CN109082774A - A kind of anti-oxidant nano-fiber composite film and preparation method and application containing Folium Nerviliae fordii extract - Google Patents
A kind of anti-oxidant nano-fiber composite film and preparation method and application containing Folium Nerviliae fordii extract Download PDFInfo
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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
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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Abstract
The invention belongs to nano material and packaging material for food field, it is related specifically to that Folium Nerviliae fordii extract is prepared into Folium Nerviliae fordii extract/polyvinyl alcohol polyethylene pyrrolidones nano-fiber composite film method and its application using electrostatic spinning technique.Include the following steps: to prepare the spinning solution containing Folium Nerviliae fordii extract, polyvinylpyrrolidone and poly-vinyl alcohol solution, then spinning solution is carried out electrostatic spinning, obtain the nano fibrous membrane containing Folium Nerviliae fordii extract by electrostatic spinning apparatus；Spinning voltage is 13-25kV, and the distance of syringe needle to receiver is 12-16cm, and spinning rate is 0.2-0.6mL/h.Present invention process is simple, mild condition, meanwhile, Folium Nerviliae fordii extract is embedded by polymer, enhances the dissolubility of Folium Nerviliae fordii extract；In addition, Folium Nerviliae fordii extract had good sustained release effect, has good inoxidizability, hypotoxicity, has broad application prospects in packaging material for food field.
Description
Technical field
The invention belongs to nano material and packaging material for food field, it is related specifically to utilize electrostatic spinning technique by the blue sky
Certain herbaceous plants with big flowers plant extracts is prepared into a kind of method and its application of anti-oxidant nano-fiber composite film containing Folium Nerviliae fordii extract.
Background technique
Food oxydating resistance active packing is a certain amount of antioxidant to be dispersed in packaging material or coated in material table
Face extends a kind of active packing mode of Food Shelf-life by inhibiting the oxygenolysis of food.Antioxidant is that one kind can
Scavenging activated oxygen suppresses or eliminates and slows down the substance of oxidation reaction.Antioxidant master used in food packaging at present
There are artificial synthetized oxidation preventive agent and natural.Artificial synthesized antioxidant can be obtained by chemically synthesized method
It arrives, mainly has butylated hydroxy anisole (BHA), dibutyl hydroxy toluene (BHT), propylgallate (PG), tertiary butyl to benzene
Diphenol (TBHQ) etc., the effect of these antioxidant inoxidizability is strong, and stability is good, but studies and find that they all have certain poison
Property, which greatly limits its applications.Natural derives from organism (plant, animal, microorganism), mainly
Including Radix Glycyrrhizae, garlic, vitamin C (VC), vitamin E (VE), tea polyphenols, phosphatide, amino acid etc., wherein VCAnd VEIt is relatively common,
But its light-exposed easy decomposition, stability is poor, is subject to certain restrictions its application.From the Natural Antioxidants of plant
(flavonoids, phenolic acid class, polysaccharide) has good in oxidation resistance, highly-safe and advantages of environment protection, in recent years, to contain this
The plant extraction liquid of a little active materials prepares food oxydating resistance Active Packaging Materials and receives the concern of people.
Electrostatic spinning is a kind of simple and widely used technology for preparing polymer nanofiber.Polymer solution is molten
Body overcomes the surface tension and viscous force of itself under high-pressure electrostatic effect, is fallen on receiver board, is formed with high-speed screw movement
The fiber assembly of similar non-woven fabric-like.It is 5-1000nm using nanofiber diameter made from electrostatic spinning, due to polymer
Nanofiber has high specific surface area, big porosity and good mechanical performance, thus in food, weaving, national defence and life
The fields such as object medical material have broad application prospects.
Ford nervilia leaf (Nervilia fordii) also known as sole leaf lotus, clethra loosestrife root or herb etc., are distributed widely in Guangdong, Guangxi, Hainan
Area is the peculiar medicinal material of South China.Ford nervilia leaf contain the various actives such as flavones, steroidal, triterpene, amino acid, volatile oil at
Point, the substances such as flavonoids therein have good antioxidant activity, however so far, it is related mixed using electrostatic spinning technique
The research that spinning Folium Nerviliae fordii extract prepares anti-oxidant nano-packaging film has not been reported.Although flavonoids, phenol in plant extraction liquid
Acid antioxidant effect is good, but it is insoluble in water, and unstable, and then limits its answering in food packaging applications
With.
Summary of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, the primary purpose of the present invention is that providing a kind of containing ford nervilia leaf
The preparation method of the anti-oxidant nano-fiber composite film of extract.
Another object of the present invention is to provide a kind of anti-oxidant nanometer containing Folium Nerviliae fordii extract prepared by the above method
Composite fiber membrane.
Still a further object of the present invention is to provide the above-mentioned anti-oxidant nano-fiber composite film containing Folium Nerviliae fordii extract in food
The application in packaging material field.
The purpose of the present invention is realized by following proposal:
A kind of preparation method of the nano-fiber composite film containing Folium Nerviliae fordii extract, includes the following steps:
It is molten that Folium Nerviliae fordii extract, polyvinylpyrrolidone (PVP) and poly-vinyl alcohol solution (PVA) are mixed and made into spinning
Then spinning solution is carried out electrostatic spinning, obtains the nanofiber containing Folium Nerviliae fordii extract by liquid by electrostatic spinning apparatus
Film；Wherein spinning voltage is 13-25kV, and the distance of syringe needle to receiver is 12-16cm, and spinning rate is 0.2-0.6mL/h.
The spinning solution the preparation method comprises the following steps: by polyvinyl alcohol it is soluble in water obtain quality volume fraction be 5%-10%
Poly-vinyl alcohol solution；Polyvinylpyrrolidone is dissolved in 90% ethanol solution, obtaining quality volume fraction is 9%-19%'s
Then Folium Nerviliae fordii extract is added in polyvinylpyrrolidonesolution solution；Again by the polyvinylpyrrolidone containing Folium Nerviliae fordii extract
Solution is added in poly-vinyl alcohol solution；The volume ratio of poly-vinyl alcohol solution and polyvinylpyrrolidonesolution solution is 1:1-2:1, institute
The concentration for obtaining Folium Nerviliae fordii extract in mixed solution is 3.5-4.5mg/mL.
Preferably, the quality volume fraction of added polyvinylpyrrolidonesolution solution is 15% in the spinning solution, institute
The quality volume fraction for adding poly-vinyl alcohol solution is 10%, the volume ratio of poly-vinyl alcohol solution and polyvinylpyrrolidonesolution solution
For 1:1, the concentration of Folium Nerviliae fordii extract is 4mg/mL in spinning mixed solution.
The Folium Nerviliae fordii extract the preparation method comprises the following steps:
(1) ford nervilia leaf is crushed, is extracted with organic solvent；
(2) by step (1) the extraction product pass sequentially through petroleum ether, ethyl acetate extract or pass sequentially through petroleum ether,
Ethyl acetate, extracting n-butyl alcohol, every phase extract 3-5 times, each 3-5h, obtain Folium Nerviliae fordii extract.
Step (1) organic solvent is one of ethyl alcohol, methanol or acetone or a variety of, volume fraction 40%-
95%, solid-liquid ratio 1:5-1:20, it is described to be extracted as reflux extraction, intensified by ultrasonic wave extraction, in microwave-assisted extraction
It is one or more, number be 1-3 time, each 1-3h, Extracting temperature be 50 DEG C -90 DEG C.
Preferably, step (1) ford nervilia leaf is ford nervilia leaf, and organic solvent is the ethyl alcohol of volume fraction 56%, is extracted
Temperature is 75 DEG C, solid-liquid ratio 1:14；Extraction time is 2 times, each 2h.
The step (2) is that step (1) described Folium Nerviliae fordii extract is passed sequentially through to petroleum ether, ethyl acetate extraction, often
Mutually extraction 4 times, each 4h.
The spinning voltage is 15kV, and the distance of syringe needle to receiver is 14cm, and spinning rate is 0.3mL/h.
A kind of anti-oxidant nano-fiber composite film containing Folium Nerviliae fordii extract prepared according to the above method.
The application of the anti-oxidant nano-fiber composite film in anti-oxidant packaging material containing Folium Nerviliae fordii extract.
The temperature of room temperature of the present invention is 30-35 DEG C, and the temperature of room temperature is 28-35 DEG C.
The PVP that the present invention uses is amphiphilic species, is on the one hand embedded to embedding Folium Nerviliae fordii extract, on the other hand
The characteristics of improving Folium Nerviliae fordii extract poorly water-soluble.Secondly substrate PVA and PVP has good biocompatibility, utilizes this
The characteristics of substrate embedding Folium Nerviliae fordii extract improves its poorly water-soluble, and food packaging applications can be applied to.
The present invention compared with the existing technology, have the following advantages and the utility model has the advantages that
(1) using electrostatic spinning technique natural anti-oxidation Nanowire is made in polymer, plant extracts cospinning by the present invention
Film is tieed up, the application range of electrostatic spinning technique has been expanded.
(2) the applicable substrate of the present invention has good biocompatibility, and added ford nervilia leaf is natural extract, green peace
Entirely, and the composite membrane can finally degrade, and environmental pollution is small.
(3) present invention process is simple, mild condition, easy to operate, meanwhile, Flavonoid substances are wrapped by polymer
It buries, enhances the stability of Flavonoid substances；In addition, prepared nano fibrous membrane flavones had good sustained release effect, has good
Inoxidizability.
(4) nano-fiber composite film prepared by the present invention has preferable inoxidizability, hypotoxicity, so in food packaging
Material Field has broad application prospects.
Detailed description of the invention
Fig. 1 be the different volume fraction of ethanol (a) of embodiment 1, different Extracting temperatures (b), different feed liquid ratio (c) DPPH from
By base clearance rate figure.
Fig. 2 is the DPPH free radical scavenging activity figure at the different extraction positions of embodiment 2.
Fig. 3 is the lipid determination oxidative result figure of embodiment 5.
Fig. 4 is the reducing power measurement result figure of embodiment 6.
Fig. 5 is 7 nano-fiber composite film scanning electron microscope (SEM) photograph of embodiment.
Fig. 6 is 8 nano-fiber composite film scanning electron microscope (SEM) photograph of embodiment.
Fig. 7 (a) is embodiment 9, (b) is embodiment 10, (c) is the nano-fiber composite film scanning electron microscope of embodiment 11
Figure.
Fig. 8 is DPPH free radical scavenging activity figure of the embodiment 12 in different dissolution mediums.
Fig. 9 is the determination of total flavonoids figure in different dissolution mediums of embodiment 12.
Figure 10 is 13 infrared absorpting light spectra of embodiment.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Agents useful for same can routinely be bought unless otherwise specified from market in embodiment.
Embodiment 1
The optimization of ford nervilia leaf extraction conditions, the specific steps are as follows:
(1) it chooses different conditions and extracts ford nervilia leaf
20g ford nervilia leaf powder is dissolved in 40%, 60%, 80%, 95% ethanol solution, by solid-liquid ratio 1:20 at 80 DEG C
It refluxing extraction 2 times, each 2h, is then concentrated by Rotary Evaporators, obtains each alcohol extract；
20g ford nervilia leaf powder is dissolved in 60% ethanol solution, in 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C of Extracting temperatures
Under, by solid-liquid ratio 1:20 refluxing extraction 2 times, each 2h, then it is concentrated by Rotary Evaporators, obtains each alcohol extract；
20g ford nervilia leaf powder is dissolved in 60% ethanol solution, by solid-liquid ratio 1:5,1:10,1:15,1:20 at 70 DEG C
It refluxing extraction 2 times, each 2h, is then concentrated by Rotary Evaporators, obtains each alcohol extract；
(2) each alcohol extract being concentrated to get is determined into its anti-oxidation characteristics by measurement DPPH free radical scavenging activity, had
Body test method:
First centrifuge tube adds 0.4mL sample solution and 3.6mLDPPH ethanol solution (150mM), mixes, is denoted as A1；
Second centrifuge tube adds 0.4mL sample solution and 3.6mL dehydrated alcohol, mixes, is denoted as A2；
Third branch centrifuge tube adds 0.4mL dehydrated alcohol and 3.6mLDPPH ethyl alcohol, mixes, is denoted as A0；
To test A at 517nm1、A2And A3Absorbance be measured.
Clearance rate=(1- (A1-A2)/A0) * 100%
The inoxidizability of extract is shown in Fig. 1 under above-mentioned experiment condition.
(3) ford nervilia leaf extracting method is advanced optimized by response surface experiment, the specific steps are as follows:
Choose different volume fraction of ethanol 55%, 60%, 65%, 65 DEG C of different Extracting temperatures, 70 DEG C, 75 DEG C, difference material
Liquor ratio 1:5,1:10,1:15 Three factors-levels carry out response surface experiment.
(4) experimental result obtained in step (3) is analyzed by BBD software, by comparing DPPH clearance rate
Actual value and predicted value carry out analysis comparison, pass through the conspicuousness to model, the conspicuousness and R of the quasi- item of mistake2It is analyzed, in conjunction with
It is volume fraction of ethanol 56%, 75 DEG C of Extracting temperature, solid-liquid ratio 1:14 that response surface figure, which obtains optimal ford nervilia leaf extraction conditions,.
Embodiment 2
The antioxidant activity for the Folium Nerviliae fordii extract that different extractants obtain is evaluated, specific steps are as follows:
(1) ford nervilia leaf alcohol extract is prepared according to the method in embodiment 1.Specific step is as follows: 20g ford nervilia leaf powder,
It is extracted under the conditions of volume fraction of ethanol 56%, 75 DEG C of temperature, solid-liquid ratio 1:14, is concentrated to give alcohol extract by Rotary Evaporators.
(2) 3 kinds of petroleum ether, ethyl acetate and n-butanol extractants is selected successively to be obtained according to the polar difference of extractant
The Folium Nerviliae fordii extract of opposed polarity.Method particularly includes: the dissolution of 100mL water is added in gained alcohol extract in (1), be then added etc.
The petroleum ether of amount extracts 4h, collects upper layer, and as petroleum ether extraction phase, lower layer's water phase uses 100mL petroleum ether extraction, phase again
It is repeated 3 times, is then mutually concentrated by evaporation all upper layer petroleum ether extractions, this is ligroin extraction with method.Petroleum ether extraction
After taking, lower water is mutually subsequently added into 100mL ethyl acetate and is extracted, and extracts 4h, collects upper layer, and as ethyl acetate extracts
Phase, lower layer's water phase use 100mL ethyl acetate to extract again, and same procedure is repeated 3 times, and then extract all upper layer ethyl acetate
It takes and is mutually concentrated by evaporation, this is ethyl acetate extract.After ethyl acetate has extracted, lower water is mutually subsequently added into 100mL n-butanol
It is extracted, extracts 4h, collect upper layer, as extracting n-butyl alcohol phase, lower layer's water phase uses extracting n-butyl alcohol, same procedure weight again
Multiple 3 times, then all upper layer extracting n-butyl alcohols are mutually concentrated by evaporation, this for n-butanol extract, lower layer are water extract.
(3) four kinds of extracts obtained in step (2) carry out DPPH free radical scavenging activity by the method for embodiment 1
Measurement, replaces sample solution to make mark product with mass concentration by the ascorbic acid solution of 20-200 μ g/mL.
Fig. 2 is the DPPH free radical scavenging activity figure of the different extractants under above-mentioned process conditions, as seen from the figure, anti-oxidant
The optimal extraction position, that is, ethyl acetate extract of effect.
Embodiment 3
The total phenol content measurement of different extraction phases uses forint phenol colorimetric method, the specific steps are as follows:
(1) different Folium Nerviliae fordii extracts are prepared according to the method in embodiment 2.
(2) various concentration (0.1mg/mL, 0.5mg/mL, 1mg/mL, 2mg/mL) for taking 100 μ L to be configured with 70% ethyl alcohol
0.5mL forint phenol reagent and 7.9mL water is added in each extraction phase, is uniformly mixed.It is protected from light 5min, it is rear to be added the 10% of 1.5mL
Na2CO3Solution is protected from light 2h at room temperature after mixing, its absorbance is measured at 765nm.With the gallic acid of various concentration (20,
40,60,80,100 μ g/mL) make mark product, by mark song calculate each extraction phase total phenol content, total phenol under above-mentioned process conditions
Assay the results are shown in Table 1.By comparing discovery, ethyl acetate extract total phenol content highest, i.e. antioxidant effect is best.
The total phenol content measurement result at the different extraction positions of table 1
Embodiment 4
The determination of total flavonoids of different extraction phases uses AlCl3- HAc-NaAc (pH 5.5) method, the specific steps are as follows:
(1) different Folium Nerviliae fordii extracts are prepared according to the method in embodiment 2.
(2) various concentration (0.1mg/mL, 0.5mg/mL, 1mg/mL, 2mg/mL) for taking 200 μ L to be configured with 70% ethyl alcohol
The 0.1mol/L AlCl of 300 μ L is added in each extraction phase3Solution, 200 μ L HAc-NaAc (pH 5.5) buffer solution after use
70% ethyl alcohol is supplied solution and is measured at 405nm to its absorbance at room temperature after mixing to 5mL.Use various concentration
Rutin (5-35 μ g/mL) make mark product, by mark song calculate each extraction phase general flavone content, it is total yellow under above-mentioned process conditions
Ketone assay the results are shown in Table 2.As a result, it has been found that ethyl acetate extract flavones content highest, antioxidant effect are best.
The determination of total flavonoids result at the different extraction positions of table 2
Embodiment 5
The ethyl acetate phase best to antioxidant effect carries out the measurement of lipid peroxidation capacity, use lipovitellinin for
The LPO model reaction system of substrate, the specific steps are as follows:
(1) ethyl acetate extract of ford nervilia leaf is prepared according to the method in embodiment 2.
(2) preparation of yolk liquid: Fresh Egg removes egg white, and yolk is matched with isometric 0.1M phosphate buffer (pH 7.4)
At the suspension of 1:1, magnetic agitation 10min, then be diluted to PBS the yolk suspension of 1:25 is placed in 4 DEG C, spare.
(3) the step of taking 0.2mL (2) solution, it is rear that 0.1mL step (1) resulting ethyl acetate extract and 0.2mL is added
25mM FeSO4Solution is mixed with PBS make-up solution to 2mL, is placed in 37 DEG C of water-bath 1h.After taking-up, it is added 0.5mL's
20% trichloroacetic acid (TCA) solution is centrifuged 10min at 4000rpm after standing 10min.Supernatant 2mL after taking centrifugation, adds
Enter 0.8% thiobarbituricacidα- (TBA) solution of 1mL, takes out and be cooled to room temperature after boiling water bath 15min, measure it at 532nm
Absorbance.Make mark product with ascorbic acid.
Calculation formula inhibiting rate S (%)=((A0-Ax)/A0) * 100%
Wherein AxFor the light absorption value containing ethyl acetate extract, A0For the light absorption value without ethyl acetate extract.
Lipid peroxidation measurement result under above-mentioned process conditions is shown in Fig. 3.
Embodiment 6
The ethyl acetate phase best to antioxidant effect carries out the measurement of reducing power, specific to walk using Prussia's blue laws
It is rapid as follows:
(1) ethyl acetate extract of ford nervilia leaf is prepared according to the method in embodiment 2.
(2) the step of taking 1mL various concentration (0.1-6mg/mL) (1) solution, is added the 0.2M phosphate buffer of 2.5mL
1% potassium ferricyanide solution of (pH 6.6), 2.5mL, in 50 DEG C of water-bath 20min after mixing.It after taking-up, is cooled to room temperature, is added
It is mixed after 10% solution of trichloroacetic acid of 2.5mL, stands 1min and terminate reaction, mixed liquor is centrifuged 10min at 3,000 rpm.
Precision draws 2.5mL supernatant in testing tube, sequentially adds 2.5mL distilled water and 0.1% ferric chloride solution, mixes, room temperature
10min is reacted, measures its absorbance at 700 nm.Make mark product with ascorbic acid.
The reducing power measurement result of ethyl acetate extract is shown in Fig. 4 under above-mentioned process conditions.
Embodiment 7
A kind of preparation method of the anti-oxidant nano-fiber composite film of the ethyl acetate extract containing ford nervilia leaf, specific steps are such as
Under:
(1) ethyl acetate extract of ford nervilia leaf is prepared according to the method in embodiment 2；
(2) 8g polyvinyl alcohol is dissolved in 100mL distilled water, and in 80 DEG C of stirring 2h, obtaining quality volume fraction is 8% poly- second
Enolate solution is cooled to room temperature；
(3) 9g, 11g, 13g, 15g, 17g, 19g polyvinylpyrrolidone is taken to be dissolved in 90% ethyl alcohol of 100mL, in room temperature
It stirs evenly, respectively obtaining quality volume fraction is that 9%, 11%, 13%, 15%, 17%, 19% polyvinylpyrrolidone is molten
Liquid；The ethyl acetate extract of the ford nervilia leaf of 800mg step (1) preparation is added, makes its concentration 8mg/mL；
(4) it takes (3) solution of equivalent to be added in (2) solution of equivalent, is uniformly mixed, the mixing for obtaining different ratio is spun
Silk solution, the concentration of ford nervilia leaf ethyl acetate extract is 4mg/mL at this time；
(5) gained spinning solution in (3) is sucked into 10mL syringe, loads onto diameter 0.6mm syringe needle, adjustment syringe needle to reception
The distance of device is 14cm, adjusts voltage in 15kV, and temperature is 27 DEG C, humidity 60%, flow control in 0.3mL/h, spinning 8h,
Then 12h is dried in vacuo at 35 DEG C to get the nano-fiber composite film of different ratio is arrived.
The SEM of the nano-fiber composite film prepared under above-mentioned process conditions is shown in Fig. 5.Pass through Electronic Speculum graph discovery, 15%PVP tool
There is preferable fiber morphology.
Embodiment 8
The present embodiment and embodiment 7 are the difference is that the quality volume fraction of polyvinylpyrrolidone is 15%, so
After be separately added into quality volume fraction be 5%, 6%, 7%, 8%, 9%, 10% poly-vinyl alcohol solution.
The SEM of the nano-fiber composite film prepared under above-mentioned process conditions is shown in Fig. 6, passes through Electronic Speculum graph discovery, 10%PVA tool
There is preferable fiber morphology.
Embodiment 9
The present embodiment and embodiment 7 are gathered the difference is that the quality volume fraction of polyvinylpyrrolidone is 15%
The quality volume fraction of vinyl alcohol is 10%, and the distance of syringe needle to receiver is 12cm, 14cm, 16cm.
Embodiment 10
The present embodiment and embodiment 7 are gathered the difference is that the quality volume fraction of polyvinylpyrrolidone is 15%
The quality volume fraction of vinyl alcohol is 10%, and spinning voltage is in 10kV, 15kV, 20kV.
Embodiment 11
The present embodiment and embodiment 7 are gathered the difference is that the quality volume fraction of polyvinylpyrrolidone is 15%
The quality volume fraction of vinyl alcohol is 10%, flow velocity 0.15mL/h, 0.3mL/h, 0.45mL/h.
Fig. 7 (a), (b), (c) are respectively the nano-fiber composite film scanning electricity of embodiment 9, embodiment 10 and embodiment 11
Mirror figure.Pass through Electronic Speculum graph discovery, under conditions of spinning voltage 15kV, receiving distance 14cm, flow velocity 0.3mL/h, spinning film tool
There is preferable fiber morphology.
Embodiment 12
Nano-fiber composite film containing Folium Nerviliae fordii extract is as anti-oxidant packaging material in different food products simulated system
Using, the specific steps are as follows:
(1) the first and second the third four kinds of nano fibrous membranes of fourth of configuration, steps are as follows for concrete configuration:
First: 3g PVP is dissolved in 90% ethyl alcohol of 20mL, uniform in stirring at normal temperature, and 160mg sample is added, makes sample concentration
For 8mg/mL；2g PVA is dissolved in 20mL water, in 80 DEG C of stirring 2h, is obtained 10%PVA solution, is cooled to room temperature；By the two
Mixing, being made into final volume ratio is 10%PVA:15%PVP=1:1, and sample concentration is the 40mL spinning solution of 4mg/mL.
Second: same to first, being made into final volume ratio is 10%PVA:10%PVP=1:1, and the 40mL that sample concentration is 4mg/mL is spun
Silk solution.
Third: same to first, being made into final volume ratio is 10%PVA:15%PVP=2:1, and the 40mL that sample concentration is 4mg/mL is spun
Silk solution.
Fourth: same to first, being made into final volume ratio is 10%PVA:10%PVP=2:1, and the 40mL that sample concentration is 4mg/mL is spun
Silk solution.
(2) each spinning solution of gained in (1) is sucked into 10mL syringe, loads onto diameter 0.6mm syringe needle, adjustment syringe needle is to connecing
The distance for receiving device is 14cm, adjusts voltage in 15kV, temperature is 27 DEG C, and humidity 60%, flow control is in 0.3mL/h, spinning
Then 8h is dried in vacuo 12h at 35 DEG C to get different nano-fiber composite films is arrived.
(3) certain mass (2) spinning film is taken to be dissolved in different dissolution mediums (water, 3% acetic acid, 10% ethyl alcohol, 50% respectively
Ethyl alcohol, 95% ethyl alcohol) in, it cultivates at 25 DEG C, is sampled every 1d, carry out the measurement that DPPH removes power and general flavone content.
Fig. 8 is the anti-oxidant measuring result of different films under above-mentioned process conditions.Fig. 9 is different under above-mentioned process conditions
The release profiles of Folium Nerviliae fordii extract in film.As shown in Figure 9, since Folium Nerviliae fordii extract is lyophobic dust, so being included in
The rate that Folium Nerviliae fordii extract in nano-fiber composite film discharges in 95% ethyl alcohol is most fast, also can sustained release but final
25 days or more.Secondly, including that Folium Nerviliae fordii extract in nano-fiber composite film also can be carried out duration release in water, say
The problem of bright present invention improves the poorly water-soluble of Folium Nerviliae fordii extract well, expands its answering in food packaging applications
With.
Embodiment 13
(1) 15g PVP is dissolved in 90% ethyl alcohol, uniform in stirring at normal temperature, obtains 15%PVP solution, and preparation 15%PVP receives
Rice tunica fibrosa；
(2) 10g polyvinyl alcohol is dissolved in 100mL distilled water, in 80 DEG C of stirring 2h, obtains 10% poly-vinyl alcohol solution, cold
But to room temperature, 10%PVA nano fibrous membrane is prepared；
(3) first, second, third, fourth nano-fiber composite film are prepared according to method in embodiment 10；
(4) (1), (2), (3) resulting nano-fiber composite film and ford nervilia leaf ethyl acetate extract are subjected to infrared light
Spectrum scanning, 4000~400cm of scanning range-1, the former uses ATR, and the latter uses KRr tabletting (see Figure 10).
By Figure 10 (a) it is found that the characteristic absorption peak of pure PVP is 3435cm-1The O-H absorption peak at place, 2955cm-1The C-H at place
Flexible peak, 1644cm-1The C=O absorption peak at place；The characteristic absorption peak of pure PVA is 3275cm-1The O-H absorption peak at place, 2936cm-1
The CH at place2, 1680cm-1The C=O absorption peak at place, 1420cm-1The CH at place2Flexural vibrations peak, 1088cm-1The C-O-C at place is flexible
Peak；
It can be seen that the increase with PVA content from Figure 10 (b), O-H absorption peak thinks that low frequency is mobile, illustrates hydrogen bond
It is formed, and in 2936cm-1、1680cm-1、1088cm-1The characteristic absorption peak for locating PVA increases also with PVA content, and peak type increases
Add.In 4 kinds of prepared tunica fibrosas, the absorption peak of extract has all been vanished from sight, and illustrates that it is embedded in fiber.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of the nano-fiber composite film containing Folium Nerviliae fordii extract, it is characterised in that include the following steps:
Folium Nerviliae fordii extract, polyvinylpyrrolidone and poly-vinyl alcohol solution are mixed and made into spinning solution, it is then that spinning is molten
Liquid carries out electrostatic spinning, obtains the nano fibrous membrane containing Folium Nerviliae fordii extract by electrostatic spinning apparatus；Wherein spinning voltage is
13-25kV, the distance of syringe needle to receiver are 12-16cm, and spinning rate is 0.2-0.6mL/h.
2. preparation method according to claim 1, it is characterised in that the spinning solution the preparation method comprises the following steps:
By the polyvinyl alcohol quality volume fraction soluble in water that obtains for the poly-vinyl alcohol solution of 5%-10%；By polyvinylpyrrolidine
Ketone is dissolved in 90% ethanol solution, obtains the polyvinylpyrrolidonesolution solution that quality volume fraction is 9%-19%, is then added green
Semiaquilegia root extract；The polyvinylpyrrolidonesolution solution containing Folium Nerviliae fordii extract is added in poly-vinyl alcohol solution again；Poly- second
The volume ratio of enolate solution and polyvinylpyrrolidonesolution solution is 1:1-2:1, and Folium Nerviliae fordii extract is dense in gained mixed solution
Degree is 3.5-4.5mg/mL.
3. preparation method according to claim 2, it is characterised in that added polyvinylpyrrolidine in the spinning solution
The quality volume fraction of ketone solution is 15%, and the quality volume fraction of added poly-vinyl alcohol solution is 10%, and polyvinyl alcohol is molten
The volume ratio of liquid and polyvinylpyrrolidonesolution solution is 1:1, and the concentration of Folium Nerviliae fordii extract is 4mg/mL in spinning solution.
4. preparation method according to claim 1 or 2 or 3, it is characterised in that the preparation method of the Folium Nerviliae fordii extract
Are as follows:
(1) ford nervilia leaf is crushed, is extracted with organic solvent；
(2) the extraction product of step (1) is passed sequentially through into petroleum ether, ethyl acetate extracts or pass sequentially through petroleum ether, acetic acid second
Ester, extracting n-butyl alcohol, every phase extract 3-5 times, each 3-5h, obtain Folium Nerviliae fordii extract.
5. the preparation method according to claim 4, it is characterised in that step (1) organic solvent be ethyl alcohol, methanol or
One of acetone is a variety of, volume fraction 40%-95%, solid-liquid ratio 1:5-1:20, it is described be extracted as reflux extraction,
One of intensified by ultrasonic wave extraction, microwave-assisted extraction are a variety of, and number is 1-3 times, each 1-3h, and Extracting temperature is
50℃-90℃。
6. the preparation method according to claim 4, it is characterised in that step (1) ford nervilia leaf is ford nervilia leaf, organic
Solvent is the ethyl alcohol of volume fraction 56%, and Extracting temperature is 75 DEG C, solid-liquid ratio 1:14；Extraction time is 2 times, each 2h.
7. the preparation method according to claim 4, it is characterised in that the step (2) is to produce step (1) extraction
Object passes sequentially through petroleum ether, ethyl acetate extraction, and every phase extracts 4 times, each 4h.
8. preparation method according to claim 1 or 2 or 3, it is characterised in that the spinning voltage is 15kV, and syringe needle is to connecing
The distance for receiving device is 14cm, and spinning rate is 0.3mL/h.
9. a kind of anti-oxidant nano-fiber composite film containing Folium Nerviliae fordii extract of method preparation according to claims 1 to 8.
10. the anti-oxidant nano-fiber composite film according to claim 9 containing Folium Nerviliae fordii extract is in anti-oxidant packing timber
Application in material.
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