CN103725017B - A kind of fish collagen antibacterial film with slow releasing function and preparation method thereof - Google Patents
A kind of fish collagen antibacterial film with slow releasing function and preparation method thereof Download PDFInfo
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- CN103725017B CN103725017B CN201310721581.3A CN201310721581A CN103725017B CN 103725017 B CN103725017 B CN 103725017B CN 201310721581 A CN201310721581 A CN 201310721581A CN 103725017 B CN103725017 B CN 103725017B
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Abstract
The invention discloses a kind of fish collagen antibacterial film with slow releasing function and preparation method thereof, is belong to nanometer liposome slowly-releasing and antibacterial applied technical field.First Isin glue collagen and glycerine are dissolved in the water and make Isin glue collagen solution, then add cinnamon essential oil nano lipidosome suspension altogether, stir, ultrasonic degas, pipettes and spreads in drying and forming-film on poly (methyl methacrylate) plate.The antibacterial film that the present invention makes anti-microbial property compared with simple collagen film is greatly improved, and due to the provide protection of liposome to cinnamon essential oil and the slowly-releasing of cinnamon essential oil, makes the anti-microbial property of the composite membrane sustainable long period.In addition, this film can be biodegradable, can not to environment in use procedure, have and prevent the flavour substances of food to scatter and disappear, the function such as prevent food contaminated and oxidized, reaches the effect of food fresh keeping and Shelf-life.
Description
Technical field
The invention belongs to nanometer liposome slowly-releasing and antibacterial applied technical field, be specifically related to a kind of fish collagen antibacterial film with slow releasing function and preparation method thereof.
Background technology
Collagen protein is a kind of important natural macromolecular material, antigenicity is low, has good biocompatibility and biodegradability, therefore, as natural biomass resource, the importance applied in the industry such as food, biomedicine, makeup and economic status become increasingly conspicuous.But simple collagen film physicochemical property are relatively weak, in order to improve the character of film, Cucumber can be added in collagen solution before film forming, such as, can add and there is antibacterial ability or the antioxidant property that bioactive natural product improves collagen film; Or add the mechanical property of polysaccharide or lipid change collagen film as required, permeability etc.But due to essential oil itself, there is certain volatility and add rayed, oxygen and other factors affect that itself is easily oxidized, decompose and destroy, and it can not be played a role for a long time.In order to extend the anti-microbial activity of film, the biologically active substance to adding can being adopted first to add protection, making it in use maintain long activity.Present invention employs and active substance made nanometer liposome form and first add protection and add to again in collagen solution, make cinnamon essential oil nano lipidosome collagen film, control the release of cinnamon essential oil, extend the germ resistance of film.
Summary of the invention
The object of the present invention is to provide a kind of fish collagen antibacterial film with slow releasing function and preparation method thereof; the antibacterial film that the present invention makes anti-microbial property compared with simple collagen film is greatly improved; and due to the provide protection of liposome to cinnamon essential oil and the slowly-releasing of cinnamon essential oil, make the anti-microbial property of the composite membrane sustainable long period.In addition, this film can be biodegradable, can not to environment in use procedure, have and prevent the flavour substances of food to scatter and disappear, the function such as prevent food contaminated and oxidized, reaches the effect of food fresh keeping and Shelf-life.
For achieving the above object, the present invention adopts following technical scheme:
A kind of have in the component of the fish collagen antibacterial film of slow releasing function containing cinnamon essential oil nano lipidosome, Isin glue collagen and glycerine.
The method that preparation has the fish collagen antibacterial film of slow releasing function as above comprises the following steps:
(1) cinnamon essential oil nano lipidosome suspension is altogether prepared
Taking soybean lecithin 200mg, cinnamon essential oil 100-140mg, cholesterol 25mg, VE1.5mg and Sodium cholic acid 2mg, to be dissolved in volume be in the chloroform of 60ml, and decompression rotary evaporation removes organic solvent, makes lipid form film in flask walls; Then the phosphoric acid buffer 60ml adding pH=7.0 in flask forms suspension, makes it mix suspension at 40 DEG C of water-bath rotary evaporation in vacuo; The last tween-80 adding 300ul in suspension, through Probe Ultrasonic Searching process: 100W, 2s open, 2s stops, ultrasonic 6min, obtains cinnamon essential oil nano lipidosome suspension altogether;
(2) Isin glue collagen solution is prepared
2-3g Isin glue collagen is placed in 100ml round-bottomed flask, and with 50ml deionized water at room temperature swelling 2h, add 0.5-0.75g glycerine as softening agent, then stirring and dissolving 1h at 45 DEG C, makes it mix, and makes Isin glue collagen solution;
(3) the antibiosis rubber collagen film of preparation containing cinnamon essential oil nano lipidosome
Cinnamon essential oil nano lipidosome step (1) prepared altogether suspension 50ml joins in the Isin glue collagen solution of 50ml prepared by step (2), stirs, ultrasonic degas, 45 DEG C of insulations; Pipette the Isin glue collagen solution that 10ml with the addition of cinnamon essential oil nano lipidosome at every turn and spread into film forming on poly (methyl methacrylate) plate, film-forming temperature is 45 DEG C, and film formation time is 48h, the obtained antibiosis rubber collagen film containing cinnamon essential oil nano lipidosome.
The analytical procedure that the present invention adopts:
(1) cinnamon essential oil nano lipidosome median size: with ZETASIZER3000 laser nano particle size analyzer determination.
(2) cinnamon essential oil nano lipidosome encapsulation rate: measure with UV-2450 Zi Wai – visible spectrophotometer.
(3) Zeta potential: measure with ZataSizer2000 type Zeta potential determinator.
(4) release experiment: survey its burst size with Agilent1100 high performance liquid chromatography.The collagen film that what in figure, ■ represented is containing cinnamon essential oil solution, and zero represents is the collagen film being added with cinnamon essential oil nano lipidosome.
(5) antibacterial stability: measure with disc diffusion method.
Beneficial effect of the present invention is: the present invention adopts nanometer liposome slowly-releasing and antibacterial edible film technology to prepare the antibiosis rubber collagen film of fixing cinnamon essential oil nano lipidosome, control the release of cinnamon essential oil in collagen film, extend the antibacterial effect of collagen film.
Accompanying drawing explanation
Fig. 1 is cinnamon essential oil nano lipidosome antibiosis rubber collagen film and the release graphics of collagen film under 4 degree contrasting cinnamon essential oil.
To be antibiosis rubber collagen film containing cinnamon essential oil nano lipidosome compare 3 days and the colibacillary ability of suppression after storing 30 days with the collagen film contrasting cinnamon essential oil Fig. 2 respectively.The collagen film of a, contrast cinnamon essential oil, the antibiosis rubber collagen film of b, cinnamon essential oil nano lipidosome.
Embodiment
A kind of preparation method with the fish collagen antibacterial film of slow releasing function comprises the following steps:
(1) cinnamon essential oil nano lipidosome suspension is altogether prepared
Taking soybean lecithin 200mg, cinnamon essential oil 100-140mg, cholesterol 25mg, VE1.5mg and Sodium cholic acid 2mg, to be dissolved in volume be in the chloroform of 60ml, and decompression rotary evaporation removes organic solvent, makes lipid form film in flask walls; Then the phosphoric acid buffer 60ml adding pH=7.0 in flask forms suspension, makes it mix suspension at 40 DEG C of water-bath rotary evaporation in vacuo; The last tween-80 adding 300ul in suspension, through Probe Ultrasonic Searching process: 100W, 2s open, 2s stops, ultrasonic 6min, obtains cinnamon essential oil nano lipidosome suspension altogether;
(2) Isin glue collagen solution is prepared
2-3g Isin glue collagen is placed in 100ml round-bottomed flask, and with 50ml deionized water at room temperature swelling 2h, add 0.5-0.75g glycerine as softening agent, then stirring and dissolving 1h at 45 DEG C, makes it mix, and makes Isin glue collagen solution;
(3) the antibiosis rubber collagen film of preparation containing cinnamon essential oil nano lipidosome
Cinnamon essential oil nano lipidosome step (1) prepared altogether suspension 50ml joins in the Isin glue collagen solution of 50ml prepared by step (2), stirs, ultrasonic degas, 45 DEG C of insulations; Pipette the Isin glue collagen solution that 10ml with the addition of cinnamon essential oil nano lipidosome at every turn and spread into film forming on poly (methyl methacrylate) plate, film-forming temperature is 45 DEG C, and film formation time is 48h, the obtained antibiosis rubber collagen film containing cinnamon essential oil nano lipidosome.
embodiment 1
Take soybean lecithin 200mg, cinnamon essential oil 100mg, cholesterol 25mg, VE1.5mg, it is in the chloroformic solution of 60ml that Sodium cholic acid 2mg is dissolved in volume, and decompression rotary evaporation removes organic solvent, makes lipid form film in flask walls; Then the phosphoric acid buffer 60ml adding pH=7.0 in flask forms suspension, makes it mix suspension at 40 DEG C of water-bath rotary evaporation in vacuo; The last tween-80 adding 300ul in suspension, and by it at ice-water bath Probe Ultrasonic Searching (100W, 2s stop, and 2s opens) 6min, cinnamon essential oil nano lipidosome.
2g collagen protein is placed in 100ml beaker, and with 50ml deionized water at room temperature swelling 2h, add 0.5g glycerine as softening agent, then stirring and dissolving 1h at 45 DEG C, makes it mix, makes collagen solution.
Cinnamon essential oil nano lipidosome is total to suspension 50ml to be joined in the gelatin solution of 50ml, stirs, ultrasonic degas, 45 DEG C of insulations; Pipette the collagen solution that 10ml with the addition of cinnamon essential oil nano lipidosome at every turn and spread into film forming on poly (methyl methacrylate) plate, film-forming temperature is 45 DEG C, and film formation time is 48h.
embodiment 2
Take soybean lecithin 200mg, cinnamon essential oil 140mg, cholesterol 25mg, VE1.5mg, it is in the chloroformic solution of 60ml that Sodium cholic acid 2mg is dissolved in volume, and decompression rotary evaporation removes organic solvent, makes lipid form film in flask walls; Then the phosphoric acid buffer 60ml adding pH=7.0 in flask forms suspension, makes it mix suspension at 40 DEG C of water-bath rotary evaporation in vacuo; The last tween-80 adding 300ul in suspension, and by it at ice-water bath Probe Ultrasonic Searching (100W, 2s stop, and 2s opens) 6min, cinnamon essential oil nano lipidosome.
3g collagen protein is placed in 100ml beaker, and with 50ml deionized water at room temperature swelling 2h, add 0.75g glycerine as softening agent, then stirring and dissolving 1h at 45 DEG C, makes it mix, makes collagen solution.
Cinnamon essential oil nano lipidosome is total to suspension 50ml to be joined in the gelatin solution of 50ml, stirs, ultrasonic degas, 45 DEG C of insulations; Pipette the collagen solution that 10ml with the addition of cinnamon essential oil nano lipidosome at every turn and spread into film forming on poly (methyl methacrylate) plate, film-forming temperature is 45 DEG C, and film formation time is 48h.
As can be seen from Fig. 1 we, join in collagem membrane compared with directly joining in collagem membrane with cinnamon essential oil solution after cinnamon essential oil being made nanometer liposome, the former release rate reduces a lot, reach the effect of slowly-releasing, therefore, with this film wrap food can be more lasting fresh-keeping foodstuff thus extend its shelf-lives.
As can be seen from Figure 2, at the beginning in the initial period (the 3rd day) that this film preparation is good, this film is to colibacillary suppression, and the collagen film containing contrast cinnamon essential oil, compared with the antibiosis rubber collagen film of cinnamon essential oil nano lipidosome, shows slightly high antibacterial ability.But along with the prolongation in storage time; the antibacterial ability of the latter's film is on the contrary higher than the former; this is not mainly because the main antimicrobial component phenylacrolein in the bilayer structural defence cinnamon essential oil of nanometer liposome is by external interference; and this structure also extends the residence time in cinnamon essential oil bilayer; active ingredient phenylacrolein in cinnamon essential oil can be slowly released in time; reach the effect of slowly-releasing, thus increase the antibacterial stability of liposome collagen film.Visible cinnamon essential oil is made nanometer liposome after, along with the prolongation of time, the germ resistance that can not only improve this film also extends the shelf-lives of food simultaneously.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (1)
1. there is a preparation method for the fish collagen antibacterial film of slow releasing function, it is characterized in that: containing cinnamon essential oil nano lipidosome, Isin glue collagen and glycerine in described membrane component;
Preparation method comprises the following steps:
(1) cinnamon essential oil nano lipidosome suspension is altogether prepared
Taking soybean lecithin 200mg, cinnamon essential oil 100-140mg, cholesterol 25mg, VE1.5mg and Sodium cholic acid 2mg, to be dissolved in volume be in the chloroform of 60ml, and decompression rotary evaporation removes organic solvent, makes lipid form film in flask walls; Then the phosphoric acid buffer 60ml adding pH=7.0 in flask forms suspension, makes it mix suspension at 40 DEG C of water-bath rotary evaporation in vacuo; The last tween-80 adding 300 μ l in suspension, through Probe Ultrasonic Searching process: 100W, 2s open, 2s stops, ultrasonic 6min, obtains cinnamon essential oil nano lipidosome suspension altogether;
(2) Isin glue collagen solution is prepared
2-3g Isin glue collagen is placed in 100ml round-bottomed flask, and with 50ml deionized water at room temperature swelling 2h, add 0.5-0.75g glycerine as softening agent, then stirring and dissolving 1h at 45 DEG C, makes it mix, and makes Isin glue collagen solution;
(3) preparation has the fish collagen antibacterial film of slow releasing function
Cinnamon essential oil nano lipidosome step (1) prepared altogether suspension 50ml joins in the Isin glue collagen solution of 50ml prepared by step (2), stirs, ultrasonic degas, 45 DEG C of insulations; Pipette the Isin glue collagen solution that 10ml with the addition of cinnamon essential oil nano lipidosome at every turn and spread into film forming on poly (methyl methacrylate) plate, film-forming temperature is 45 DEG C, and film formation time is 48h, the obtained fish collagen antibacterial film with slow releasing function.
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| CN104164090A (en) * | 2014-05-30 | 2014-11-26 | 中国计量学院 | EGCG nano liposome edible film and preparation method thereof |
| CN104387779A (en) * | 2014-11-05 | 2015-03-04 | 福州大学 | Antioxidative collagen film containing active plant extract nanoliposome |
| CN104382039A (en) * | 2014-12-19 | 2015-03-04 | 福州大学 | Nano lipidosome containing green tea extractive, and preparation method thereof |
| CN106317909A (en) * | 2016-08-25 | 2017-01-11 | 董晓 | Preparing method of antibacterial medical grade thin film material |
| CN112021393A (en) * | 2019-06-03 | 2020-12-04 | 浙江工商大学 | Composite preservative containing natural essential oil nanoliposome and application of composite preservative in sturgeon fillet preservation |
| CN114698676A (en) * | 2022-03-23 | 2022-07-05 | 福州大学 | Preparation method and application of silver carp skin collagen-based antibacterial and antioxidant active coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101461534A (en) * | 2009-01-14 | 2009-06-24 | 江南大学 | Method for preparing antioxidation gelatine membrane containing tea polyphenol nano lipidosome |
| CN103030979A (en) * | 2012-12-27 | 2013-04-10 | 福建省博特生物科技有限公司 | Collagen antibacterial membrane containing cinnamon essential oil and preparation method of collagen antibacterial membrane |
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| HUP0700426A2 (en) * | 2007-06-19 | 2010-03-29 | Invencio 21 Gyogyhatasu Keszit | Liposomal compound |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101461534A (en) * | 2009-01-14 | 2009-06-24 | 江南大学 | Method for preparing antioxidation gelatine membrane containing tea polyphenol nano lipidosome |
| CN103030979A (en) * | 2012-12-27 | 2013-04-10 | 福建省博特生物科技有限公司 | Collagen antibacterial membrane containing cinnamon essential oil and preparation method of collagen antibacterial membrane |
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