463—Edible packaging materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2389/00—Characterised by the use of proteins; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2403/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2403/04—Starch derivatives
- C08J2403/10—Oxidised starch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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Abstract
The present invention proposes a kind of isinglass/compound edible film of oxidized starch dual network, preparation method and its application, belongs to edible packaging technical field.The compound edible film using isinglass as matrix, using oxidized starch as crosslinking agent, using schiff base reaction and heat treatment induction isinglass and oxidized starch between crosslinking interpenetrating be prepared.In terms of compound edible film provided by the present invention can be applied to packaging material for food, with good barrier property, quality deterioration caused by food is waited because of oxidation/moisture evaporation/enzymatic reaction can be effectively relieved, provide a kind of environmentally protective edible packaging material for food service industry.
Description
Technical field
It can the invention belongs to edible packaging technical field more particularly to a kind of isinglass/oxidized starch dual network is compound
Eat film, preparation method and its application.
Background technique
In recent years, it is widely used by the packaging material of raw material of petroleum alkene polymer, non-biodegradable results in sternly
The environmental pollution of weight.With the improvement of people's environmental awareness, especially being proposed to food, pharmaceutical packing to commodity packaging
Higher requirement.Biological macromolecule material using biodegradability is that environmental type packaging material made of substrate is more next
More it is valued by people.
Edible film is to come using edible natural substance to have porous network structure film made from raw material with raw material
The advantages that source is extensive, safe and non-toxic, becomes one of research hotspot of packaging field.Isinglass is passed through by collagen in fish-skin, fish-bone
The polypeptides matter that partial hydrolysis obtains has good film forming, biocompatibility and biodegradability and is answered extensively
Exploitation for protide membrane material.However, the barrier property and antioxygenic property of the single film of isinglass are poor, as food packet
The performance of package material, isinglass (FG) single film is still to be improved.
Oxidized starch (OS) is to aoxidize ative starch under given conditions using oxidant, so that the alcohol hydroxyl on the position C2, C3, C6
Base is oxidized to aldehyde radical, ketone group or carboxyl, and α-Isosorbide-5-Nitrae-glycosidic bond is oxidized the converted starch that the degree of polymerization that fracture obtains reduces.Oxygen
Changing starch has many excellent performances, as water dispersible is good, mobility is strong, gelatinization point is low, good film-forming property, easy cross-linked graft
Deng.Especially schiff base reaction can occur with protein, can be cross-linking modified to protein progress, improve the stability and power of protein
Learn performance etc..However, for preparing the research of composite membrane using isinglass and oxidized starch blending almost without report.
Summary of the invention
The present invention proposes a kind of isinglass/compound edible film of oxidized starch dual network, preparation method and its application, this is multiple
Closing edible film has good barrier property and fresh-keeping effect.
In order to achieve the above object, the present invention provides a kind of isinglass/compound edible films of oxidized starch dual network, this is multiple
Close edible film using isinglass as matrix, using oxidized starch as crosslinking agent, using schiff base reaction and heat treatment induction isinglass and
Interpenetrating is crosslinked between oxidized starch to be prepared.
The present invention also provides a kind of isinglass/oxidized starch dual network compound edible film preparation method, including it is following
Step:
Isinglass solution and oxidized starch solution are prepared respectively, and isinglass solution and oxidized starch solution are carried out respectively
Isinglass solution and oxidized starch solution are mixed after cooling, after sufficiently reacting under constant temperature, obtain casting solution by heat treatment, will
Casting solution pours into culture dish, dry, obtains isinglass/compound edible film of oxidized starch dual network.
Preferably, the mass ratio of isinglass and oxidized starch is 10:(1-5 in the casting solution).
Preferably, the mass ratio of isinglass and oxidized starch is 10:3 in the casting solution.
Preferably, the casting solution further includes the glycerol that mass fraction is 3%.
Preferably, it is described respectively to isinglass solution and oxidized starch solution carry out heat treatment include:
Isinglass solution is heated at 80 DEG C, oxidized starch solution is heated at 60 DEG C.
Preferably, the reaction temperature sufficiently reacted under the constant temperature is 50 DEG C, time 4h.
The present invention also provides a kind of isinglass as described in the above technical scheme/compound edible films of oxidized starch dual network
Application in terms of packaging material for food.
Compared with prior art, the advantages and positive effects of the present invention are:
By the covalent cross-linking between isinglass and oxidized starch, the isinglass/oxidized starch being prepared is compound edible
Film has good barrier property, and it is bad that quality caused by food is waited because of oxidation/moisture evaporation/enzymatic reaction can be effectively relieved
Change, while the compound edible film has the characteristics that nontoxic, biodegradable, good biocompatibility, provides one for food service industry
The environmentally protective edible packaging material of kind.
Detailed description of the invention
Fig. 1 is the SEM schematic diagram of compound edible film provided by the embodiment of the present invention and single film, wherein (a) adds for OS
Dosage is the SEM schematic diagram of the 1.5% compound edible film being prepared；(b) be OS additive amount be 1% be prepared it is compound can
Eat the SEM schematic diagram of film；It (c) is the SEM schematic diagram of the single film of isinglass；
Fig. 2 is influence schematic diagram of the difference coating processing provided by the embodiment of the present invention to apple sample b* value；
Fig. 3 is influence schematic diagram of the difference coating processing provided by the embodiment of the present invention to apple sample weight loss rate；
Fig. 4 is influence of the difference coating processing to apple sample solubility solid content provided by the embodiment of the present invention
Schematic diagram；
Fig. 5 is influence signal of the difference coating processing provided by the embodiment of the present invention to apple sample titratable acid content
Figure；
Fig. 6 is the FTIR spectrogram of compound edible film provided by the embodiment of the present invention and single film.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The embodiment of the invention provides a kind of isinglass/compound edible film of oxidized starch dual network, the compound edible film with
Isinglass is matrix, using oxidized starch as crosslinking agent, using schiff base reaction and heat treatment induction isinglass and oxidized starch it
Between crosslinking interpenetrating be prepared.
In the embodiment, it is that isinglass is by the collagen warp in fish-skin, fish-bone using isinglass as the advantage of matrix
The polypeptides matter that partial hydrolysis obtains has good film forming, biocompatibility and biodegradability.Oxidized starch is
Aoxidize ative starch under given conditions using oxidant so that the alcoholic extract hydroxyl group on the position C2, C3, C6 be oxidized to aldehyde radical, ketone group or
Carboxyl, α-Isosorbide-5-Nitrae-glycosidic bond are oxidized the converted starch that the degree of polymerization that fracture obtains reduces.Oxidized starch has many Optimalities
Can, such as water dispersible is good, mobility is strong, gelatinization point is low, good film-forming property, easy cross-linked graft.Using oxidized starch as crosslinking agent,
Schiff base reaction occurs by oxidized starch and isinglass, covalent cross-linking effect occurs for formation-C=N group, can to isinglass into
Row is cross-linking modified, forms the compound edible film of isinglass/oxidized starch of dual network structure, improves the stability of compound edible film
And mechanical property.The compound edible film has good water content, moisture-vapor transmission, oil penetrating rate, OTR oxygen transmission rate, transparency
And external appearance characteristic, meanwhile, it is a kind of novel environmentally protective edible film which, which has the characteristics that environmentally protective,.
Isinglass/oxidized starch is prepared using crosslinking interpenetrating between schiff base reaction and heat treatment induction isinglass and oxidized starch
The compound edible film of dual network, wherein heat treatment is that the good isinglass of transparency/oxidized starch dual network is prepared is compound edible
The key of film.
The embodiment of the invention also provides a kind of isinglass/oxidized starch dual network compound edible film preparation method, packets
Include following steps:
Isinglass solution and oxidized starch solution are prepared respectively, and isinglass solution and oxidized starch solution are carried out respectively
Isinglass solution and oxidized starch solution are mixed after cooling, after sufficiently reacting under constant temperature, obtain casting solution by heat treatment, will
Casting solution pours into culture dish, dry, obtains isinglass/compound edible film of oxidized starch dual network.
In the embodiment, it is bright to be that one side is conducive to fish for the advantage of preparation isinglass solution and oxidized starch solution respectively
The abundant dissolution of glue and oxidized starch；On the other hand protein uncoiling degenerative process has occurred in dissolved isinglass, solves spiral shell
Isinglass after rotation denaturation, which is easier to crosslink with oxidized starch, to react.Isinglass solution and oxidized starch solution are carried out respectively
The reason of heat treatment, is, if isinglass solution and oxidized starch solution are prepared before mixing without heat treatment
Film transparency it is not high；Isinglass solution by heat treatment can carry out uncoiling degenerative process to a greater extent, warp
Oxidized starch solution after crossing heat treatment can more fully be dissolved, and may advantageously facilitate between isinglass and oxidized starch
Cross-linking reaction, improve the compound edible film of isinglass/oxidized starch transparency.Isinglass and oxidized starch are abundant at a constant temperature
Reaction, the process are crosslinked interpenetrating using between heat treatment induction isinglass and oxidized starch, obtain casting solution, carry out to casting solution
It is dried, obtains isinglass/compound edible film of oxidized starch dual network.
In a preferred embodiment, the mass ratio of isinglass and oxidized starch is 10:(1-5 in the casting solution).The reality
It applies example and specifically defines the mass ratio of isinglass and oxidized starch in casting solution, the reason is that, the matter of isinglass and oxidized starch
Amount compares water content, moisture-vapor transmission, oil penetrating rate, OTR oxygen transmission rate, the transparency of the compound edible film of isinglass/oxidized starch
It is affected with external appearance characteristic.The two ratio is lower than 10:5 or when being higher than 10:1, the correlation for the compound edible film being prepared
It can be poor.It is understood that the mass ratio of isinglass and oxidized starch can also be in 10:4,10:3,10:2 and its range
Any point value ratio.
In a preferred embodiment, the mass ratio of isinglass and oxidized starch is 10:3 in the casting solution.The embodiment
Specifically define in casting solution that the mass ratio of isinglass and oxidized starch is 10:3, the reason is that, when in casting solution isinglass with
When the mass ratio of oxidized starch is 10:3, its water content of the best performance of the compound edible film of isinglass/oxidized starch is
14.54%, moisture-vapor transmission 3.64gm-1d-1MPa-1, oil penetrating rate 0.88gm-2h-1, OTR oxygen transmission rate 11.23cm3m-2d-10.1MPa-1, the compound edible film under the proportion has that compatibility is optimal between good barrier property and matrix, can reach most
Good fresh-keeping effect.In addition, SEM schematic diagram as shown in Figure 1 is it can be found that when the additive amount of oxidized starch is 1.5%, fish is bright
When the content of glue is 5%, compound edible film smooth surface is intermolecular phenomenon of phase separation do not occur；The surface layer of single film
Inhomogenous, flatness is poor, there is obvious gap and particle, this may be due to intermolecular interaction in the single film of FG
It is weaker to cause；With the increase of oxidized starch additive amount, when oxidized starch additive amount is 2%, and the content of isinglass is 5%,
, there is a little granular substance in compound edible film surface smoothness decline, it may be possible to due to the excessive caused molecule of solute concentration
Reunion causes.SEM result is demonstrated from microcosmic angle when the mass ratio of isinglass in casting solution and oxidized starch is 10:3, system
The best performance of standby obtained compound edible film.
In a preferred embodiment, the casting solution further includes the glycerol that mass fraction is 3%.In the embodiment, it is added
Glycerol can make film obtained soft and have certain tensile strength as plasticizer.It is understood that in embodiment
Plasticizer be not limited to cited by above-described embodiment, can also be those skilled in the art according to common sense this field into
Other substances that row is reasonably selected and adjusted.
In a preferred embodiment, it is described respectively to isinglass solution and oxidized starch solution carry out heat treatment include:
Isinglass solution is heated at 80 DEG C, oxidized starch solution is heated at 60 DEG C.
In this embodiment, isinglass solution and oxidized starch solution are heat-treated within specified temperatures, reason is 80
DEG C carrying out heat treatment to isinglass may be implemented isinglass protein uncoiling degenerative process, at 60 DEG C to oxidized starch solution into
Row heat treatment is conducive to the abundant dissolution of oxidized starch, promotes the cross-linking reaction between isinglass and oxidized starch.
In a preferred embodiment, the reaction temperature sufficiently reacted under the constant temperature is 50 DEG C, time 4h.The embodiment
Specifically reaction temperature and the time of isinglass and oxidized starch are defined, the reason is that, under this condition, isinglass and oxidation are formed sediment
The compatibility of powder solution is best, can sufficiently crosslink reaction, otherwise, it is insufficient to will lead to reaction.
Isinglass/oxidized starch dual network that the embodiment of the invention also provides a kind of as described in above-mentioned any embodiment is multiple
Close application of the edible film in terms of packaging material for food.The isinglass/compound edible film of oxidized starch dual network can be effectively relieved
Food because of quality deterioration caused by oxidation/moisture evaporation/enzymatic reaction etc., while have the characteristics that again it is nontoxic, biodegradable,
The problem of white pollution for non-degradable film is able to solve as packaging material bringing and the wasting of resources, while overcoming again single
Film is existing barrier property and the poor technical problem of antioxygenic property as packaging material for food, provides a kind of green ring
Protect edible packaging material.
In order to become apparent from, to introduce isinglass provided by the embodiment of the present invention/oxidized starch dual network in detail compound edible
Film, preparation method and its application, are described below in conjunction with specific embodiment.
Embodiment 1
The oxidized starch solution that the isinglass solution and concentration that compound concentration is 10% respectively are 5%, magnetic agitation 5h make
Sample sufficiently dissolves.Isinglass solution is stirred into 30min, oxidized starch stirring in water bath 30min at 60 DEG C under 80 DEG C of water-baths.
After cooling, isinglass solution and oxidized starch solution are mixed with isinglass and oxidized starch mass ratio for the ratio of 10:1,
In, the mass fraction of isinglass is 10% in mixed solution, and the mass fraction of oxidized starch is 1%, and water-bath 4h makes at 50 DEG C
After the two is sufficiently reacted, 3% glycerol is added, stirs evenly.10g film liquid is taken to pour into the polyethylene culture dish that diameter is 90mm
In, it is put into 50 DEG C of baking oven dry 15h, isinglass/compound edible film of oxidized starch dual network is prepared.
Embodiment 2
Isinglass/the preparation method is the same as that of Example 1 for the compound edible film of oxidized starch dual network, the difference is that isinglass
It is 10:2 with oxidized starch mass ratio.
Embodiment 3
Isinglass/the preparation method is the same as that of Example 1 for the compound edible film of oxidized starch dual network, the difference is that isinglass
It is 10:3 with oxidized starch mass ratio.
Embodiment 4
Isinglass/the preparation method is the same as that of Example 1 for the compound edible film of oxidized starch dual network, the difference is that isinglass
It is 10:4 with oxidized starch mass ratio.
Embodiment 5
Isinglass/the preparation method is the same as that of Example 1 for the compound edible film of oxidized starch dual network, the difference is that isinglass
It is 10:5 with oxidized starch mass ratio.
Comparative example 1
The isinglass solution that compound concentration is 5%, magnetic agitation 5h dissolve sample sufficiently.By isinglass solution at 80 DEG C
Stir 30min under water-bath, after cooling, by it at 50 DEG C water-bath 4h, 3% glycerol is added, stirs evenly.10g film liquid is taken to fall
Enter in the polyethylene culture dish that diameter is 90mm, is put into 50 DEG C of baking oven dry 15h, it is edible that isinglass list network is prepared
Film.
Comparative example 2
Alginic acid is prepared centainly to match (sodium alginate additive amount (w/w) 1.5%, isinglass additive amount (w/w) 3.5%)
Its magnetic agitation 5h dissolves sample sufficiently by sodium-isinglass mixed solution, and the glycerol of rear addition 3% stirs evenly.It will mix
The sample got togather is placed in heating 40min (period is stirred continuously) in 70 DEG C of water-baths, is immediately placed in ultrasonic water bath pot after taking-up
It is de-gassed (30min).It takes 10g film liquid to pour into the polyethylene culture dish that diameter is 90mm, is put into 50 DEG C of baking oven dry
The compound edible film of isinglass-sodium alginate is prepared in 15h.
Comparative example 3
Isinglass/the preparation method is the same as that of Example 1 for the compound edible film of oxidized starch dual network, the difference is that, fish is bright
Sol solution and oxidized starch solution are not heat-treated.
In composite membrane preparation process, there is insoluble phenomenon in composite membrane liquid, it is seen that apparent white solid, isinglass with
Reaction cannot be crosslinked between oxidized starch, the composite film surface particle being prepared is obvious.
Performance test
It prepared by the isinglass prepared by embodiment 1-5/compound edible film of oxidized starch dual network, comparative example 1
Isinglass/oxidized starch of isinglass/sodium alginate composite membrane, the preparation of comparative example 3 prepared by the single film of isinglass, comparative example 2
Composite membrane is put into the drying basin (RH 60%, room temperature) for filling saturation KBr solution and saves, and measures every film properties afterwards for 24 hours.
1, thickness measurement
With micrometer measurement isinglass/compound edible film of oxidized starch dual network, the single film of isinglass and isinglass/
The thickness of four vertex of sodium alginate composite membrane and central point, calculates the thickness that average value is calculated as the film, and data are shown in Table 1.
2, water content test (MC test)
Weigh respectively 0.3g isinglass/compound edible film of oxidized starch dual network, the single film of isinglass and isinglass/
Sodium alginate composite membrane, counting its quality is m1, drying is placed it in into the aluminium box of constant weight, and both meters gross mass is m2After be put into
105 DEG C of oven dryings are to constant weight m3。
Calculate film moisture content:
MC=(m2- m3)/m1× 100% (1)
In formula, m1For membrane sample quality, g；m2It is dry preceding aluminium box and membrane sample quality, g；m3For aluminium box and film after drying
Sample quality, g.
The MC data of composite membrane and single film are shown in Table 1.
3, moisture-vapor transmission test (WVP test)
It is bright unabroken isinglass/compound edible film of oxidized starch dual network, the single film of isinglass and fish have been taken
Glue/sodium alginate composite membrane, is overlying on the glass bottle opening equipped with 9g anhydrous calcium chloride, is around bonded with vaseline, weighing.It sets
It balances in the drying basin of RH 60%, weighs after 4d.
Calculate the moisture-vapor transmission of composite membrane and single film:
WVP=Δ md/At Δ P (2)
In formula, WVP- moisture transmitance, gm-1d-1MPa-1；Δ m- vial quality incrementss, g；The thickness of d- film, m；A-
Effective moisture-inhibiting area of film, m2；T- moisture-inhibiting time, d；Δ P- film two sides water vapour pressure is poor, MPa.
The WVP data of composite membrane and single film are shown in Table 1.
4, oil penetrating rate test (OP test)
Test tube is dry to constant weight, 5mL or so soybean oil is added, the edible film sealing taken covers one on sealed membrane
Open filter paper stable in advance, weighing.Test tube is inverted and placed into the environment of RH 60%, weighs the quality of filter paper afterwards for 24 hours.
Calculate the oil penetrating rate of edible film:
OP=Δ m/At (3)
In formula, OP- oil penetrating rate, gm-2h-1；Δ m- filter paper quality incrementss, g；Effective pasta product of A- film, m2；T- is saturating
Oily time, h.
The OP data of composite membrane and single film are shown in Table 1.
5, OTR oxygen transmission rate test (OTR test)
According to GB/T1038-2000 " plastic film and thin slice gas-premeable test method ", air permeability tester is used
Carry out oxygen flow test.The OTR data of composite membrane and single film are shown in Table 1.
The barrier property test data of 1 composite membrane of table and single film
As seen from the results in Table 1, comparative example 1 is below by WVP, OP, OTR data of the embodiment 1-5 composite membrane prepared to make
Standby single film, composite membrane data prepared by comparative example 2,3, and WVP, OP, OTR data of film are the important fingers of film barrier property
Mark, value is lower, and the barrier property of film is better.Therefore, the composite membrane of heat treatment preparation, resistance are combined by addition oxidized starch
Separating performance is greatly improved.In addition, MC, WVP, OP, OTR of composite membrane are influenced by oxidized starch additive amount, when fish is bright
When the concentration of glue and oxidized starch is respectively 5% and 1.5%, the barrier property of composite membrane is best.
6, fresh keeping property is tested
It takes position pulp among apple to be cut into 15mm × 15mm × 15mm cube, is placed in open aluminium box, it will
Film is overlying at aluminium box mouth, and is tied up with rubber band.Choosing, as control, is placed at room temperature without the coated sample of film, is become in monitoring 5d
Change.
6.1 appearance color
Observe the apparent variation of apple, shooting record.Using color difference meter, first use whiteboard calibration, after measured with color difference meter
Apple surface color scale obtains measuring fruit surface chromatic value b* with color evaluating.B* is one of color scale of object color,
Champac color is represented, numerical value can reflect the degree of oxidizing brown stain during Apples to a certain extent.Experimental result is shown in figures
2。
6.2 mass change
Weight-loss ratio calculates:
R=(m1-m2)/m1× 100% (4)
In formula, R is weight-loss ratio；m1For the initial weight of apple, g；m2To store fruit quality after a certain period of time, g.
Experimental result is shown in Fig. 3 for weight-loss ratio.
6.3 flavor indexs and nutritional quality
Soluble solid refers to the general name that can be dissolved in the compound of water, including soluble sugar, titratable acid, dimension in fruits and vegetables
Raw element etc., content changes with fruits and vegetables after-ripening process, and the fruits and vegetables stage of ripeness is continuously increased, and the fruits and vegetables aging rotten stage is then continuous
The soluble solid content for declining fruits and vegetables, can be used as an important indicator for judging fruits and vegetables storability.
Titratable acid is one of the important indicator for evaluating fruit-vegetable quality, the breathing of the catabolism and fruit of organic acid content
Act on related, titratable acid changes of contents amplitude is smaller, illustrates that membrane sample inhibits the effect of respiration of fruits effect better.
Apple total dissoluble solid content (TSS) is measured using hand-held saccharometer, as a result sees Fig. 4；Aqueous slkali titration
Titratable acid content is measured, as a result sees Fig. 5.
Fresh keeping property test result shows composite membrane to the fresh keeping property of apple better than single film, isinglass/oxidized starch
Composite membrane has lower OTR oxygen transmission rate, stronger water preventing ability, can effectively prevent apple sample from being oxidized discoloration and apple
Weightlessness caused by due to dehydration；The soluble solid content of the apple sample of composite membrane covering presents to rise in storage period to become
Gesture, but occur without peak value, illustrate that the putrefaction process of fruit is retarded, meanwhile, the solubility of the apple sample of composite membrane covering
Solid content is lower than the soluble solid content of single film；The test result of titratable acid shows composite membrane and single film pair
Apple sample was metabolized certain adjustment effect, thus delay the cumulative process of the substances such as titratable acid in apple sample,
Simultaneously because the crosslinked action of isinglass and oxidized starch forms result more closely in composite membrane, uniform membrane structure is right
Delaying the cumulative process of the substances such as titratable acid in apple sample has better effect.Particularly, when the additive amount of isinglass is
5%, when the additive amount of oxidized starch is 1.5%, the properties of composite membrane are best.
7, FTIR is tested
By above-mentioned test result it can be found that the properties of composite membrane are superior to the performance of single film, and work as isinglass
Additive amount be 5%, when the additive amount of oxidized starch is 1.5%, the properties of composite membrane are best, each in order to study composite membrane
The reason of raising of item performance, FTIR test analysis is carried out to composite membrane and single film, as a result such as Fig. 6.Wherein, 3283-
3284cm-1Place be-OH the absorption peak (amide A) to be formed is superimposed with the stretching vibration absworption peak of-NH, the absorption peak peak shape it is wider and
Greatly；3299cm-1Place is the-OH absorption peak in OS；2924-2930cm-1The absorption peak at place is the-CH stretching vibration (amide of side chain
B)；1632-1637cm-1Place is the stretching vibration of I area C=O of amide, related with Secondary structure；1549cm-1It inhales at place
The bending vibration that peak is II area-NH of amide is received, it is related with the aquation of protein molecule；1239cm-1Place is III area C-N of amide
It is related with tropocollagen molecule helical structure with absorption peak caused by-NH stretching vibration；1037cm-1Place is-OH and-C- in glycerol
O-C- stretching vibration absworption peak.
As can be seen from Table 2, there is some difference for each absorption peak wavelength of different samples, analysis the reason is as follows that.It is compound in amide A
The absorption peak of film is mobile to low wave direction, and reason may be that FG and OS forms intermolecular hydrogen bonding, and the formation of hydrogen bond keeps electron cloud close
Degree equalization causes infrared spectroscopy mobile to low wave direction so that stretching vibration frequency be made to reduce.Meanwhile the single film of FG is to low
The movement of wave direction also demonstrates the presence of intramolecular hydrogen bond.
The different edible film sample F TIR characteristic absorption peak tables of comparisons of table 2
Composite membrane absorption peak is mobile to high wave direction in amide B, and absorption intensity increases, and reason is the peak Raman spectrum-CH
The displacement of position is related with aliphatic amino acid residue hydrophobicity, shadow of the FG aliphatic amino acid side chains by hydrophobicity ring in OS
It rings, the increase of absorption intensity, bond energy enhancing in part causes the variation of compound film dynamic performance.
I area's composite membrane absorption peak of amide is mobile to low wave direction, illustrates that both isinglass and oxidized starch occur nucleophilic and take
Generation reaction generates amide, the absorption intensity decline of 5%+2.0% composite membrane, and reason may be that oxidized starch is full of in isinglass egg
In white matter network structure, it is broken a part of Harmonic Protein Molecular Chains.And the absorption intensity of 5%+1.5% composite membrane increases, explanation
Compatibility is preferable between isinglass and oxidized starch under this concentration.
Absorption intensity enhancing in II area's composite membrane of amide, illustrates isinglass and oxidized starch is intermolecular stronger hydrogen bond
Effect, the formation of hydrogen bond have the dispersion conducive to oxidized starch in isinglass film, can make to protect between isinglass and oxidized starch
Hold good compatibility.The variation of 5%+1.5% composite membrane is more apparent, illustrates that composite membrane mixed effect is preferable under this concentration.
For the absorption frequency of composite membrane and single film at this absorption peak without significant change, reason may be fish in IIIth area of amide
No change has taken place for the helical structure of gelatin tropocollagen molecule.
In addition, composite membrane is in 1157-1179cm-1There is new absorption peak in place, shows to deposit between isinglass and oxidized starch
It is acted in covalent cross-linking, and the high similarity of composite membrane and single film infrared absorpting light spectra also illustrates that isinglass and oxidation form sediment
There is good compatibility between powder.
Claims (8)
1. isinglass/compound the edible film of oxidized starch dual network, which is characterized in that the compound edible film is using isinglass as base
Matter, using oxidized starch as crosslinking agent, using schiff base reaction and heat treatment induction isinglass and oxidized starch between be crosslinked interpenetrating
It is prepared.
2. isinglass according to claim 1/oxidized starch dual network compound edible film preparation method, feature exist
In, comprising the following steps:
Isinglass solution and oxidized starch solution are prepared respectively, and isinglass solution and oxidized starch solution are heated respectively
Isinglass solution and oxidized starch solution are mixed after cooling, after sufficiently reacting under constant temperature, casting solution are obtained, by casting film by processing
Liquid pours into culture dish, dry, obtains isinglass/compound edible film of oxidized starch dual network.
3. according to the method described in claim 2, it is characterized in that, in the casting solution isinglass and oxidized starch mass ratio
For 10:(1-5).
4. according to the method described in claim 3, it is characterized in that, in the casting solution isinglass and oxidized starch mass ratio
For 10:3.
5. according to the method described in claim 2, it is characterized in that, the casting solution further includes the glycerol that mass fraction is 3%.
6. according to the method described in claim 2, it is characterized in that, it is described respectively to isinglass solution and oxidized starch solution into
Row heats
Isinglass solution is heated at 80 DEG C, oxidized starch solution is heated at 60 DEG C.
7. according to the method described in claim 2, it is characterized in that, the reaction temperature sufficiently reacted under the constant temperature be 50 DEG C,
Time is 4h.
8. isinglass according to claim 1/compound edible film of oxidized starch dual network is in terms of packaging material for food
Using.
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| CN112314838A (en) * | 2020-10-29 | 2021-02-05 | 成都大学 | Antibacterial food fresh-keeping Pickering emulsion and preparation method thereof |
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