CN106868708A - A kind of beta cyclodextrin/Pluronic F-127 antibacterial film and preparation method and purposes - Google Patents
A kind of beta cyclodextrin/Pluronic F-127 antibacterial film and preparation method and purposes Download PDFInfo
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- CN106868708A CN106868708A CN201710082618.0A CN201710082618A CN106868708A CN 106868708 A CN106868708 A CN 106868708A CN 201710082618 A CN201710082618 A CN 201710082618A CN 106868708 A CN106868708 A CN 106868708A
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- pluronic
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- schardinger dextrin
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
-
- 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
- B65D81/00—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents
- B65D81/24—Adaptations for preventing deterioration or decay of contents; Applications to the container or packaging material of food preservatives, fungicides, pesticides or animal repellants
- B65D81/28—Applications of food preservatives, fungicides, pesticides or animal repellants
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
- D06M10/025—Corona discharge or low temperature plasma
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Food Science & Technology (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Mechanical Engineering (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention belongs to food fresh keeping packaging material field, and in particular to a kind of beta cyclodextrin/Pluronic F-127 antibacterial film and preparation method and purposes.10min is stirred in hot water by the way that beta cyclodextrin is dissolved in, then adds Pluronic F-127 to be made electrostatic spinning liquid wherein, electrospun fibers film is made by the method for electrostatic spinning, then tunica fibrosa processed by cold plasma and obtains nanofiber antibacterial film.The present invention is simple to operate, and electrostatic spinning and cold plasma treatment technology are all more ripe, and antibacterial film application is wider, there is good market value.
Description
Technical field
The invention belongs to food anti-bacterial refreshing field, and in particular to a kind of beta-schardinger dextrin/Pluronic F-127 antibacterial film and system
Preparation Method and purposes.
Background technology
Cyclodextrin (Cyclodextrin) is starch in the case where no hydrone is participated in, and is turned through cyclodextrin glucose base
A series of general name of cyclic oligomers obtained from enzymatic degradation is moved, 6~12 D- glucopyranose units are usually contained.Its
It is middle to study more and with important practical usage be, containing 6,7,8 molecules of glucose unit, to be referred to as α-ring
Dextrin, beta-schardinger dextrin and gamma-cyclodextrin.Because alpha-cyclodextrin molecule cavity hole is smaller, range of application is smaller；Gamma-cyclodextrin
Molecule cavity it is big, but its production cost is high, industrially can not largely produce, and its application is restricted；The molecule of beta-schardinger dextrin
Cavity is moderate, has a wide range of application, low production cost, is industrially to use most cyclodextrin products at present.Cyclodextrin simultaneously because
Its Bc, biodegradability and it is pollution-free the features such as have use value very high.
Electrostatic spinning is the dropping liquid for applying high voltage at capillary, and then dropping liquid is powered, when electrostatic repulsion counteracts table
Face tension force, so as to stretch drop on surface into silk.Electrostatic spinning be can continuously prepare nanofiber at present and mode of operation compared with
Gentle mode, its nano fibrous membrane for preparing has the packaging effects high of big specific surface area, nanoscale hole and reactive compound
The advantages of.Spin solvent is also a lot, such as Pluronic F-127, polyvinyl alcohol and polycaprolactone.It is quiet with the development of nanometer technology
Electrospun as a kind of New Processing of simple and effective produced nanofiber, will bio-medical material, filtering and
Play a great role in the fields such as protection, catalysis, the energy, photoelectricity, food engineering, cosmetics.
There are many patent applications on electrostatic spinning the country.Chinese patent CN105297286A discloses a kind of feature
The preparation method of poly- methyl e pioic acid methyl ester, cyclodextrin and carbon nano tube composite nanofiber membrane；Chinese patent CN105220362A
Disclose a kind of beta-schardinger dextrin based nano-fiber film and preparation method thereof and the application in Dye Adsorption, separation；It is Chinese special
Sharp CN102926029A discloses a kind of electrostatic spinning and prepares the method that nanometer nitrifies beta-schardinger dextrin fiber.
The concept of plasma was suggested first in nineteen twenty-eight, and pointed out that plasma is the collection of approximate electroneutral
Zoarium, is made up of ion with electronic population, and electric field and magnetic field can be responded.Plasma technique is to apply plasma
The partially ionized plasma that body generator is produced completes the means of certain industrial production target.Surface plasma light in 2008
Catalysis is also formally suggested, and this series of proof all show superperformance of the surface plasma in photocatalysis.Utilize
The high temperature of plasma or active particle therein facilitate some to chemically react with radiation, are more popular to obtain new material
Study hotspot.
Beta-schardinger dextrin nano fibrous membrane is combined with cold plasma, facilitates tunica fibrosa to there occurs change, so as to prepare
The antibacterial film with antimicrobial effect is obtained, with preferable application prospect and market value.
The content of the invention
Beta-schardinger dextrin/Pluronic F-127 antibacterial film and preparation it is an object of the invention to provide a kind for the treatment of of cold plasma
Method and purposes, are stirred by the way that beta-schardinger dextrin is dissolved in hot water, and add Pluronic F-127 to prepare electrostatic spinning solution,
Ultrasound degassing obtains spinning precursor solution after normal temperature magnetic stirrer over night.Syringe draws spinning precursor solution and carries out electrostatic
Spinning, nano fibrous membrane is obtained using flat panel collector method, and nanofiber antibacterial film is obtained after being processed through cold plasma.
The present invention is made nanofiber antibacterial film by beta-schardinger dextrin, Pluronic F-127, can be used for food fresh keeping.
The preparation method of nanofiber antibacterial film, comprises the following steps：
(1) preparation method of nano fibrous membrane：Beta-schardinger dextrin is slowly added to heated at constant temperature in 65 DEG C of deionized water
Pluronic F-127 is added to prepare Pluronic F-127 electrostatic spinning liquid after once stirring, overnight rear ultrasound deaerates stirring at normal temperature
To spinning precursor solution, syringe draws spinning precursor solution and carries out electrostatic spinning, is received using flat panel collector legal system
Rice tunica fibrosa, beta-schardinger dextrin/Pluronic F-127 antibacterial film is obtained by sterilizing, cold plasma treatment；Spinning-aid agent polycyclic oxygen second
Alkene, interacts with beta-schardinger dextrin in spinning and cold plasma processing procedure and produces antimicrobial effect.
The time of the first time stirring is 10min；Ultrasonic degassing time is 30min.
The electrostatic spinning voltage is 5kV-30kV, and propulsion speed is 0.1-3mL/h, and it is 10-20cm, air to receive distance
Humid control is below 35%.
The mass ratio of the Pluronic F-127, beta-schardinger dextrin and deionized water is：6：9：100.
Described flat panel collector method is to receive tunica fibrosa, respectively masking foil and brown paper using two kinds of materials, after 3h
Obtain nano fibrous membrane.
The sterilizing refers to and is positioned over sterilization treatment 2h under uviol lamp.
Using nitrogen protection, nitrogen flow is 100sccm for cold plasma treatment, cold plasma process time is 4~
5min, processing power is 400~500W.
Brief description of the drawings
Fig. 1 Pluronic F-127s tunica fibrosa and beta-schardinger dextrin nano fibrous membrane.
The anti-Escherichia coli figure of Fig. 2 beta-schardinger dextrin nanofiber antibacterial films.Note：PEO:Pluronic F-127；NM：Nanofiber
Film；β-CD：Beta-schardinger dextrin；Plasma:Cold plasma；PVA：Polyvinyl alcohol.
Beta-schardinger dextrin nanofiber antibacterial film anti-Staphylococcus aureus figure on Fig. 3 masking foils；Note：PEO:Polycyclic oxygen second
Alkene；NM：Nano fibrous membrane；β-CD：Beta-schardinger dextrin；Plasma:Cold plasma.
Beta-schardinger dextrin nanofiber antibacterial film anti-Staphylococcus aureus figure on Fig. 4 brown paper；Note：PEO:Polycyclic oxygen second
Alkene；NM：Nano fibrous membrane；β-CD：Beta-schardinger dextrin；Plasma:Cold plasma.
Specific embodiment
Specific embodiment of the invention, but protection content of the invention are illustrated by Examples below, this is not only limited to.
The sign of 1 beta-schardinger dextrin of embodiment/Pluronic F-127 nano fibrous membrane
1 experiment material
Beta-schardinger dextrin BR Chemical Reagent Co., Ltd., Sinopharm Group
Pluronic F-127 SIGMA-ALDRICH
2 experimental techniques
1) preparation of beta-schardinger dextrin/Pluronic F-127 nano fibrous membrane
In the deionized water of the beta-schardinger dextrin for 1. weighing 900mg be slowly added into 10mL 65 DEG C, heated at constant temperature stirring
10min。
2. the Pluronic F-127 for weighing 600mg is slowly added into above-mentioned solution, stirring at normal temperature ultrasonic degassing after overnight
The Pluronic F-127 spinning precursor solution of 6% (W/W) is obtained after 30min.
3. syringe draws 5mL spinning precursor solutions and assembles and start spinning, and electrostatic spinning voltage is 18kV, propulsion
Speed is 0.5mL/h, and it is 15.5cm to receive distance, and air humidity is controlled below 35%, using flat panel collector method, using two kinds
Material receives tunica fibrosa, respectively masking foil and brown paper, and nano fibrous membrane is obtained after 3h.
4. by above step can prepare spinning-aid agent be polyvinyl alcohol beta-schardinger dextrin nano fibrous membrane, by step 2. in
The Pluronic F-127 of 600mg is changed to the polyvinyl alcohol of 1000mg, that is, weigh 1000mg polyvinyl alcohol be slowly added to the β of 10mL-
In cyclodextrin aqueous solution, stirring at normal temperature obtains the polyvinyl alcohol spinning presoma of 10% (W/W) after ultrasonic degassing 30min after overnight
Solution, spinning can obtain beta-schardinger dextrin/polyvinyl alcohol nanofiber membrane.
2) SEM observations electrospun fibers film
Use the form of JSM-7001F scanning electronic microscope examination nano fibrous membranes.Au/Pd mixtures are used under vacuo
Different samples are sputtered, and all of SEM experiments are carried out under 30kV.
3) SEM experimental results
Scanning electron microscope (SEM) photograph as shown in figure 1, with the addition of the nano fibrous membrane of beta-schardinger dextrin diameter increase, show beta-schardinger dextrin
Wrapped up wherein well, and with good ropiness.
The measure of 2 beta-schardinger dextrins of embodiment/Pluronic F-127 antibacterial film bacteriostasis property
1 experiment material
Masking foil：Pluronic F-127 tunica fibrosa-cold plasma, beta-schardinger dextrin/Pluronic F-127 tunica fibrosa, β-ring paste
Essence/Pluronic F-127 tunica fibrosa-cold plasma, beta-schardinger dextrin/polyethylene glycol fiber films-cold plasma
Strain：Escherichia coli
2 experimental techniques
1) bacterium solution is prepared
Inoculation Escherichia coli shaken cultivation 24h in ordinary nutritional broth bouillon (NB), 37 DEG C of shaking tables, obtains logarithm life
Long-term bacteria suspension.Take appropriate Escherichia coli 0 times of ladder of 0.03mol/L phosphate buffer 1s in growth logarithmic phase saturation
1000 times (about 10 of degree dilution5cfu/mL)。
2) electrospun fibers film process
Prepared according to embodiment 1 Pluronic F-127 tunica fibrosa on masking foil, beta-schardinger dextrin/Pluronic F-127 tunica fibrosa and
Beta-schardinger dextrin/polyethylene glycol fiber films are in oven drying 4h.Film is cut into the specification of 2cm × 2cm and is positioned under uviol lamp and is gone out
Bacterium processes 2h with standby.
3) the method for plate culture count is determined
Three kinds of tunica fibrosas after by sterilizing process 4min through cold plasma 500W.15mL phosphorus is added in the centrifuge tube of 50mL
Phthalate buffer sterilization treatment, four kinds of films is respectively placed in and contains Escherichia coli (about 105Cfu/mL phosphate buffer)
In, centrifuge tube is placed in air table the concussion reaction under conditions of 37 DEG C.Determined using the method for plate culture count, existed respectively
Appropriate nutrient solution is taken when 4h, 8h, 16h and 24h carries out ten times of gradient dilutions to suitable concentration, then pipettes 100 μ L dilutions
Drip on solid medium, inversion culture in 37 DEG C of constant temperature and humidity incubators is put into after coating is uniform.Flat board bacterium is carried out after 48h
Fall to counting, so as to the antibacterial activity to antibacterial film is evaluated.Experiment is triplicate, results averaged.
4) experimental result
As shown in Figure 2, during spinning and cold plasma, beta-schardinger dextrin there occurs certain with Pluronic F-127
Change, makes the nano fibrous membrane that it is prepared by there is certain anti-microbial property after cold plasma.
The measure of the beta-schardinger dextrin nanofiber antibacterial film bacteriostasis property of embodiment 3
1 experiment material
Masking foil：Beta-schardinger dextrin/Pluronic F-127 tunica fibrosa, beta-schardinger dextrin/Pluronic F-127 tunica fibrosa-cold plasma
Brown paper：Beta-schardinger dextrin/Pluronic F-127 tunica fibrosa, beta-schardinger dextrin/Pluronic F-127 tunica fibrosa-cold plasma
Strain：Staphylococcus aureus
2 experimental techniques
1) bacterium solution is prepared
Inoculation staphylococcus aureus shaken cultivation 48h in ordinary nutritional broth bouillon (NB), 37 DEG C of shaking tables, obtains
The bacteria suspension of exponential phase.Take the appropriate staphylococcus aureus 0.03mol/L phosphate in growth logarithmic phase saturation
10 times of buffer solution, 1000 times of gradient dilution (about 105cfu/mL)。
2) electrospun fibers film process
According to embodiment 1 prepare two kinds receive the Pluronic F-127 tunica fibrosa of material masking foil and brown paper, beta-schardinger dextrin/
Pluronic F-127 tunica fibrosa is in oven drying 4h.Film is cut into the specification of 2cm × 2cm and sterilization treatment 2h under uviol lamp is positioned over
With standby.
3) the method for plate culture count is determined
By the Pluronic F-127 tunica fibrosa after sterilizing, beta-schardinger dextrin/Pluronic F-127 tunica fibrosa through cold plasma 500W
Treatment 4min.15mL phosphate buffer sterilization treatments are added in the centrifuge tube of 50mL, by above-mentioned every kind of receive material two kinds
Film is respectively placed in and contains staphylococcus aureus (about 105Cfu/mL in phosphate buffer), centrifuge tube is placed in air and shakes
Bed under conditions of 37 DEG C concussion reaction.Determined using the method for plate culture count, taken in 4h, 8h, 16h and 24h respectively suitable
Amount nutrient solution carries out ten times of gradient dilutions to suitable concentration, then pipettes 100 μ L dilutions and drips on solid medium, is coated with
Inversion culture in 37 DEG C of constant temperature and humidity incubators is put into after uniform.Plate count is carried out after 48h, so as to antibacterial film
Antibacterial activity is evaluated.Experiment is triplicate, results averaged.
4) experimental result
From Fig. 3 and Fig. 4, the beta-schardinger dextrin nanofiber on cold plasma treated masking foil and brown paper resists
Mycoderm has certain antibacterial effect to staphylococcus aureus.
Claims (8)
1. the preparation method of a kind of beta-schardinger dextrin/Pluronic F-127 antibacterial film, it is characterised in that preparation process is as follows：By β-ring paste
Essence is slowly added to add Pluronic F-127 to prepare polycyclic oxygen second after heated at constant temperature is stirred for the first time in 65 DEG C of deionized water
Alkene electrostatic spinning liquid, overnight rear ultrasound degassing obtains spinning precursor solution to stirring at normal temperature, and it is molten that syringe draws spinning presoma
Liquid carries out electrostatic spinning, and nano fibrous membrane is obtained using flat panel collector legal system, and β-ring is obtained by sterilizing, cold plasma treatment
Dextrin/Pluronic F-127 antibacterial film；Spinning-aid agent Pluronic F-127, with beta-schardinger dextrin in spinning and cold plasma processing procedure
Interact and produce antimicrobial effect.
2. the preparation method of a kind of beta-schardinger dextrin/Pluronic F-127 antibacterial film as claimed in claim 1, it is characterised in that：Institute
The time for stating stirring for the first time is 10min；Ultrasonic degassing time is 30min.
3. the preparation method of a kind of beta-schardinger dextrin/Pluronic F-127 antibacterial film as claimed in claim 1, it is characterised in that：Institute
Electrostatic spinning voltage is stated for 5kV-30kV, propulsion speed is 0.1-3mL/h, it is 10-20cm to receive distance, and air humidity control exists
Less than 35%.
4. the preparation method of a kind of beta-schardinger dextrin/Pluronic F-127 antibacterial film as claimed in claim 1, it is characterised in that：Institute
The mass ratio for stating Pluronic F-127, beta-schardinger dextrin and deionized water is：6：9：100.
5. the preparation method of a kind of beta-schardinger dextrin/Pluronic F-127 antibacterial film as claimed in claim 1, it is characterised in that：Institute
The flat panel collector method stated is to receive tunica fibrosa, respectively masking foil and brown paper using two kinds of materials, and Nanowire is obtained after 3h
Dimension film.
6. the preparation method of a kind of beta-schardinger dextrin/Pluronic F-127 antibacterial film as claimed in claim 1, it is characterised in that：Institute
State sterilizing and refer to and be positioned over sterilization treatment 2h under uviol lamp.
7. the preparation method of a kind of beta-schardinger dextrin/Pluronic F-127 antibacterial film as claimed in claim 1, it is characterised in that：It is cold
Corona treatment is protected using nitrogen, and nitrogen flow is 100sccm, and cold plasma process time is 4~5min, processes work(
Rate is 400~500W.
8. beta-schardinger dextrin/Pluronic F-127 antibacterial film that prepared by the method as described in claim 1-7 is any is in food fresh keeping
Purposes.
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Cited By (4)
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| CN109675450A (en) * | 2018-12-26 | 2019-04-26 | 中国科学院深圳先进技术研究院 | A kind of antibacterial composite nano-fiber membrane and its preparation method and application |
| CN112300425A (en) * | 2020-11-17 | 2021-02-02 | 上海海洋大学 | Gelatin/fiber composite antibacterial film and preparation method and application thereof |
| CN112391696A (en) * | 2020-08-24 | 2021-02-23 | 江苏大学 | Dill essential oil/pleurotus eryngii polysaccharide antibacterial nanofiber as well as preparation method and application thereof |
| CN112391697A (en) * | 2020-08-24 | 2021-02-23 | 江苏大学 | Antibacterial nanofiber containing ilex essential oil/lycium barbarum polysaccharide and preparation method and application of antibacterial nanofiber |
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| CN109675450A (en) * | 2018-12-26 | 2019-04-26 | 中国科学院深圳先进技术研究院 | A kind of antibacterial composite nano-fiber membrane and its preparation method and application |
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| CN112391696A (en) * | 2020-08-24 | 2021-02-23 | 江苏大学 | Dill essential oil/pleurotus eryngii polysaccharide antibacterial nanofiber as well as preparation method and application thereof |
| CN112391697A (en) * | 2020-08-24 | 2021-02-23 | 江苏大学 | Antibacterial nanofiber containing ilex essential oil/lycium barbarum polysaccharide and preparation method and application of antibacterial nanofiber |
| CN112391696B (en) * | 2020-08-24 | 2023-03-21 | 江苏大学 | Dill essential oil/pleurotus eryngii polysaccharide antibacterial nanofiber as well as preparation method and application thereof |
| CN112391697B (en) * | 2020-08-24 | 2023-03-21 | 江苏大学 | Antibacterial nanofiber containing ilex essential oil/lycium barbarum polysaccharide and preparation method and application of antibacterial nanofiber |
| CN112300425A (en) * | 2020-11-17 | 2021-02-02 | 上海海洋大学 | Gelatin/fiber composite antibacterial film and preparation method and application thereof |
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