CN105694320A - Plant source extract anti-bacterial preservative film, and preparation method and application thereof - Google Patents

Plant source extract anti-bacterial preservative film, and preparation method and application thereof Download PDF

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CN105694320A
CN105694320A CN201610169863.0A CN201610169863A CN105694320A CN 105694320 A CN105694320 A CN 105694320A CN 201610169863 A CN201610169863 A CN 201610169863A CN 105694320 A CN105694320 A CN 105694320A
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solution
preservative film
extracts
film
preparation
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CN105694320B (en
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周武艺
李锦珍
梁淦
谷文祥
刘威
董先明
许维田
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Guangzhou Yixinshu Biotechnology Co.,Ltd.
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South China Agricultural University
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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
    • C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
    • C08L29/02—Homopolymers or copolymers of unsaturated alcohols
    • C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • 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
    • 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
    • C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
    • C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • 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
    • C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
    • C08J2471/02—Polyalkylene oxides
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/06—Biodegradable
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/14—Gas barrier composition
    • 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

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
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Abstract

The invention discloses a plant source extract anti-bacterial preservative film, and a preparation method and application thereof. According to the method, boracic acid and hydrochloric acid are used for modifying vinol; then, the modified vinol is uniformly mixed with nanometer titania; next, the mixture is uniformly mixed with crofton weed ethanol extracts emulsified by tween-80; film casting is performed; the materials are dried under the natural conditions; the plant source extract anti-bacterial preservative film is obtained. The film has the proper oxygen permeability and moisture permeability; due to plant source extracts contained in the preservative film, preserved articles can be prevented from getting rotten through being infected by bacteria; ethylene gas generated by fruit and vegetables can be degraded by nanometer materials; meanwhile, the film also has excellent mechanical property. The plant source extract anti-bacterial preservative film is mainly applied to the fields of preservative package of fruit and vegetables, sea products and cereal subsidiary food and the like, and can also be applied to food container coverage, so that the food is prevented from getting rotten through being polluted by bacteria; the storage life is prolonged.

Description

A kind of Extracts from Plant Recourses antimicrobial preservative film and preparation method thereof and application
Technical field
The present invention relates to a kind of preservative film, particularly to a kind of Extracts from Plant Recourses antimicrobial preservative film and preparation method thereof and application。
Background technology
Along with the growth in the living standard of society, fruit increasingly frequently occurs on dining table, becomes daily necessities。How to keep the fresh mouthfeel of fruit, become orchard worker and consumer's questions of common interest。Conventional preservation method is cold preservation, but as tropical fruit (tree) preservations in the environment that temperature is relatively low such as Fructus Musae, fresh litchi, fresh Arillus Longan and Fructus Mangifera Indicae can destroy its color and luster and nutritive value, causes huge waste。The storage method that another one is commonly used utilizes preservative film that fresh vegetables fruit is preserved exactly。Preservative film in the market is PE and PP preservative film, this kind of preservative film is low due to water vapor transmittance, although the moisture of vegetable and fruit can well be kept, but can cause that the container bottom placing vegetable and fruit deposits a lot of moisture and carbon dioxide, some vegetable and fruit shelf lives can be made on the contrary very not desirable because of carbon dioxide poisoning etc.；Furthermore this kind of preservative film is all disposable, generally when rubbish abandons after being finished, and owing to reclaiming difficulty and can not degrade, cause severe contamination to environment。Along with consumer's enhancing gradually to food safety growing interest and environmental consciousness, safety is high and the biodegradable packaging material of product better quality can be kept to become the focus of research。The preservative film of the present invention, not only will not bring secondary pollution to environment but also steam and carbon dioxide balance inside and outside film can be reached, excellent sterilization component in eupatorium adenophorum extracting solution is applied in preservative film, not only makes it obtain rationalization utilization, also improve the suppression to fruit and vegetable surfaces mushroom。
Summary of the invention
The primary and foremost purpose of the present invention is in that the shortcoming overcoming prior art is with not enough, it is provided that the preparation method of a kind of Extracts from Plant Recourses antimicrobial preservative film。
Another object of the present invention is to provide the Extracts from Plant Recourses antimicrobial preservative film obtained by above-mentioned preparation method。
It is still another object of the present invention to provide the application of described Extracts from Plant Recourses antimicrobial preservative film。
The purpose of the present invention is achieved through the following technical solutions: the preparation method of a kind of Extracts from Plant Recourses antimicrobial preservative film, comprises the steps:
(1) polyvinyl alcohol is joined in deionized water, stand fully swelling to polyvinyl alcohol；Then stir under 80～95 DEG C of conditions and be completely dissolved to polyvinyl alcohol, obtain the poly-vinyl alcohol solution that concentration is 5～15wt%；In 30～45 DEG C, add, toward poly-vinyl alcohol solution, the boric acid solution that concentration is mass percent 5% under stirring, add hydrochloric acid solution and glycerol that concentration is 4mol/L after stirring reaction, continue at 30～45 DEG C of stirrings, obtain solution I；Concentration is the consumption of the boric acid solution of mass percent 5% is every 5～15g polyvinyl alcohol proportioning 3～5ml boric acid solution；Concentration is the consumption of the hydrochloric acid solution of 4mol/L is every 5～15g polyvinyl alcohol proportioning 2ml hydrochloric acid solution；The consumption of glycerol is every 5～15g polyvinyl alcohol proportioning 1～1.2g glycerol；
(2) nanometer titanium dioxide titanium solution is joined in solution I, in 30～45 DEG C of stirrings to being uniformly dispersed, obtain solution II；The consumption of nano titanium oxide is every 5～15g polyvinyl alcohol proportioning 0.01～0.03g nano titanium oxide；
(3) Eupatorium cannabinum L. (Eupatorium coelestinum L.) ethanol extraction and Tween 80 5～10:1～2 proportioning in mass ratio that concentration is 60mg/ml are mixed, stir to emulsifying uniform, obtain solution III；
(4) temperature treating solution II is 20～30 DEG C, drips solution III, stir in the solution II being under stirring, ultrasonic, stands, obtains solution IV；Effect that is ultrasonic and that stand is deaeration；The consumption of the solution III of solution II sum calculates by the Eupatorium cannabinum L. (Eupatorium coelestinum L.) ethanol extraction that every 5～15g polyvinyl alcohol proportioning 5～10g concentration is 60mg/ml；
(5) on clean flat board, pour solution IV, casting film-forming into, dry under natural conditions, obtain Extracts from Plant Recourses antimicrobial preservative film。
The time of the standing described in step (1) is preferably 12h。
Stirring described in step (1) be completely dissolved to polyvinyl alcohol in stirring condition be preferably 200rpm stir 1h。
The speed of the stirring described in step (1)～(3) is preferably 200rpm。
The time of the stirring reaction described in step (1) is preferably 0.5h。
The time continuing at 30～45 DEG C of stirrings described in step (1) is preferably 1h。
The concentration of the nanometer titanium dioxide titanium solution described in step (2) is preferably 10mg/ml。
The time of the stirring described in step (2) is preferably 0.5h。
Eupatorium cannabinum L. (Eupatorium coelestinum L.) ethanol extraction described in step (2) prepares preferably by following steps: dried Eupatorium cannabinum L. (Eupatorium coelestinum L.) is pulverized, sieved；The Eupatorium cannabinum L. (Eupatorium coelestinum L.) powder dehydrated alcohol obtained or alcohol solution dipping extract, and filter, and concentration obtains purple stem boneset extract。
Described sieve is preferably 40～100 mesh sieves。
Described alcoholic solution is the alcoholic solution of percent by volume 90～99.9%, it is preferred to the alcoholic solution of percent by volume 95%。
The condition of described extraction is preferably extracts 24h in 25～50 DEG C。
The number of times of described extraction is 1～3 time；It is preferably 3 times。
The speed of the stirring described in step (4) is preferably 500rpm。
The time stirred described in step (4) is preferably 0.5h。
Ultrasonic condition described in step (4) is preferably the ultrasonic 1h of 120W, 40000Hz。
The time of the standing described in step (4) is preferably 24h。
Flat board described in step (5) is preferably glass plate。
A kind of Extracts from Plant Recourses antimicrobial preservative film, is obtained by above-mentioned preparation method。
The application in packaging for foodstuff of the described Extracts from Plant Recourses antimicrobial preservative film。
The present invention has such advantages as relative to prior art and effect
(1) Extracts from Plant Recourses provided by the invention has a characteristic that 1. antimicrobial preservative film has a broad antifungal spectrum, and various bacteria brood body, fungal spore are all had inhibitory action；2. excellent slow release effect；3. PVA defect soluble in water is improved；4. Antibacterial Constituents will not directly contact with fruit and vegerable, and food stage packaging material are nontoxic；5. environmentally friendly Biodegradable material, does not constitute secondary pollution to environment；6. good permeability, long fresh-keeping period；7. when material of vegetable origin is Eupatorium cannabinum L. (Eupatorium coelestinum L.), belonging to weeds Appropriate application, cost is substantially reduced, and is conducive to commercially promoting。
(2) present invention utilizes the plant extraction liquid of biodegradable high molecular polymer and safety non-toxic evil and nano material to prepare antimicrobial preservative film。Do not affecting on the basis of PVA mechanical performance, giving the good antibiotic property of PVA and moisture pick-up properties, meanwhile, PVA is being made suitable modified so that it is there is after film forming excellent resistance to water, and method of modifying and material simple and convenient。The antibacterial guarantor's film making gained had both had the advantages such as easy to operate, with low cost, good mechanical performance, also has the performances such as good moisture-penetrable ventilated, antimildew and antibacterial simultaneously, has great application potential at food packaging applications。This preservative film can intercept steam and OTR oxygen transmission rate so that it is has suitable water vapor transmittance and fabulous oxygen obstruction rate, makes fruit and vegetable keep suitable moisture and is extended fresh keeping time without contacting with oxygen, thus having good fresh-keeping function。
Accompanying drawing explanation
Fig. 1 be PE film and PVA film to the weight-loss ratio testing result figure after fresh-keeping 7 days of cherry tomato, Fructus Jujubae and Capsicum frutescens L．Var．1o m Bail。
Fig. 2 be PE film and PVA film to the Decayed rate testing result figure after fresh-keeping 7 days of cherry tomato, Fructus Jujubae and Capsicum frutescens L．Var．1o m Bail。
Fig. 3 is the hot strength test figure of PE film and PVA film。
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this。
The preparation process of the Eupatorium cannabinum L. (Eupatorium coelestinum L.) ethanol extraction used by the present invention is as follows: Eupatorium cannabinum L. (Eupatorium coelestinum L.) leaf at room temperature dried and crushed, crosses 50 sieves, obtains Eupatorium cannabinum L. (Eupatorium coelestinum L.) powder；Eupatorium cannabinum L. (Eupatorium coelestinum L.) powder is put in extraction still, add the alcoholic solution that concentration is percent by volume 95%, in 40 DEG C of soak extraction 3 times, extract 24h every time, 8 layers of filtered through gauze, the gross mass consumption of alcoholic solution is equivalent to 4 times of Eupatorium cannabinum L. (Eupatorium coelestinum L.) leaf quality, and the filtrate after being combined carries out vacuum concentration with Rotary Evaporators, being concentrated into concentration is 60mg/ml (containing 60mg solids in every 1ml), obtains the concentrated solution of Eupatorium cannabinum L. (Eupatorium coelestinum L.)。
Concentration determination: accurately pipette uniform extract 1ml with liquid-transfering gun in vessel, is placed on freeze dryer and removes solvent, concentrate concentration=(m1-m2)/1ml, wherein m1For the quality of vessel and solid, m2Quality for vessel。
Embodiment 1
(1) preparation PVA film containing heterogeneity:
A film: join in 90g deionized water by 10g polyvinyl alcohol (PVA-088200), stands 12h so that it is fully swelling。Stirring 1h with the speed of 200 revs/min at the temperature of 80 DEG C, polyvinyl alcohol is completely dissolved, and prepared concentration is the poly-vinyl alcohol solution I of 10wt%；Solution I in 40 DEG C, add the boric acid solution 3ml of 0.5wt% under stirring (200rpm) state, add the hydrochloric acid 2ml and glycerol 1g of 4mol/L after stirring 0.5h, continue insulated and stirred 1h, obtain solution II；Take the nano-TiO that solids content is 10mg/ml2Solution 3mL adds in solution II, and insulated and stirred 30min is uniformly dispersed, obtains solution III, pours appropriate solution III, casting film-forming into, dry, obtain A film and be stored in exsiccator, treating antibacterial test under natural conditions on a clean plate glass；
B film: join in 90g deionized water by 10g polyvinyl alcohol (PVA-088200), stands 12h so that it is fully swelling。Stirring 1h with the speed of 200 revs/min at the temperature of 80 DEG C, polyvinyl alcohol is completely dissolved, and prepared concentration is the poly-vinyl alcohol solution I of 10wt%；Solution I in 40 DEG C, add the boric acid solution 3ml of 0.5wt% under stirring (200rpm) state, add the hydrochloric acid 2ml and glycerol 1g of 4mol/L after stirring 0.5h, continue insulated and stirred 1h, obtain solution II；Take the Eupatorium cannabinum L. (Eupatorium coelestinum L.) ethanol extraction 10g that solids content is 60mg/ml, add 1g Tween 80, at room temperature with the speed stirring and emulsifying of 200 revs/min, obtain solution III；Treat that solution II is cooled to room temperature, stir with the speed of 500 revs/min, in solution II, be slowly added dropwise solution III, stir 0.5h, 120W, the ultrasonic deaeration 1h of 40000Hz, stand 24h deaeration, obtain solution IV；A clean plate glass pours appropriate solution IV, casting film-forming into, dries under natural conditions, obtain B film and be stored in exsiccator, treating antibacterial test；
C film: join in 90g deionized water by 10g polyvinyl alcohol (PVA-088200), stands 12h so that it is fully swelling。Stirring 1h with the speed of 200 revs/min at the temperature of 80 DEG C, polyvinyl alcohol is completely dissolved, and prepared concentration is the poly-vinyl alcohol solution I of 10wt%；Solution I in 40 DEG C, add the boric acid solution 3ml of 0.5wt% under stirring (200rpm) state, add the hydrochloric acid 2ml and glycerol 1g of 4mol/L after stirring 0.5h, continue insulated and stirred 1h, obtain solution II；Take nano-TiO2(10mg/ml) solution 3mL adds in solution II, and insulated and stirred 30min is uniformly dispersed, obtains solution III；Take Eupatorium cannabinum L. (Eupatorium coelestinum L.) ethanol extraction (60mg/ml) 10g, add 2g Tween 80, at room temperature with the speed stirring and emulsifying of 200 revs/min, obtain solution IV；Treat that solution III is cooled to room temperature, stir with the speed of 500 revs/min, in solution III, be slowly added dropwise solution IV, stir 0.5h, 120W, the ultrasonic deaeration 1h of 40000Hz, stand 24h deaeration, obtain solution V；A clean plate glass pours appropriate solution V, casting film-forming into, dries under natural conditions, obtain C film and be stored in exsiccator, treating antibacterial test；
D film: join in 90g deionized water by 10g polyvinyl alcohol (PVA-088200), stands 12h so that it is fully swelling。Stirring 1h with the speed of 200 revs/min at the temperature of 80 DEG C, polyvinyl alcohol is completely dissolved, and prepared concentration is the poly-vinyl alcohol solution I of 10wt%；Solution I in 40 DEG C, add the boric acid solution 3ml of 0.5wt% under stirring (200rpm) state, the hydrochloric acid 2ml and glycerol 1g of 4mol/L is added after stirring 0.5h, continue insulated and stirred 1h, obtain solution II, a clean plate glass pours appropriate solution II, casting film-forming into, dries under natural conditions, obtain D film and be stored in exsiccator, treating antibacterial test。
(2) detection of antibiotic property:
The present invention adopts agar plate diffusion method to evaluate PVA preservative film to reference culture staphylococcus aureus (Staphylococcusaureus, deposit number CICC10001, Chinese industrial Microbiological Culture Collection administrative center) and escherichia coli (Escherichiacoli, deposit number CICC10899, Chinese industrial Microbiological Culture Collection administrative center) anti-microbial property。
The preparation of agar culture medium and fluid medium: bacteriological peptone 10g, beef extract 3g, sodium chloride 5g, agar powder 20g, add distilled water and be settled to 1000mL and boil abundant dissolving, regulating pH by NaOH solution is 7.0 ± 0.2, stand-by。Inoculum: bacteriological peptone 1g, beef extract 0.3g, sodium chloride 0.5g, add distilled water and be settled to 100mL, boil dissolving, regulating pH by NaOH solution is 6.8, stand-by。
Sterilizing: the test tube used by antibacterial experiment, culture dish, graduated cylinder, liquid-transfering gun rifle head, bacteria culture media, agar culture medium has to pass through high pressure steam sterilization before use and processes。Concrete operations are: wrapped by glass drying oven newspaper, bottleneck is encased after sealing by culture medium silica gel plug with newspaper, it is placed in high pressure steam sterilization sterilizing 1h, after sterilizing completes, all vessel are put on clean operating board, and A, B, C, D film card punch prepared by the present embodiment 1 gets the circle of diameter 5mm, open ultraviolet lamp sterilization 20min in the lump。
The cultivation of bacterium solution: preserve from the antibacterial in 3-10 generation and take a ring antibacterial strain inclined plane, rule on agar plate, and cultivate 18-24h at 37 DEG C。From flat board, choose typical colony inoculation in the bacteria culture media of 10mL with connecing collarium, after 37 DEG C of shaken cultivation 18-24h, obtain bacteria suspension。In the bacteria suspension prepared, clump count is bigger, it is necessary to controlled by the clump count in bacteria suspension at the identical order of magnitude, to ensure that bacterial concentration is certain。
Coated plate: draw the 50 μ L bacterium solution (concentration of bacterium solution: 1 × 10 with liquid-transfering gun8～5 × 108Cfu/ml), and with spreading rod it is uniformly coated on agar culture medium。Sample is placed: with alcohol burner flame envelope calcination tweezers, is cooled to after room temperature until tweezers, materialses (each sample repeats 3 times) with tweezers, and it is placed on gently in culture medium and makes sample be close to culture medium。
Antibacterial culturing: the culture dish placing sample is put in water proof constant incubator, 18-24h is cultivated under 37 ± 2 DEG C of conditions, measure inhibition zone width: measure antibacterial circle diameter with ruler, different directions is surveyed four times, averaging the antibacterial circle diameter as sample, preservative film antibacterial effect is as shown in table 1。
Table 1 preservative film is to staphylococcus aureus and colibacillary inhibition
From the data of table 1 it can be seen that work as A film to add nano-TiO2Time, there is certain fungistatic effect, but be not as obvious；When B film solely adds plant extract, fungistatic effect is clearly；But add plant extraction liquid and nano-TiO not as good as the PVA of C film simultaneously2, its inhibition zone is significantly greater than single plus nano TiO2Or inhibition zone during extract, this is main probably due to the effective active composition that nanoparticle can give extract provides free electron so that it is bacteriostasis property increases；And D film (pure PVA) is substantially free of inhibition zone, illustrate that it does not have fungistatic effect。
Embodiment 2
(1) 15g polyvinyl alcohol (088-20) is joined in 85g deionized water, stand 12h so that it is fully swelling。1h is stirred with the speed of 200 revs/min at the temperature of 95 DEG C, polyvinyl alcohol is completely dissolved, prepared concentration is the poly-vinyl alcohol solution of 15wt%, and in 45 DEG C, add the boric acid solution 5ml of 0.5wt% under stirring (200rpm), the hydrochloric acid 2ml and glycerol 1.2g of 4mol/L is added after stirring 0.5h, continue insulated and stirred 1h, obtain solution I；
(2) 10mg/ml nano-TiO is taken2Solution 3mL, adds in the solution I that step (1) prepares, and continues at 45 DEG C of stirring 30min to being uniformly dispersed, obtains solution II；
(3) take the Eupatorium cannabinum L. (Eupatorium coelestinum L.) ethanol extraction 5g of 60mg/ml, add 0.5g Tween 80, at room temperature with the speed stirring and emulsifying of 200 revs/min, obtain solution III；
(4) treat that solution II is cooled to room temperature, stir with the speed of 500 revs/min, in solution II, be slowly added dropwise solution III, stir 0.5h, 120W, the ultrasonic deaeration 1h of 40000Hz, stand 24h deaeration, obtain solution IV；
(5) on a clean plate glass, pour appropriate solution IV, casting film-forming into, dry under natural conditions, take film, be stored in exsiccator。
With cherry tomato, Fructus Jujubae and Capsicum frutescens L．Var．1o m Bail for by Perserving materials, prepared natural complex fresh-keeping film being made freshness protection package, simultaneously with commercially available PE preservative film for matched group, fresh-retaining preserving 7 days in 25 DEG C of environment, see its weight-loss ratio and healthy fruit。Its weight-loss ratio computing formula is:
Weight-loss ratio=(m0-mi)/m0×100
Wherein, m0For preserving the quality of front fruit, unit is g；
miThe quality of fruit when preserving i-th day, unit is g；
Its healthy fruit computing formula is:
Healthy fruit=(total fruit number-corruption fruit number)/total fruit number × 100
In preservation process, fruit is without scab, without rotting, do not have deliquescing fruit as well。Preservative film is to the fresh-keeping effect of sample as depicted in figs. 1 and 2。
Can be seen that from the weight-loss ratio of Fig. 1 the weight-loss ratio of test sample is nearly identical to commercially available PE preservative film by the PVA natural complex fresh-keeping film of the present invention, illustrate that PVA natural complex fresh-keeping film has the effect preventing fruit and vegerable moisture from evaporating；And Fig. 2 finds out, the healthy fruit of PVA natural complex fresh-keeping film is substantially better than PE preservative film, has two reasons, and one is nano-TiO in PVA composite membrane2Forming micropore along with film after solidifying in film, the property of can select that passes through the gas that some diameters are less。When fresh-keeping storage, main selection, through being unfavorable for the gas that fruit and vegerable store, leaves the gas being conducive to fruit and vegerable to store, to regulate CO in packaging bag simultaneously2And O2Volume ratio, it is suppressed that the Repiration of fruit and vegerable, making fruit and vegerable be in a kind of low consumption state, reducing the consumption of fruit vegetable nutrient material, thus reaching fresh-keeping purpose。Two be antipathogenic composition in PVA composite membrane when sample dress stores fruit and vegerable by effects such as the slow releasing of antibiotic substance and photocatalysis, thus killing periphery antibacterial or fungus reaches fresh-keeping effect。
Embodiment 3
(1) 10g polyvinyl alcohol is joined in 90g deionized water, stand 12h so that it is fully swelling。1h is stirred with the speed of 200 revs/min at the temperature of 95 DEG C, polyvinyl alcohol is completely dissolved, prepared concentration is the poly-vinyl alcohol solution of 10wt%, and in 30 DEG C, under stirring (200rpm), add the boric acid solution 5ml of 0.5wt%, the hydrochloric acid 2ml and glycerol 1.2g of 4mol/L is added after stirring 0.5h, continue insulated and stirred 1h, obtain solution I；
(2) nano-TiO is taken2(10mg/ml) solution 3mL, adds in the solution I that step (1) prepares, stirs 30min in 30 DEG C, obtain solution II；
(3) take the Eupatorium cannabinum L. (Eupatorium coelestinum L.) ethanol extraction 10g that concentration is 60mg/ml, add 1.0g Tween 80, at room temperature with the speed stirring and emulsifying of 200 revs/min, obtain solution III；
(4) treat that solution II is cooled to room temperature, stir with the speed of 500 revs/min, in solution II, be slowly added dropwise solution III, stir 0.5h, 120W, the ultrasonic deaeration 1h of 40000Hz, stand 24h deaeration, obtain solution IV；
(5) on a clean plate glass, pour appropriate solution IV, casting film-forming into, dry under natural conditions, obtain 10%PVA natural complex fresh-keeping film, be stored in exsiccator。
(6) use above same procedure, change the concentration of PVA, respectively obtain 5%PVA natural complex fresh-keeping film and 15%PVA natural complex fresh-keeping film。
In order to explore the preservative film of the embodiment 3 preparation good mechanical property in application, the PVA laminated film of preparation having been carried out hot strength test, made film, with the consistency of thickness of PE film (commercially available) when, sets following method of testing:
Testing program: the measure and calculation standard of thin film and thin slice tensile property: GB/T1040.3-2006
Specimen shape: sheet material
Test speed: 100mm/min
Specimen width: 10mm
Sample thickness: 0.45mm
Original gauge length: 100mm
From the figure 3, it may be seen that compared to PE film, PVA series thin film has better hot strength；And along with the increase of PVA concentration has enhancing by a small margin, this series composite membrane has the hot strength of more than 40MPa, intensity meets the needs as preservative film, and can make up the mechanical property defect that PE preservative film runs in life is daily。
Above-described embodiment is the present invention preferably embodiment; but embodiments of the present invention are also not restricted to the described embodiments; the change made under other any spirit without departing from the present invention and principle, modification, replacement, combination, simplification; all should be the substitute mode of equivalence, be included within protection scope of the present invention。

Claims (10)

1. the preparation method of an Extracts from Plant Recourses antimicrobial preservative film, it is characterised in that comprise the steps:
(1) polyvinyl alcohol is joined in deionized water, stand fully swelling to polyvinyl alcohol；Then stir under 80～95 DEG C of conditions and be completely dissolved to polyvinyl alcohol, obtain the poly-vinyl alcohol solution that concentration is 5～15wt%；In 30～45 DEG C, add, toward poly-vinyl alcohol solution, the boric acid solution that concentration is mass percent 5% under stirring, add hydrochloric acid solution and glycerol that concentration is 4mol/L after stirring reaction, continue at 30～45 DEG C of stirrings, obtain solution I；Concentration is the consumption of the boric acid solution of mass percent 5% is every 5～15g polyvinyl alcohol proportioning 3～5ml boric acid solution；Concentration is the consumption of the hydrochloric acid solution of 4mol/L is every 5～15g polyvinyl alcohol proportioning 2ml hydrochloric acid solution；The consumption of glycerol is every 5～15g polyvinyl alcohol proportioning 1～1.2g glycerol；
(2) nanometer titanium dioxide titanium solution is joined in solution I, in 30～45 DEG C of stirrings to being uniformly dispersed, obtain solution II；The consumption of nano titanium oxide is every 5～15g polyvinyl alcohol proportioning 0.01～0.03g nano titanium oxide；
(3) Eupatorium cannabinum L. (Eupatorium coelestinum L.) ethanol extraction and Tween 80 5～10:1～2 proportioning in mass ratio that concentration is 60mg/ml are mixed, stir to emulsifying uniform, obtain solution III；
(4) temperature treating solution II is 20～30 DEG C, drips solution III, stir in the solution II being under stirring, ultrasonic, stands, obtains solution IV；Effect that is ultrasonic and that stand is deaeration；The consumption of the solution III of solution II sum calculates by the Eupatorium cannabinum L. (Eupatorium coelestinum L.) ethanol extraction that every 5～15g polyvinyl alcohol proportioning 5～10g concentration is 60mg/ml；
(5) on clean flat board, pour solution IV, casting film-forming into, dry under natural conditions, obtain Extracts from Plant Recourses antimicrobial preservative film。
2. the preparation method of Extracts from Plant Recourses antimicrobial preservative film according to claim 1, it is characterised in that: the Eupatorium cannabinum L. (Eupatorium coelestinum L.) ethanol extraction described in step (2) prepares as follows: dried Eupatorium cannabinum L. (Eupatorium coelestinum L.) is pulverized, sieved；The Eupatorium cannabinum L. (Eupatorium coelestinum L.) powder dehydrated alcohol obtained or alcohol solution dipping extract, and filter, and concentration obtains purple stem boneset extract。
3. the preparation method of Extracts from Plant Recourses antimicrobial preservative film according to claim 2, it is characterised in that: described sieve is 40～100 mesh sieves；
Described alcoholic solution is the alcoholic solution of percent by volume 90～99.9%；
The condition of described extraction is extract 24h in 25～50 DEG C；
The number of times of described extraction is 1～3 time。
4. the preparation method of Extracts from Plant Recourses antimicrobial preservative film according to claim 1, it is characterised in that:
The time of the standing described in step (1) is 12h；
Stirring described in step (1) be completely dissolved to polyvinyl alcohol in stirring condition be 200rpm stir 1h；
The speed of the stirring described in step (1) is 200rpm；
The time of the stirring reaction described in step (1) is 0.5h；
The time continuing at 30～45 DEG C of stirrings described in step (1) is 1h。
5. the preparation method of Extracts from Plant Recourses antimicrobial preservative film according to claim 1, it is characterised in that: the concentration of the nanometer titanium dioxide titanium solution described in step (2) is 10mg/ml。
6. the preparation method of Extracts from Plant Recourses antimicrobial preservative film according to claim 1, it is characterised in that: the time of the stirring described in step (2) is 0.5h；
The speed of the stirring described in step (2) and (3) is 200rpm。
7. the preparation method of Extracts from Plant Recourses antimicrobial preservative film according to claim 1, it is characterised in that: the speed of the stirring described in step (4) is 500rpm；
The time stirred described in step (4) is 0.5h；
Ultrasonic condition described in step (4) is the ultrasonic 1h of 120W, 40000Hz；
The time of the standing described in step (4) is 24h。
8. the preparation method of Extracts from Plant Recourses antimicrobial preservative film according to claim 1, it is characterised in that: the flat board described in step (5) is glass plate。
9. an Extracts from Plant Recourses antimicrobial preservative film, it is characterised in that: obtained by the preparation method described in any one of claim 1～8。
10. the application in packaging for foodstuff of the Extracts from Plant Recourses antimicrobial preservative film described in claim 9。
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CN106212449A (en) * 2016-07-11 2016-12-14 董晓 A kind of preparation method of plant source slow-release bactericide
CN106400310A (en) * 2016-08-30 2017-02-15 华南农业大学 Nano-fiber anti-microbial fruit-vegetable preservative film with porous structure, and preparation method and application
CN106751270A (en) * 2016-12-14 2017-05-31 陈强 A kind of tear-resistant polyvinyl alcohol preserving fruit and vegetable utilizing film and preparation method thereof
CN107141501A (en) * 2017-04-27 2017-09-08 上海交通大学 The preparation method of degradable water resistance nano antibacterial film
CN108384092A (en) * 2018-02-27 2018-08-10 合肥帧讯低温科技有限公司 Safe, antibacterial and environment-friendly fruit and vegetable preservative film and preparation method thereof
EP3428222A4 (en) * 2017-05-02 2019-05-15 Shanghai Ocean University Method for use in preparing intelligent chromogenic antibacterial anti-oxidation protective film
CN111057336A (en) * 2019-12-30 2020-04-24 武汉轻工大学 Composite film for food and preparation method thereof

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106212449A (en) * 2016-07-11 2016-12-14 董晓 A kind of preparation method of plant source slow-release bactericide
CN106400310A (en) * 2016-08-30 2017-02-15 华南农业大学 Nano-fiber anti-microbial fruit-vegetable preservative film with porous structure, and preparation method and application
CN106751270A (en) * 2016-12-14 2017-05-31 陈强 A kind of tear-resistant polyvinyl alcohol preserving fruit and vegetable utilizing film and preparation method thereof
CN107141501A (en) * 2017-04-27 2017-09-08 上海交通大学 The preparation method of degradable water resistance nano antibacterial film
CN107141501B (en) * 2017-04-27 2020-06-12 上海交通大学 Preparation method of degradable water-resistant nano antibacterial film
EP3428222A4 (en) * 2017-05-02 2019-05-15 Shanghai Ocean University Method for use in preparing intelligent chromogenic antibacterial anti-oxidation protective film
CN108384092A (en) * 2018-02-27 2018-08-10 合肥帧讯低温科技有限公司 Safe, antibacterial and environment-friendly fruit and vegetable preservative film and preparation method thereof
CN111057336A (en) * 2019-12-30 2020-04-24 武汉轻工大学 Composite film for food and preparation method thereof
CN111057336B (en) * 2019-12-30 2023-02-03 武汉轻工大学 Composite film for food and preparation method thereof

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