CN106543743B - A kind of collagen hydrolysate containing linalool/edible antibacterial film of chitosan quaternary ammonium salt and preparation method thereof - Google Patents
A kind of collagen hydrolysate containing linalool/edible antibacterial film of chitosan quaternary ammonium salt and preparation method thereof Download PDFInfo
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- CN106543743B CN106543743B CN201610917687.4A CN201610917687A CN106543743B CN 106543743 B CN106543743 B CN 106543743B CN 201610917687 A CN201610917687 A CN 201610917687A CN 106543743 B CN106543743 B CN 106543743B
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- quaternary ammonium
- linalool
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- ammonium salt
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L89/00—Compositions of proteins; Compositions of derivatives thereof
-
- 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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- 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
- 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
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
Abstract
The present invention relates to a kind of collagen hydrolysate containing linalool/edible antibacterial film of chitosan quaternary ammonium salt and preparation method thereof, the raw material components of the antibacterial film are as follows: collagen hydrolysate 4-8 wt%, chitosan quaternary ammonium salt 1-4 wt%, linalool 0.4-1.2 wt%, glycerol 0.8-1.6 wt%, Tween-80 0.1-0.3 wt%, surplus are deionized water.Edibility antibacterial film prepared by the present invention has good anti-microbial property, and chitosan quaternary ammonium salt and linalool show good Synergistic antimicrobial to Escherichia coli, and preparation is simple, at low cost, safe and non-toxic.
Description
Technical field
The invention belongs to antibiotic packaging material technical fields, and in particular to a kind of collagen hydrolysate/shell containing linalool
Edible antibacterial film of glycan quaternary ammonium salt and preparation method thereof.
Background technique
Plastic package material has many advantages, such as the molding of light, durable, at low cost, easy processing, to consumer bring it is many just
Benefit.But its refractory organics causes serious environmental problem.Environmental problem caused by plastics package is to the life of people at present
Living and animals and plants existence pose a serious threat.With the raising of the level of consumption, more and more consumers is more focused on eating
The safety and sense organ of product, put forward higher requirements the quality of packaging material for food.In recent years, edibility antimicrobial packaging is as one
Kind green package becomes research hotspot.Edible packing film is that one kind had not only had food packaging function but also edible packing timber
Material.It for raw material, is made with edible natural large biological molecule (such as protein, polysaccharide, lipid) by certain processing technology
The film that compact structure prepared by interaction occurs between different molecular, since its good film forming and biology can drop
Solution property and by favor.
In order to improve the storage quality of fruits and vegetables, extend its shelf life, some antibacterial agents, which are often used in, inhibits fruits and vegetables to rot.
Common antibacterial agent is divided into synthetic antibacterial agents and natural antibacterial agent, it is contemplated that synthetic antibacterial agents bring security risk, Ren Menyue
More to tend to the development and utilization of highly-safe, good biocompatibility natural antibacterial agent.Natural antibacterial agent is divided into mineral substance again
(such as blue stone, realgar), animal class (such as chitin, chitosan and its derivative etc.) and plant (such as cortex cinnamomi, lemon,
Thymol etc.).In recent years, preparing the most common natural antibacterial agent of antibacterial film mainly includes chitosan and its derivative and plant
Essential oil class.Since the biocidal property of chitosan and its derivative is influenced by factors such as preparation conditions, tend not to reach fine
Fungistatic effect.Plants essential oil is usually the substance with aromatic odor extracted from positions such as the root of plant, stem, leaf, fruits,
Wherein comprising there are many with bacteriostatic activity alcohol, phenol, aldehyde, terpenes constituents, they be not only able to kill contacted with film it is thin
Bacterium can also inhibit the growth of film surrounding bacterial by its volatility, to greatly improve its fungistatic effect and increase antibacterial
Range.The present invention in order to improve collagen hydrolysate/chitosan quaternary ammonium salt edible antibacterial film antibacterial activity, plant by addition antibiotic property
The effective component linalool of object essential oil prepares the packaging material for food with good antibacterial activity.In addition to this, due to edible virtue
The peculiar property of camphor tree alcohol, in terms of prepared membrane material can also be applied to beauty skin-care face mask, edible cosmetic mask.
Summary of the invention
The purpose of the present invention is to provide a kind of collagen hydrolysate containing linalool/edible antibacterial film of chitosan quaternary ammonium salt
And preparation method thereof, the shortcomings that making up the antibacterial range and intensity limitation of single antibacterial agent, preparation has Synergistic antimicrobial activity,
And the green package membrane material with good mechanical properties.The present invention selects collagen hydrolysate and chitosan quaternary ammonium salt as film
Material matrix adds linalool as natural antibacterial agent, is prepared by mixing into the membrane material with good antibacterial activity.
Collagen hydrolysate is the large biological molecule through extracting in fish-skin and fish-bone, because it is with good biocompatibility
It is widely used in the exploitation of protide membrane material with biodegradability, the collagen hydrolysate that the present invention selects is mostly derived from
Tuna, inkfish and the extraction of squid.Chitosan quaternary ammonium salt is to pass through one kind of chemical modification preparation by chitosan with water-soluble
Property higher derivative, antibiotic property is all had under acid, alkalinity and neutrallty condition, although chitosan quaternary ammonium salt is as antibacterial
Agent has safe and nontoxic advantage, but its antibacterial ability is limited, bad especially for fungal microbe inhibitory effect.And
Linalool is due to its special physicochemical properties, to Escherichia coli, proteus, enteritis film bacillus, staphylococcus, wine brewing ferment
Female bacterium, white have good antibacterial activity containing coccus, black-koji mould etc..The present invention is by collagen hydrolysate and chitosan quaternary ammonium
Matrix of the salt as membrane material, mixing linalool preparation have the antibacterial film of synergetic antibacterial effect.Due to chitosan quaternary ammonium salt and
The Antibacterial Mechanism of linalool is different, and the opposite membrane material containing single antibacterial agent, antimicrobial film material of the present invention has better antibacterial
Property.In addition to this, inventive film material has good mechanical performance.
To achieve the above object, the present invention adopts the following technical scheme that, a kind of collagen hydrolysate/shell containing linalool is poly-
The sugared edible antibacterial film of quaternary ammonium salt, the raw material components of the antibacterial film are as follows: collagen hydrolysate 4-8 wt%, chitosan quaternary ammonium salt 1-4
Wt%, linalool 0.4-1.2 wt%, glycerol 0.8-1.6 wt%, Tween-80 0.1-0.3 wt%, surplus is deionized water.
Further, the raw material components of the antibacterial film are as follows: 4 wt% of collagen hydrolysate, 1 wt% of chitosan quaternary ammonium salt,
1.2 wt% of linalool, 1 wt% of glycerol, 0.3 wt% of Tween-80, surplus is deionized water.
The present invention also protects the preparation side of the collagen hydrolysate containing the linalool/edible antibacterial film of chitosan quaternary ammonium salt
Method, comprising the following steps:
(1) it the preparation of collagen hydrolyzate solution: weighs suitable collagen hydrolysate and deionized water is added, be placed in 50-
Magnetic agitation forms collagen hydrolyzate solution in 80 DEG C of water-baths；
(2) it the preparation of chitosan quaternary ammonium salting liquid: weighs suitable chitosan quaternary ammonium salt and deionized water is added, be placed in 50-
Magnetic agitation forms chitosan quaternary ammonium salting liquid in 80 DEG C of water-baths；
(3) preparation of linalool solution: linalool is added in the deionized water containing Tween-80, magnetic agitation is equal
Linalool solution is formed after even；
(4) preparation of edible antibacterial film: first by the chitosan of the collagen hydrolyzate solution of step (1) and step (2)
Quaternary ammonium salt solution is uniformly mixed, and the linalool solution of step (3) and the glycerol as plasticizer is then added, by high speed dispersion
Film liquid is finally spread over drying and forming-film 24-48h on poly (methyl methacrylate) plate under the conditions of 25-40 DEG C by standing and defoaming afterwards, is made containing virtue
The collagen hydrolysate of the camphor tree alcohol/edible antibacterial film of chitosan quaternary ammonium salt.
Further, the magnetic agitation time of step (1) and step (2) is respectively 30min and 60min.
Further, in step (4) at revolving speed 20000rpm high speed dispersion 3-10min.
Compared with prior art, the present invention having the following beneficial effects:
(1) present invention selects collagen hydrolysate as membrane material matrix, and abundance is cheap.It is mainly
It is obtained from fish-skin and fish-bone through peracid or alkali partial hydrolysis, there is good film formation at low temp.
(2) present invention selects chitosan quaternary ammonium salt as membrane matrix and antibacterial agent, and good water solubility to prepare work
Skill is simpler, and in addition it all has antibiotic property under acid, alkalinity and neutrallty condition, and safe and nontoxic.
(3) plant-derived essential oil linalool is used in antibacterial film by the present invention, has obtained the green package with antibiotic property
Film, while having widened the application field of linalool.
(4) edibility antibacterial film prepared by the present invention has good anti-microbial property, and chitosan quaternary ammonium salt and fragrant camphor tree
Alcohol shows good Synergistic antimicrobial to Escherichia coli, and effect is apparently higher than single antibacterial agent, while its antibacterial effect is also bright
Aobvious the case where being higher than chitosan and addition plants essential oil such as limonene.In addition, due to the superior water solubility of chitosan quaternary ammonium salt,
So that preparation is simple, and it is at low cost, it is safe and non-toxic.
Detailed description of the invention
Fig. 1 is inhibition zone of the film prepared by Examples 1 to 4 to Escherichia coli
Wherein (a), (b), (c), Examples 1 to 4 (d) is respectively represented.
Inhibition zone of the film prepared by Fig. 2 Examples 1 to 4 to staphylococcus aureus
Wherein (A), (B), (C), (D) respectively represent Examples 1 to 4.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, without structure
At limitation of the present invention.
Embodiment 1
It weighs the magnetic agitation dissolution in 60 DEG C of water-baths of 4g collagen hydrolysate 95.2mL deionized water and fish glue is made
Former hydrolyzate solution is added 0.8g glycerol as plasticizer, stirs evenly, 60 DEG C of standing and defoamings.Finally pipette the film liquid of 20mL
It spreads on poly (methyl methacrylate) plate, film-forming temperature is 25 DEG C, film formation time 48h, can be from poly (methyl methacrylate) plate after film is dry
Removing obtains collagen hydrolysate/edible antibacterial film of chitosan quaternary ammonium salt.Film liquid antibacterial activity is measured using borehole method, diameter is
The circular hole of 10mm investigates antibacterial film to the fungistatic effect of Escherichia coli and staphylococcus aureus respectively, and the results are shown in Table 1.
In addition the thickness of film, mechanical performance are determined, the results are shown in Table 2.
Embodiment 2
It weighs the magnetic agitation dissolution in 60 DEG C of water-baths of 4g collagen hydrolysate 50mL deionized water and collagen is made
Hydrolyzate solution；By 1g chitosan quaternary ammonium salt, with 44mL deionized water, chitosan is made in the magnetic agitation dissolution in 60 DEG C of water-baths
Then quaternary ammonium salt aqueous solution mixes the two, 1g glycerol is added as plasticizer, stirs evenly, 60 DEG C of standing and defoamings.Most move back
The film liquid of 20mL is taken to spread on poly (methyl methacrylate) plate, film-forming temperature is 25 DEG C, film formation time 48h, can be from after film is dry
Removing obtains collagen hydrolysate/edible antibacterial film of chitosan quaternary ammonium salt on poly (methyl methacrylate) plate.It is anti-using borehole method measurement film liquid
Bacterium activity, diameter are the circular hole of 10mm, investigate antibacterial film respectively to the fungistatic effect of Escherichia coli and staphylococcus aureus, knot
Fruit is as shown in Figure 1 and Figure 2.In addition the thickness of film, mechanical performance are determined, the results are shown in Table 2.
Embodiment 3
It weighs the magnetic agitation dissolution in 60 DEG C of water-baths of 4g collagen hydrolysate 50mL deionized water and collagen is made
Hydrolyzate solution；By 1g chitosan quaternary ammonium salt, with 44mL deionized water, chitosan is made in the magnetic agitation dissolution in 60 DEG C of water-baths
Then quaternary ammonium salt aqueous solution mixes the two, 1g glycerol is added as plasticizer, stirs evenly；The linalool of 0.4g is being contained
There is dissolution in the 5mL deionized water of 0.12g Tween-80 that linalool lotion is made, it is poly- to be then added into collagen hydrolysate/shell
In sugared quaternary ammonium mixed salt solution, and high speed dispersion is carried out, 60 DEG C of standing and defoamings.The film liquid for finally pipetting 20mL spreads into organic glass
In glass plate, film-forming temperature is 25 DEG C, film formation time 48h, can remove from poly (methyl methacrylate) plate after film is dry and obtain fish glue
The former edible antibacterial film of hydrolysate/chitosan quaternary ammonium salt.Film liquid antibacterial activity is measured using borehole method, diameter is the circular hole of 10mm,
Antibacterial film is investigated respectively to the fungistatic effect of Escherichia coli and staphylococcus aureus, and the results are shown in Table 1.In addition to the thickness of film
Degree, mechanical performance are determined, and the results are shown in Table 2.
Embodiment 4
It weighs the magnetic agitation dissolution in 60 DEG C of water-baths of 4g collagen hydrolysate 50mL deionized water and collagen is made
Hydrolysate aqueous solution；By 1g chitosan quaternary ammonium salt, with 44mL deionized water, the magnetic agitation dissolution in 60 DEG C of water-baths is made shell and gathers
Sugared quaternary ammonium salt aqueous solution, then mixes the two, and 1g glycerol is added as plasticizer, stirs evenly；The linalool of 1.2g is existed
Linalool lotion is made in dissolution in 5mL deionized water containing 0.36g Tween-80, is then added into collagen hydrolysate/shell
In glycan quaternary ammonium mixed salt solution, and high speed dispersion is carried out, 60 DEG C of standing and defoamings.Finally pipette 20mL film liquid spread into it is organic
On glass plate, film-forming temperature is 25 DEG C, film formation time 48h, can remove from poly (methyl methacrylate) plate after film is dry and obtain fish
The edible antibacterial film of collagen hydrolysate/chitosan quaternary ammonium salt.Film liquid antibacterial activity is measured using borehole method, diameter is the circle of 10mm
Antibacterial film is investigated to the fungistatic effect of Escherichia coli and staphylococcus aureus in hole respectively, and the results are shown in Table 1.In addition to film
Thickness, mechanical performance be determined, the results are shown in Table 2.
Collagen hydrolysate film and collagen hydrolysate/the edible antibacterial of chitosan quaternary ammonium salt prepared under 1 different condition of table
The inhibition zone of film
As shown in Table 1, pure collagen hydrolysate film is without inhibition zone, after adding chitosan quaternary ammonium salt it is visible have it is antibacterial
Circle.It adds after linalool it can be seen that apparent inhibition zone, and with the increase of linalool concentration, inhibition zone is gradually increased.Separately
Outer chitosan quaternary ammonium salt and linalool, which have the inhibition of Escherichia coli and staphylococcus aureus, to act synergistically, embodiment 4
Effect it is especially pronounced.
Collagen hydrolysate film and collagen hydrolysate/the edible antibacterial of chitosan quaternary ammonium salt prepared under 2 different condition of table
The mechanical performance of film
As shown in Table 2, compared to pure collagen hydrolysate film, the addition of chitosan quaternary ammonium salt destroys collagen hydrolysate point
The ordered structure of subchain keeps strand more loose, so as to cause the increase of film thickness.In addition with the addition of linalool, film
Thickness be also gradually increased.Mainly since linalool is lyophobic dust, the incompatibility of it and collagen hydrolysate film makes
The microstructure of antibacterial film becomes more loose, and then causes the thickness of film to increase, while the tensile strength of film is dropped
It is low, but the increase of elongation at break avoids the brittle fracture of film, and the effect of embodiment 4 is especially pronounced.
Embodiment described above is preferred embodiments of the invention, without limiting practical range of the invention.Therefore, all
It is equivalent modifications made by the essence of content according to the present invention, all should belong within the scope of the present invention.
Claims (4)
1. a kind of collagen hydrolysate containing linalool/edible antibacterial film of chitosan quaternary ammonium salt, which is characterized in that described edible anti-
The raw material components of mycoderm are as follows: collagen hydrolysate 4-8 wt%, chitosan quaternary ammonium salt 1-4 wt%, linalool 0.4-1.2 wt%, sweet
Oily 0.8-1.6 wt%, Tween-80 0.1-0.3 wt%, surplus is deionized water；Preparation method are as follows:
(1) it the preparation of collagen hydrolyzate solution: weighs suitable collagen hydrolysate and deionized water is added, be placed in 50-80 DEG C
Magnetic agitation forms collagen hydrolyzate solution in water-bath；
(2) it the preparation of chitosan quaternary ammonium salting liquid: weighs suitable chitosan quaternary ammonium salt and deionized water is added, be placed in 50-80 DEG C
Magnetic agitation forms chitosan quaternary ammonium salting liquid in water-bath；
(3) preparation of linalool solution: linalool is added in the deionized water containing Tween-80, after magnetic agitation is uniform
Form linalool solution；
(4) preparation of edible antibacterial film: first by the chitosan quaternary ammonium of the collagen hydrolyzate solution of step (1) and step (2)
Salting liquid is uniformly mixed, and the linalool solution of step (3) and the glycerol as plasticizer is then added, quiet after high speed dispersion
Deaeration is set, film liquid is finally spread over into drying and forming-film 24-48h on poly (methyl methacrylate) plate under the conditions of 25-40 DEG C, is made and contains linalool
Collagen hydrolysate/edible antibacterial film of chitosan quaternary ammonium salt.
2. edible antibacterial film according to claim 1, which is characterized in that the raw material components of the edible antibacterial film are as follows: fish
4 wt% of collagen hydrolysate, 1 wt% of chitosan quaternary ammonium salt, 1.2 wt% of linalool, 1 wt% of glycerol, Tween-80 0.3 wt% are remaining
Amount is deionized water.
3. edible antibacterial film according to claim 1, which is characterized in that the magnetic agitation time of step (1) and step (2)
Respectively 30min and 60min.
4. edible antibacterial film according to claim 1, which is characterized in that in step (4) at revolving speed 20000rpm at a high speed
Disperse 3-10min.
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| CN201610917687.4A CN106543743B (en) | 2016-10-21 | 2016-10-21 | A kind of collagen hydrolysate containing linalool/edible antibacterial film of chitosan quaternary ammonium salt and preparation method thereof |
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| CN201610917687.4A CN106543743B (en) | 2016-10-21 | 2016-10-21 | A kind of collagen hydrolysate containing linalool/edible antibacterial film of chitosan quaternary ammonium salt and preparation method thereof |
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| CN107903638A (en) * | 2017-11-20 | 2018-04-13 | 武汉大学 | A kind of soybean protein isolate/chitosan quaternary ammonium salt composite membrane and preparation method and application |
| CN110200190A (en) * | 2019-07-18 | 2019-09-06 | 广东省生物工程研究所（广州甘蔗糖业研究所） | Harmful microbe spice composition in a kind of inhibition food |
| CN111620966B (en) * | 2020-06-23 | 2021-07-27 | 江南大学 | Chitosan oligosaccharide-N-linalool copolymer and preparation method and application thereof |
| CN115226889B (en) * | 2022-07-25 | 2024-04-05 | 广州市宝桃食品有限公司 | Green and safe food additive and preparation method thereof |
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| CN105384974A (en) * | 2015-12-15 | 2016-03-09 | 张进 | Chitosan biomembrane |
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| CN105384974A (en) * | 2015-12-15 | 2016-03-09 | 张进 | Chitosan biomembrane |
Non-Patent Citations (2)
| Title |
|---|
| Diffusion of linalool and methylchavicol from polyethylene-based antimicrobial packaging films;Panuwat Suppakul et al;《LWT-Food Science and Technology》;20111231;第44卷;第432-438页 |
| Effect of chitosan-gelatin film incorporated with ethanolic red grape seed extract and Ziziphora clinopodioides essential oil on survival of Listeria monocytogenes and chemical, microbial and sensory properties of minced trout fillet;Shabnam Kakaei et al;《LWT-Food Science and Technology》;20160508(第72期);第1888-1893页 |
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