CN101397695B - Method for preparing stable gelatine nano fiber for bionic stent material - Google Patents
Method for preparing stable gelatine nano fiber for bionic stent material Download PDFInfo
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- CN101397695B CN101397695B CN2008102021670A CN200810202167A CN101397695B CN 101397695 B CN101397695 B CN 101397695B CN 2008102021670 A CN2008102021670 A CN 2008102021670A CN 200810202167 A CN200810202167 A CN 200810202167A CN 101397695 B CN101397695 B CN 101397695B
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Abstract
The invention relates to a preparation method for preparing a stable-typed gelatin nano-fiber used in bionic support material by adopting the electrostatic spinning technology, which comprises the steps of (1) preparing an electrostatic spinning solution with the concentration of 8 percent (g/ml), (2) utilizing the electrostatic spinning technology to prepare nano-fiber filaments by utilizing the prepared solution under the control of parameters and (3) processing the electrostatic spun nano-fiber by the ways of blending, vapor, immersing and the like so as to make the bionic scaffolding material. The preparation method of the invention is simple, has little time consumption and obtains the stable bionic scaffolding material.
Description
Technical field
The invention belongs to the preparation field of gelatine nano fiber, particularly relate to a kind of preparation method who is used for the stable gelatine nano fiber of bionic bracket material.
Background technology
Electrostatic spinning technique is realized in 1934 by Formhals etc. the earliest.Be different from traditional spinning.The fibre diameter of electrostatic spinning preparation is very thin, and random the piling up of fiber formed a kind of porous film material that a large amount of micropores are arranged, and very big specific area is arranged.By changing various conditions, can prepare the different electro spinning nanometer fiber membrane of geometry forms.This nano material refilters material, and many fields such as organizational project all have potential application.
The good biocompatibility of boiomacromolecule often shows biologically actives such as promoting cell adhesion, growth, becomes the first-selection that makes up tissue engineering bracket.The extracellular stent size is very close in the fiber size of electrospinning preparation and the body, so the boiomacromolecule electrospinning fibre is used as bone, and blood vessel, skin etc. have unique advantage.But there is easily degraded in the boiomacromolecule electrospinning fibre, defectives such as instability, need carry out certain chemical modification handles to guarantee that its fibre morphology is not destroyed, but, therefore consider to adopt biological crosslinking agent Geniposide to carry out chemical modification and handle to prepare stable gelatine nano fiber in order not introduce other poisonous materials
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method who is used for the stable gelatine nano fiber of bionic bracket material, the Geniposide crosslinking agent that the present invention adopts is a kind of new bio non-toxic crosslinker, nanofiber is after modification is handled, good stability, fibre morphology is difficult for destroyed.
A kind of preparation method who is used for the stable gelatine nano fiber of bionic bracket material of the present invention comprises:
(1) preparation of solution: gelatin is dissolved in the organic solvent, is mixed with the solution that concentration is 8% (g/ml),, obtain the solution of transparent and homogeneous through the dissolving fully that is stirred well to of 24h;
Or the preparation of (2) hybrid gelatine nano fiber: the Geniposide crosslinking agent is mixed by weight 2.5%, 5%, 7.5%, 10% with gelatin, add in the above-mentioned solution, stir 30min-60min till the transparent and homogeneous, be equipped with film forming by electro-spinning, voltage is 16kv, electric field distance is 150mm, and spinning speed is 1.0ml/h, places vacuum drying chamber to remove residual solvent then;
Or the preparation of (3) steam-type gelatine nano fiber: spin step (1) prepared solution by static, voltage is 16kv, electric field distance is 150mm, spinning speed is 1.0ml/h, obtain static and spin the gelatine nano fiber film, with ethanol and water by volume 9:1 mix, and adding Geniposide, be mixed with Geniposide content and be 0.5% crosslinker solution, the culture dish that to put into a diameter be 10cm, the drier bottom that then culture dish to be put into a clean diameter be 21cm is placed on the electrostatic spinning fiber film of a 100mm * 100mm * 0.1mm on the aluminium platinum, puts into then on the disk with holes that is arranged in above the drier culture dish, evaporation by solvent vapour carries out crosslinked to film, after the crosslinked end, film is put into vacuum drying chamber place a week, remove uncrosslinked residual solvent;
Or the preparation of (4) immersion gelatine nano fiber: spin step (1) prepared solution by static, voltage is 16kv, electric field distance is 150mm, spinning speed is 1.0ml/h, obtain static and spin the gelatine nano fiber film, with ethanol and water by volume 9:1 mix, and adding Geniposide, be mixed with Geniposide content and be 0.5% crosslinker solution, get 20ml and place beaker to 30ml, then static is spun film immerse wherein carry out crosslinked, crosslinked ends back taking-up, blot surface moisture with filter paper, place vacuum drying chamber to remove residual cross-linker.
Organic solvent in the described step (1) is trifluoroethanol, hexafluoroisopropanol, trifluoroacetic acid, chloroform or acetone equal solvent;
The ratio of the crosslinking agent in the described step (2) is 2.5%, 5%, 7.5% or 10%;
The degree of cross linking can be controlled by different crosslinking times in the described step (4);
Described stable gelatine nano fiber film is applied to aspects such as wound auxiliary material, artificial blood vessel and tissue engineering bracket research.
The gelatin that the present invention is used to prepare nanofiber is a kind of biodegradable polymer, except that gelatin, can also select for use one or more the mixture in shitosan, collagen, the hyaluronic acid etc. to be used to prepare nanofiber.
Beneficial effect
The Geniposide crosslinking agent that the present invention adopts is a kind of new bio non-toxic crosslinker, nanofiber after modification is handled, good stability, fibre morphology is difficult for destroyed.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Take by weighing the 0.8g gelatin with electronic balance, be dissolved in the trifluoroethanol of 10ml, stir vibration, obtain the solution that concentration is 8% (g/ml) to dissolving fully; Ratio according to 2.5%-10% adds biological crosslinking agent Geniposide, and then stirs 30min-60min.The solution that electrostatic spinning is prepared, voltage are 16kv, and the syringe pump fltting speed is 1ml/h, and receiving range is 15cm, select syringe needle for use No. 7, aluminium foil ground connection, and the static that obtains average diameter and be 300nm spins the blend gelatine nano fiber.
Embodiment 2
Take by weighing the 0.8g gelatin with electronic balance, be dissolved in the trifluoroethanol of 10ml, stir vibration, obtain the solution that concentration is 8% (g/ml) to dissolving fully; The solution that electrostatic spinning is prepared, voltage are 16kv, and the syringe pump fltting speed is 1ml/h, and receiving range is 15cm, select syringe needle for use No. 7, aluminium foil ground connection, and the static that obtains average diameter and be 300nm spins gelatine nano fiber; Join the ethanol that contains Geniposide 0.5% solution than water 9/1, the culture dish that it is 10cm that the solution that 10ml is configured is put into a diameter, the drier bottom that then culture dish to be put into a clean diameter be 21cm, the static spinning superfine fibre film of previous preparation is placed on the aluminium platinum, put into then on the disk with holes that is arranged in above the drier culture dish, evaporation by solvent vapour comes film is carried out crosslinked, and crosslinking degree can be realized by controlling different crosslinking times.After the crosslinked end, crosslinked film is put into vacuum drying chamber place a week, remove uncrosslinked residual solvent.
Embodiment 3
Take by weighing the 0.8g gelatin with electronic balance, be dissolved in the trifluoroethanol of 10ml, stir vibration, obtain the solution that concentration is 8% (g/ml) to dissolving fully; The solution that electrostatic spinning is prepared, voltage are 16kv, and the syringe pump fltting speed is 1ml/h, and receiving range is 15cm, select syringe needle for use No. 7, aluminium foil ground connection, and the static that obtains average diameter and be 300nm spins gelatine nano fiber; Join the ethanol that contains Geniposide 0.5% solution than water 9/1, get 20ml and place beaker to 30ml, then static is spun film and immerse wherein, crosslinking degree can be realized by controlling different crosslinking times.Take out, blot surface moisture, place vacuum drying chamber to remove residual cross-linker with filter paper.
Claims (4)
1. preparation method who is used for the stable gelatine nano fiber of bionic bracket material comprises:
(1) preparation of solution: gelatin is dissolved in the organic solvent, is mixed with the solution that concentration is 8%g/ml,, obtain the solution of transparent and homogeneous through the dissolving fully that is stirred well to of 24h;
(2) preparation of hybrid gelatine nano fiber: the Geniposide crosslinking agent is mixed by weight 2.5%, 5%, 7.5% or 10% with described gelatin, add in the above-mentioned solution, stir 30min-60min till the transparent and homogeneous, be equipped with film forming by electro-spinning, voltage is 16kv, electric field distance is 150mm, and spinning speed is 1.0ml/h, places vacuum drying chamber to remove residual solvent then;
Or the preparation of (3) steam-type gelatine nano fiber: spin step (1) prepared solution by static, voltage is 16kv, electric field distance is 150mm, spinning speed is 1.0ml/h, obtain static and spin the gelatine nano fiber film, ethanol and water were mixed in 9: 1 by volume, and adding Geniposide, be mixed with Geniposide content and be 0.5% crosslinker solution, the culture dish that to put into a diameter be 10cm, the drier bottom that then culture dish to be put into a clean diameter be 21cm is placed on the electrostatic spinning fiber film of a 100mm * 100mm * 0.1mm on the aluminium platinum, puts into then on the disk with holes that is arranged in above the drier culture dish, evaporation by solvent vapour carries out crosslinked to film, after the crosslinked end, film is put into vacuum drying chamber place a week, remove uncrosslinked residual solvent;
Or the preparation of (4) immersion gelatine nano fiber: spin step (1) prepared solution by static, voltage is 16kv, electric field distance is 150mm, spinning speed is 1.0ml/h, obtain static and spin the gelatine nano fiber film, ethanol and water were mixed in 9: 1 by volume, and adding Geniposide, be mixed with Geniposide content and be 0.5% crosslinker solution, get 20ml and place beaker to 30ml, then static is spun film immerse wherein carry out crosslinked, crosslinked ends back taking-up, blot surface moisture with filter paper, place vacuum drying chamber to remove residual cross-linker.
2. a kind of preparation method who is used for the stable gelatine nano fiber of bionic bracket material according to claim 1 is characterized in that: the organic solvent in the described step (1) is trifluoroethanol, hexafluoroisopropanol, trifluoroacetic acid, chloroform or acetone.
3. a kind of preparation method who is used for the stable gelatine nano fiber of bionic bracket material according to claim 1 is characterized in that: described step (3) can be controlled by different crosslinking times with (4) middle degree of cross linking.
4. a kind of preparation method who is used for the stable gelatine nano fiber of bionic bracket material according to claim 1 is characterized in that: described stable gelatine nano fiber film is applied to wound auxiliary material, artificial blood vessel and tissue engineering bracket research aspect.
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CN103173893B (en) * | 2010-06-04 | 2015-04-22 | 康力得生技股份有限公司 | Polymer fiber and preparation method thereof |
CN102383267A (en) * | 2011-07-22 | 2012-03-21 | 北京化工大学 | Natural polymer-based nano-fibrous membrane prepared by freeze-drying method |
CN104562438B (en) * | 2013-10-17 | 2017-07-14 | 中国科学院理化技术研究所 | Gelatin-based micro-nano fiber membrane material and preparation method and application thereof |
CN103690991B (en) * | 2013-12-17 | 2015-09-30 | 李克尊 | A kind of preparation method of cartilage repairing scaffold material |
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