CN106046402B - A kind of edible packing membrane and preparation method thereof based on chitosan - Google Patents
A kind of edible packing membrane and preparation method thereof based on chitosan Download PDFInfo
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Abstract
The present invention relates to a kind of edible packing membrane and preparation method thereof based on chitosan.The industrialized production and practical, commercial of edible packing membrane are not popularized, most important the reason is that its mechanical strength is insufficient and without heat sealability.The present invention uses the tape casting, chitosan solution is mixed with gelatin solution or starch solution, glycerol, propolis and lysozyme is added, ultrasonic degassing after cooling is blended in constant temperature, standing obtains composite membrane liquid, and composite membrane liquid is laid in vacuum drying in plate and obtains edible packing membrane.Improve chitosan filming performance by large biological molecules ingredients such as addition starch, gelatin in the present invention, not only increase the mechanical performance of chitosan complex film, natural bacteriostatic ingredient lysozyme and propolis with synergy are added simultaneously, so that the ability of microbial reproduction, extension effective period of food quality is inhibited to greatly enhance when chitosan complex film is as food packaging, it can be used for industrialized production, have broad application prospects.
Description
Technical field
The present invention relates to food processing technology fields, and in particular to a kind of edible packing membrane and its system based on chitosan
Preparation Method.
Background technique
Edible packing membrane refers to is with edible natural material (such as protein, polysaccharide, cellulose and its derivates)
Raw material, the film with functional characteristic formed by the interaction between different molecular, can pass through package, coating, microcapsules
Etc. forms be covered in food surface (or internal), the infiltration of aqueous vapor, other gases or various solutes can be obstructed, and play protection
The thin layer of effect, prevent food occur in transporting procedures flavor, in terms of variation, and then guarantee food quality,
Extend Food Shelf-life, or reduces packing cost.Thus have broad application prospects in terms of food industry.
But up to the present, almost without edible packing membrane energy industrialized production and realize business application, it is most important
The reason is that edible film mechanical strength is insufficient and without heat sealability, while edible film is compared with conventional plastic packaging etc., isolation
The scarce capacity of microorganism, as food packaging in use, there is the risk of microbial contamination.
Summary of the invention
The shortcomings that in order to overcome edible packing membrane in the prior art, an object of the present invention are to provide a kind of based on shell
The edible packing membrane of glycan improves chitosan filming performance by large biological molecules ingredients such as addition starch, gelatin,
It is improved its mechanical strength and heat sealability, bacteriostasis property and oxygen resistance；By adding natural bacteriostatic agent, so that shell is poly-
The ability of microbial reproduction, extension effective period of food quality is inhibited to greatly enhance when sugared composite membrane is as food packaging.
The second object of the present invention is to provide a kind of preparation method of above-mentioned edible packing membrane based on chitosan.
The technical scheme adopted by the invention is as follows:
A kind of preparation method of the edible packing membrane based on chitosan, it is characterised in that:
Successively the following steps are included:
Step 1: by chitosan and glacial acetic acid aqueous solution (1-2.5) in mass ratio: (97.5-99) is mixed, and is placed in magnetic force and is stirred
It mixes and is stirred well to chitosan on device and is completely dissolved, ultrasonic degassing 30min, the mass fraction for obtaining clear is 1%-2.5%
Chitosan solution；
Step 2: it is (1-2): 1 ratio according to the mass ratio of chitosan and gelatin or starch, shell obtained by step 1 is gathered
Sugar juice is mixed with gelatin solution or starch solution, and the plasticizer glycerol of chitosan mass 15%-40% is added, is filtered to remove insoluble
Property impurity；Stirring on magnetic stirring apparatus is placed in 10min is blended under 80 DEG C of constant temperatures, is cooled to 25 DEG C to being uniformly mixed,
It is separately added into the propolis of chitosan mass 20%-50% and the lysozyme of chitosan mass 40%-60% again as natural bacteriostatic agent, surpasses
Sound degassing 30min, stands 1h, obtains composite membrane liquid；
Step 3: it takes 10-40ml composite membrane liquid to be laid in 10cm × 10cm square plate, is placed in a vacuum drying oven
Drying and forming-film, vacuum oven temperature are 25 DEG C -35 DEG C, drying time 32-48h.
In step 1, the deacetylation of the chitosan is 95%.
In step 1, the volume fraction of the glacial acetic acid aqueous solution is 1%.
In step 2, the starch is cornstarch, potato starch or pea starch.
In step 2, the starch solution the preparation method comprises the following steps:
By starch and distilled water (1-2) in mass ratio: (98-99) is mixed, under 80 DEG C of water bath conditions heating stirring until
Gelatinization completely obtains the starch solution that mass fraction is 1%-2%.
In step 2, the edible alcohol of propolis volume fraction 95% dissolves, the quality of the propolis and edible alcohol
Than for 1:3 or 1:4.
Edible packing membrane made from a kind of preparation method of the edible packing membrane based on chitosan as mentioned.
The present invention has following technical advantage compared with prior art: the present invention uses the tape casting, is film forming with chitosan
Matrix prepares edible packing membrane, and specific technical solution is to mix chitosan solution with gelatin solution or starch solution, is added
Ultrasonic degassing after cooling is blended in glycerol, propolis and lysozyme, constant temperature, and standing obtains composite membrane liquid, and composite membrane liquid is laid in plate
Middle vacuum drying obtains edible packing membrane.Firstly, making shell by large biological molecules ingredients such as addition starch, gelatin in the present invention
Glycan filming performance is greatly improved, and enhances the mechanical performance of chitosan complex film, the reason is that chitosan-starch or bright
Interaction of hydrogen bond between glue improves mechanical and physical property as internal factor.Meanwhile chitosan and starch or gelatin
There is compatibility well in the solution, composite membrane flat appearance obtained is smooth, and the comprehensive performance of gained edible film
It further increases.Secondly, natural bacteriostatic ingredient lysozyme and propolis with synergy is added, so that chitosan complex film is made
To inhibit the ability of microbial reproduction, extension effective period of food quality to greatly enhance when food packaging, it can be used for industrialized production, have
Wide application prospect.
Specific embodiment
The present invention will be described in detail With reference to embodiment.
Embodiment 1
In order to overcome, insufficient and without heat sealability the technological deficiency of edible film mechanical strength, the present embodiment are mentioned in the prior art
Supplied a kind of preparation method of edible packing membrane based on chitosan, successively the following steps are included:
Step 1: by chitosan and glacial acetic acid aqueous solution (1-2.5) in mass ratio: (97.5-99) is mixed, and is placed in magnetic force and is stirred
It mixes and is stirred well to chitosan on device and is completely dissolved, ultrasonic degassing 30min, the mass fraction for obtaining clear is 1%-2.5%
Chitosan solution；
Step 2: it is (1-2): 1 ratio according to the mass ratio of chitosan and gelatin or starch, shell obtained by step 1 is gathered
Sugar juice is mixed with gelatin solution or starch solution, and the plasticizer glycerol of chitosan mass 15%-40% is added, is filtered to remove insoluble
Property impurity；Stirring on magnetic stirring apparatus is placed in 10min is blended under 80 DEG C of constant temperatures, is cooled to 25 DEG C to being uniformly mixed,
It is separately added into the propolis of chitosan mass 20%-50% and the lysozyme of chitosan mass 40%-60% again as natural bacteriostatic agent, surpasses
Sound degassing 30min, stands 1h, obtains composite membrane liquid；
Step 3: it takes 10-40ml composite membrane liquid to be laid in 10cm × 10cm square plate, is placed in a vacuum drying oven
Drying and forming-film, vacuum oven temperature are 25 DEG C -35 DEG C, drying time 32-48h.
Embodiment 2:
The present embodiment on the basis of embodiment 1, as a preferred embodiment, a kind of based on the edible of chitosan
The preparation method of property packaging film, successively the following steps are included:
Step 1: chitosan is mixed with glacial acetic acid aqueous solution 2:98 in mass ratio, is placed on magnetic stirring apparatus and sufficiently stirs
It mixes to chitosan and is completely dissolved, ultrasonic degassing 30min obtains the chitosan solution that the mass fraction of clear is 2%；
Step 2: the ratio for being 1.5:1 according to the mass ratio of chitosan and gelatin or starch, by chitosan obtained by step 1
Solution is mixed with gelatin solution or starch solution, and the plasticizer glycerol of chitosan mass 25% is added, is filtered to remove insoluble miscellaneous
Matter；Stirring on magnetic stirring apparatus is placed in 10min is blended under 80 DEG C of constant temperatures, is cooled to 25 DEG C, then divide to being uniformly mixed
Not Jia Ru chitosan mass 35% propolis and chitosan mass 50% lysozyme as natural bacteriostatic agent, ultrasonic degassing 30min,
1h is stood, composite membrane liquid is obtained；
Step 3: it takes 25ml composite membrane liquid to be laid in 10cm × 10cm square plate, is placed in a vacuum drying oven dry
Dry film forming, vacuum oven temperature are 30 DEG C, drying time 40h.
As preferred embodiment, in the present embodiment step 1, chitosan and glacial acetic acid aqueous solution may be used also in mass ratio
Think 1:99 or 1.5:98.5 or 2.5:97.5, or the arbitrary value between 1:99 and 2.5:97.5, quality is made respectively
Score is 1% or 1.5% or 2.5%, or between 1%-2.5% arbitrary value chitosan solution.
As preferred embodiment, in the present embodiment step 2, chitosan and gelatin-compounded or chitosan and starch are multiple
It closes, prepares composite membrane liquid.The mass ratio of chitosan and gelatin or starch can also be 1:1 or 2:1, or between 1:1 and 2:1 it
Between arbitrary value；The additive amount of glycerol can also be the 15% or 20% or 30% or 35% or 40% of chitosan mass, or between
Arbitrary value between 15%-40%；
The additive amount of the above chitosan additive amount, chitosan and the quality of gelatin or starch when glycerol need to be according to different use
The index requests such as thickness, moisture-vapor transmission, tensile strength, the fracture elongation of way edible film are selected.
In the present embodiment step 2, the additive amount of propolis can also be chitosan mass 20% or 25% or 30% or 40%,
Or 45% or 50%, or the arbitrary value between 20%-50%；The additive amount of lysozyme can also be chitosan mass 40%, or
45% or 55% or 60%, or the arbitrary value between 40%-60%.The selection of propolis and lysozyme additive amount is according to edibility
The purposes of film, as packaging film when content species, depending on holding conditions etc..Its collaboration suppression can be determined by bacteriostatic test
Bacterium ability.
As preferred embodiment, in the present embodiment step 3, the pour mask amount of composite membrane liquid can be 10ml, or
15ml or 20ml or 30ml or 35ml or 40ml, or the arbitrary value between 10ml-40ml, reciprocal modulus is not mainly according to
Thickness requirement with purposes edible film is selected, and moisture-vapor transmission, tensile strength, the fracture elongation of film are comprehensively considered
Equal index requests.
In the present embodiment step 3, vacuum oven temperature can also be 25 DEG C or 35 DEG C, or between 25 DEG C -35 DEG C it
Between arbitrary value, mainly selected according to reciprocal modulus；Drying time can also be 32h or 34h or 36h or 40h, or
42h or 44h or 48h, 48h, or the arbitrary value between 32h-48h, are mainly selected according to reciprocal modulus and drying temperature
It selects.Optimal drying process condition can be obtained by experiment.
Embodiment 3
The present embodiment is on the basis of embodiment 1-2, as a preferred embodiment, the shell is poly- in step 1
The deacetylation of sugar is 95%, i.e., chitosan used in the present embodiment is food-grade deacetylation chitosan, deacetylation
It is 95%.
As a preferred embodiment, the volume fraction of the glacial acetic acid aqueous solution is 1%, chitosan in step 1
It can effectively dissolve.
Embodiment 4
The present embodiment is on the basis of embodiment 1-3, as a preferred embodiment, in step 2, the starch
For cornstarch, potato starch or pea starch.
Embodiment 5
The present embodiment on the basis of examples 1 to 4, as a preferred embodiment, in step 2, the starch
Solution the preparation method comprises the following steps:
By starch and distilled water (1-2) in mass ratio: (98-99) is mixed, under 80 DEG C of water bath conditions heating stirring until
Gelatinization completely obtains the starch solution that mass fraction is 1%-2%.
In the preparation of the present embodiment starch solution, the mass ratio of starch and distilled water is 1:99 or 1.5:98.5 or 2:98,
Or the arbitrary value between 1:99-2:98, mainly selected according to mass ratio of the type of starch, starch and chitosan etc..
Embodiment 6
The present embodiment is on the basis of embodiment 1-5, as a preferred embodiment, in step 2, the propolis
It is dissolved with the edible alcohol of volume fraction 95%, the mass ratio of the propolis and edible alcohol is 1:3 or 1:4.
Embodiment 7
The edible packaging as made from a kind of preparation method of edible packing membrane based on chitosan of embodiment 1-6
Film.
The obtained edible film based on chitosan in the present embodiment passes through the large biological molecules such as addition starch, gelatin
Ingredient makes chitosan filming performance be greatly improved, and enhances the mechanical performance of chitosan complex film, the reason is that chitosan-
Interaction of hydrogen bond between starch or gelatin improves mechanical and physical property as internal factor.Meanwhile chitosan and shallow lake
Powder or gelatin have good compatibility in the solution, and composite membrane flat appearance obtained is smooth, and gained edible film
Comprehensive performance further increases.Secondly, natural bacteriostatic ingredient lysozyme and propolis with synergy is added, so that chitosan
Inhibit the ability of microbial reproduction, extension effective period of food quality to greatly enhance when composite membrane is as food packaging, can be used for industrializing
Production, has broad application prospects.
Embodiment 8
In the present embodiment, to the edibility made from the preparation method of the edible packing membrane of chitosan in embodiment 7
Packaging film has carried out pertinent instruments measurement, is analyzed its thickness, moisture-vapor transmission, tensile strength and elongation percentage, tool
Body is as follows:
1, thickness:
In the present embodiment, the thickness of chitosan complex film obtained is optimal to can reach 30-65 μm.With made from the prior art
Edible film is smaller compared to its thickness, and in same thickness, mechanical strength properties are more excellent.
2, moisture-vapor transmission (water vapor permeability, WVP):
The moisture-vapor transmission of chitosan complex film referred within the unit time, under unit steam pressure, through film thickness
Degree, the water vapour amount of unit area.Moisture-vapor transmission is a very important parameter for measuring edible film performance,
Height will have a direct impact on the quality of packaging product, and different composite membranes, its moisture-vapor transmission is different, vapor
Transmitance is smaller, shows that the water preventing ability of film is better, and vapor is less susceptible to pass through, and the anti-corrosion effect of film is better, is more conducive to prolong
The shelf-life of long food.
The measuring method of moisture-vapor transmission is as follows:
Under the conditions of 25 DEG C, in test cup (1384.74mm2× 25mm) in be put into anhydrous calcium chloride (granularity be less than 2mm),
Calcium chloride and rim of a cup distance are less than 5mm, seal test rim of a cup with chitosan complex film.Test rim of a cup after weighing is placed in and is equipped with
In the drier of saturated sodium chloride solution (25 DEG C, RH75%), makes to keep certain vapour pressure deficit inside and outside film, taken every 1d
It weighs out, until mass change is less than 0.001g, each sample does 5 in parallel.Moisture-vapor transmission calculation method is shown in formula:
WVP=md/AtΔP
In formula:
Quality of the m-through the moisture of film, g；
D-sample thickness, mm；
A-penetrates the membrane area of moisture, mm2；
T-moisture penetrates time, s；
Δ P-film two sides moisture vapor pressure difference (Pa), since the RH gradient of film two sides is 100%, measuring temperature is 25 DEG C,
Therefore Δ P is 3.16kPa.
In the present embodiment, the moisture-vapor transmission of measured chitosan complex film is 7 × 10-8 g·mm-1·s-1·
pa-1~10 × 10-8 g·mm-1·s-1·pa-1.Compared with the edible film of same thickness in the prior art, vapor is saturating
It is lower to cross rate.
3, tensile strength (TS):
Single chitosan film brittleness is larger, and pulling rubbing with tearing will be crushed, and stretching force is also poor, after adding gelatin,
The tensile strength of chitosan-gelatin composite membrane becomes larger, and extensibility is also preferable.When gelatine content improves in composite membrane, film resists
Tensile strength is significantly improved compared with the single film of chitosan, illustrates to add the drawing that suitable gelatin helps to improve film in chitosan
Stretch intensity.It should be noted that the elongation at break of composite membrane is reduced with the increase of gelatine content.Chitosan has good
Film forming, and the gelatin for being not easy to form a film will lead to composite membrane and become fragile, and decline the elongation at break of film.
Chitosan-starch composite membrane tensile capacity made from three kinds of starch becomes larger, but after adding starch, composite membrane
Ductility slightly reduce, it is poor for the relatively single chitosan film of suppleness.There is correlative study report to point out, in chitosan list
When component forms a film, the tensile strength of film increases with the increase of chitosan concentration.Influence structure that its related factor is polymer,
The molecules align of average molecular weight and polymer.Chitosan concentration is bigger, i.e., the molecular number in unit volume is more, high when film forming
The interaction force of molecule interchain is stronger, and intermolecular cross-linking is closer, and film strength is bigger.
In the present embodiment, it can determine that addition gelatin still adds starch and gelatin by experiment and conjunctival purposes
Or the additive amount of starch.
The measuring method of tensile strength:
Film is cut into dumbbell shape strip with cutter, standard sample is made, measures the thickness and width of film, omnipotent test machine measurement
Tensile strength and elongation when film ruptures, determination condition 10mm/min.
Tensile strength calculates according to the following formula:
TS=P/(bd)
In formula:
TS-tensile strength, MPa；
The maximum tension born when P-sample fracture, N；
B-specimen width, mm；
D-sample thickness, mm
It can reach 16-45Mpa by the tensile strength that test measures packaging film of the present invention.
4, fracture elongation (E):
The measuring method of elongation at break:
Film is cut into dumbbell shape strip with cutter, standard sample is made, measures the thickness and width of film, omnipotent test machine measurement
Tensile strength and elongation when film ruptures, determination condition 10mm/min.
Elongation at break calculates according to the following formula:
E=(L1-L0)/L0×100%
In formula:
E-elongation at break, %；
L0Distance between the original graticule of-sample, mm；
L1Distance when-sample fracture between graticule, mm.
It can reach 5.4%-6.8% by the fracture elongation that test measures packaging film of the present invention.
5, water-soluble:
The water-soluble measuring method of composite membrane:
Film (40mm × 40mm) is put into the weighing bottle of 40 × 25mm, then is dried to constant weight, after weighing in drier
It is put into 300ml distilled water, is dissolved 12 hours at 25 DEG C of room temperature, then film is dried under conditions of 60 DEG C to constant weight, according to
Its weight change calculates water-soluble.
Water-soluble %=(W2-W3) × 100%/(W2-W1)
In formula: W1The weight of-weighing bottle, g；W2The total weight of weighing bottle and film, g when-first time drying constant weight；W3—
The total weight of weighing bottle and film, g when second of dry constant weight.
The water-soluble of composite membrane increases and reduction with chitosan ratio.Water-soluble size is related with the performance of membrane material.
Chitosan is hydrophilic high molecular material, and in water, film, which will not dissolve, to be swollen.Also containing a large amount of parents in Gelatin Macromolecule chain
Aqueous group, so it is water-soluble also in contrast lower.But starch belongs to water-soluble high-molecular material, as starch contains
Amount increases, and the ability that composite membrane is dissolved in water increases, potato and pea starch be formed by film have compared with cornstarch it is higher molten
Xie Xing.Corresponding compound film formulation can be selected according to the purposes of film.
It can reach 23%-40% by the water solubility that test measures packaging film of the present invention.
Reagent used in embodiment 1-8 and raw material are food-grade.
The contents of the present invention are not limited to cited by embodiment, and those of ordinary skill in the art are by reading description of the invention
And to any equivalent transformation that technical solution of the present invention is taken, all are covered by the claims of the invention.
Claims (4)
1. a kind of preparation method of the edible packing membrane based on chitosan, it is characterised in that:
Successively the following steps are included:
Step 1: by chitosan and glacial acetic acid aqueous solution (1-2.5) in mass ratio: (97.5-99) is mixed, and is placed in magnetic stirring apparatus
On be stirred well to chitosan and be completely dissolved, ultrasonic degassing 30min, the mass fraction for obtaining clear is the shell of 1%-2.5%
Glycan solution；
Step 2: being (1-2): 1 ratio according to the mass ratio of chitosan and gelatin, by chitosan solution obtained by step 1 with it is bright
Sol solution mixing, is added the plasticizer glycerol of chitosan mass 15%-40%, is filtered to remove insoluble impurities；It is placed in magnetic agitation
Stirring is blended 10min under 80 DEG C of constant temperatures, is cooled to 25 DEG C, then be separately added into chitosan matter to being uniformly mixed on device
The propolis of 20%-50% and the lysozyme of chitosan mass 40%-60% are measured as natural bacteriostatic agent, ultrasonic degassing 30min is stood
1h obtains composite membrane liquid；
Step 3: it takes 10-40ml composite membrane liquid to be laid in 10cm × 10cm square plate, is placed in a vacuum drying oven drying
Film forming, vacuum oven temperature are 25 DEG C -35 DEG C, drying time 32-48h；
In step 2, the edible alcohol of propolis volume fraction 95% dissolves, and the mass ratio of the propolis and edible alcohol is
1:3 or 1:4.
2. a kind of preparation method of edible packing membrane based on chitosan according to claim 1, it is characterised in that:
In step 1, the deacetylation of the chitosan is 95%.
3. a kind of preparation method of edible packing membrane based on chitosan according to claim 1, it is characterised in that:
In step 1, the volume fraction of the glacial acetic acid aqueous solution is 1%.
4. edible made from a kind of preparation method of edible packing membrane based on chitosan as claimed in claim 1,2 or 3
Property packaging film.
Priority Applications (1)
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| CN107011543A (en) * | 2017-04-05 | 2017-08-04 | 湖北工程学院 | A kind of edible food packaging film and preparation method thereof |
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| CN111434709A (en) * | 2019-01-14 | 2020-07-21 | 新疆大学 | Preparation method of hexahydro β -acid/cyclodextrin inclusion compound-chitosan antibacterial film |
| CN110100882A (en) * | 2019-04-19 | 2019-08-09 | 杭州千岛湖纯浙农业开发有限公司 | Fruit freshness preserving pulvis and preparation method thereof |
| CN112280067B (en) * | 2019-07-24 | 2022-06-10 | 南京理工大学 | Preparation method of edible antibacterial film |
| CN110483842A (en) * | 2019-08-12 | 2019-11-22 | 广东美士达药包材料股份有限公司 | A kind of preparation process of Environmentally-frieantibacterial antibacterial pharmaceutical packaging composite membrane |
| CN112300582A (en) * | 2020-11-20 | 2021-02-02 | 安阳工学院 | Degradable antibacterial film containing wormwood essential oil and preparation method thereof |
| CN112745535A (en) * | 2020-12-30 | 2021-05-04 | 江苏大学 | Preparation method of gallic acid crosslinked chitosan-gelatin active composite membrane |
| CN113174071B (en) * | 2021-04-26 | 2022-07-01 | 东北林业大学 | Press sealing method of anionic polysaccharide film |
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