CN107469127A - The preparation method of natural polysaccharide derivative/natural polymer composite fibre medical wound dressing - Google Patents
The preparation method of natural polysaccharide derivative/natural polymer composite fibre medical wound dressing Download PDFInfo
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- CN107469127A CN107469127A CN201710662863.9A CN201710662863A CN107469127A CN 107469127 A CN107469127 A CN 107469127A CN 201710662863 A CN201710662863 A CN 201710662863A CN 107469127 A CN107469127 A CN 107469127A
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- Prior art keywords
- composite fibre
- natural
- preparation
- natural polysaccharide
- wound dressing
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Classifications
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Abstract
The invention provides the preparation method of natural polysaccharide derivative/natural polymer composite fibre medical wound dressing, belong to medical dressing manufacturing field.The preparation method of described natural polysaccharide derivative/natural polymer composite fibre medical wound dressing includes：Chemical modification is carried out to natural polysaccharide, obtain modified natural polysaccharide derivative, then it is prepared into fiber with natural polymer Combined Mining with electrostatic spinning technique, composite fibre is irradiated under uviol lamp and crosslinked, then carry out Co 60 gamma ray radiation sterilization, segmentation, packaging can obtain natural polysaccharide derivative/natural polymer composite fibre medical wound dressing.Medical wound dressing raw material natural reproducible, abundance, preparation process obtained by the present invention be simple, can large area production, intensity controlled, safety and environmental protection, gas permeability and good biocompatibility, there is hemostasis, anti-inflammatory, antiallergy etc. to act on.
Description
Technical field
The invention discloses a kind of new natural polysaccharide derivative/natural polymer composite fibre medical wound dressing
Preparation method, belong to medical dressing manufacturing field.
Background technology
More than 300 kinds of Medical dressing high-end at present, can substantially be divided into four major classes：High-end moist dressing
(mainly including foam, hydrocolloid, hyaline membrane, hydrogel, seaweeds, aquation fiber), antiseptic dressing are (main to include silver system, zinc
System, iodine system, natural products addition system, antimicrobial macromolecule system, antibiosis prime system), vacuum closure Wound healing and bone regeneration VAC and nanofiber
Dressing.However, the high-end bio-medical dressing market in the whole world is mainly occupied by 30 many enterprises in Europe and the U.S. at present, such as
3M, AcryMed, Kendall Healthcare etc., these Products are dispersed throughout Chinese market substantially, and expensive.And
For domestic enterprise, such as Shenzhen Aomei is medical, sane medical treatment, Shaoxing shake moral medical dressing enterprise, its major product is still to pass
System dressing.At present, growth stage relatively short high-end dressing：Nanofiber dressing, have begun to by domestic and international correlative study
Person and the extensive concern of enterpriser.However, foreign countries have begun to nanofiber industrialization, scale, and use it for producing
High-end Wound care, skin regeneration and the bio-medical dressing with targeted drug release function.And occur being based primarily upon glue
Former protide relevant market product (such as Integra TM, Nanacell TM,Deng), and China's independent research
Nanofiber class wound dressing species is less.
Because it possesses the structure of similar cell epimatrix and component, its fibre fractionation can design nanofiber, size with
Controlled porosity.In addition, can be by artificially adding the factor, such as antibacterial needed for wound reparation in the preparation process of nanofiber
The factor, growth factor etc., so as to obtain promoting the functional nano fiber of wound reparation.According at present on nanometer dressing base
Plinth research report, natural albumen macromolecule (such as collagen, gelatin) and polysaccharide polymer (such as alginates, glucan
Deng) synthesis macromolecule relatively more enjoys favor, but for enhancing its mechanical strength, spinning property or blocked water for part researcher
Performance etc., partially synthetic macromolecule (such as polyurethane, polycaprolactone, polyethylene glycol) are also usually used.Electrostatic spinning is one
Kind prepares the simple and effective processing technology of polymer superfine fibre.Its principle is polymer melt or solution in high-voltage electrostatic field
Effect is lower to form " Taylor " cone, and when electric-field intensity is sufficiently large, polymer drop overcomes the formation injection of its own face tension force to penetrate
Stream, pass through splitting, stretching, solidification or solvent volatilization in the air, ultimately form the process of fibrous material.(Formhas
A.U.S.Patent No.1,975,504,1934.) the obtained fibre diameter of traditional spining technology generally 10~500 μm it
Between, and fiber prepared by electrostatic spinning technique is then thin more, fibre diameter typically arrives thousands of nanometers tens of.In addition, by quiet
The advantages that fiber that Electrospinning obtains also has great specific surface area, and porosity is high, make it in filtering, catalysis, biology
The fields such as medical science have a wide range of applications.(Bhardwaj N,et al.Biotechnology advances,2010,28(3):
325-347.)。
The natural polysaccharides such as glucan, konjaku glucomannan, inulin and gelatin, hyaluronic acid, chitosan, sodium alginate, carboxylic
The natural polymer natural reproducible such as methylcellulose, it is cheap and easy to get, it is safe and non-toxic, it is small to human body skin stimulation, have excellent
Biocompatibility and biodegradability, can promote wound healing, improve the power of regeneration of damaged skin cell.Also have aobvious
The anti-inflammatory of work, antiallergic activity, and can help to skin and resist exogenous various mechanically and chemically stimulate.
For medical dressing in place of using above having inconvenience, some dressing uses nondegradable material as branch at present
Frame, cause iatrogenic pollution；Meanwhile dressing absorbs the surface of a wound and oozes out night while sticked together with the surface of a wound, is damaged when causing to remove new
Raw tissue, great pain is brought to patient.And medical dressing made of nano fibrous membrane is advantageous to the steaming of wound fluid
Hair, be advantageous to oxygen transmission, the growth and regeneration of wound tissue be also beneficial to, so as to accelerate the healing of wound due to skin group
The bio-diversity and complexity knitted.In addition, the dressing of single component far can not meet that skin histology repairs demand, therefore urgently
A kind of dressing prepared using composite to be developed, to meet related needs.
The content of the invention
It is an object of the invention to provide a kind of natural polysaccharide of safety and environmental protection and good biocompatibility derivative/natural polymer
Sub- composite fibre medical wound dressing, it can stop blooding and promote wound healing, improve the power of regeneration of damaged skin cell；Again can be with
Anti-inflammatory, antiallergy, reduce wound infection.
In order to achieve the above object, the present invention adopts the following technical scheme that：
1) preparation of modified natural polysaccharide derivates：In the case where 60~85 DEG C of nitrogen are protected, by natural polysaccharide in 5~8wt%
It is completely dissolved in LiCl/DMF solution, solution temperature is down to 40~55 DEG C, is added pyridine and stir 20~40min, add first
Base acrylic anhydride carries out 5~24h of esterification, is cooled to room temperature；Then through precipitating, centrifuging, being dried in vacuo and obtain modified natural
Polysaccharide derivates.
2) preparation of Electrospun solution：Modified natural polysaccharide derivates, natural polymer, light trigger are pressed into certain matter
It is soluble in water to measure percentage, is sufficiently stirred, so that being completely dissolved, bubble is all separated out 1~2h of solution left standstill ultrasound
Obtain the Electrospun solution of transparent and homogeneous.
3) preparation of composite fibre：The Electrospun solution prepared in step 2) is used into multi-nozzle electrospinning device, led to
The condition for crossing adjustment electrostatic spinning carries out large area electrospinning, you can obtains composite fibre.
4) photo-crosslinking of composite fibre：Electrospinning composite fibre is irradiated to the crosslinking for carrying out positive and negative two sides under uviol lamp, obtained
There is the composite fibre of some strength after to crosslinking.
5) preparation of medical wound dressing：Composite fibre after crosslinking is subjected to the gamma ray radiation sterilization of cobalt -60,
Natural polysaccharide derivative/natural polymer composite fibre medical wound dressing is obtained by cutting, packing.Specifically, it is described
Natural polysaccharide is one kind in glucan, synanthrin, konjaku glucomannan；Described natural polymer is gelatin, hyaluronic acid, shell
One kind in glycan, sodium alginate, carboxymethyl cellulose.Specifically, in described medical wound dressing each component quality hundred
Divide than content and be：Modified natural polysaccharide derivates：10~30%；Natural polymer：10~40%；Light trigger：0.05%~
0.1%, surplus is water.
Specifically, the mass ratio of described modified natural polysaccharide derivates and natural polymer is 1:1~1:4.
Specifically, described light trigger be Quantacure BTC, Quantacure ABP, Quantacure BPQ,
One kind in Quantacure QTX, Darocur 2959.
Specifically, described electrospinning device is multiple spray head static spinning machine；Described spinning condition is：Spinning voltage
15~25kV, it is 10~20cm to receive distance, and spinning speed is 0.1~1.5mL/h, and shower nozzle internal diameter is 0.6mm；
Specifically, described uv light irradiation condition is：The light intensity of uviol lamp is 100~400mW/cm2, auxiliary range from for
5~10cm, the auxiliary photograph time is 1~5h.
Specifically, the time of the described gamma ray radiation sterilization of cobalt -60 is 5~8h, the gamma spoke that cobalt -60 is launched
L.33 million electro-volt energy is penetrated as 1.17 and.
The present invention has advantages below：
1) natural polysaccharide and natural polymer of the present invention, natural reproducible is cheap and easy to get, safe and non-toxic, right
Human body skin stimulation is small, has excellent biocompatibility and biodegradability, can promote wound healing, improves damaged skin
The power of regeneration of cell.Also there is significant anti-inflammatory, antiallergic activity, and can help to skin and resist exogenous various machineries
And chemical stimulation.
2) present invention uses multiple spray head static spinning machine, simple to operate, can large area electrospinning, efficiency high；Prepared
Pulp freeness is big, and porosity is high, is advantageous to oxygen transmission, the growth and regeneration of wound tissue is also beneficial to, so as to add
The healing of fast wound is due to the bio-diversity and complexity of skin histology.
3) present invention use UV-curing technology, polymerization speed, consume energy less, environmental pollution is small, at room temperature
Operation.
4) present invention is by the way that the fiber wound dressing of modified natural polysaccharide derivates and the compound preparation of natural polymer is given birth to
Produce low cost, good permeability, intensity controlled, safety and environmental protection.
Brief description of the drawings
Fig. 1 is the scanning of natural polysaccharide derivative/natural polymer composite fibre medical wound dressing prepared by embodiment 1
Electron microscope.
Fig. 2 is outer the taking into consideration of the natural polysaccharide derivative/natural polymer composite fibre medical wound dressing actually prepared
Piece.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be pointed out that these embodiments are merely to illustrate this hair
Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after present disclosure has been read, those skilled in the art
Some improvement or retouching can be made to the present invention, these are improved or retouching also should be regarded as protection scope of the present invention.
Embodiment 1
1) in the case where 85 DEG C of nitrogen are protected, the LiCl/DMF that 3.0g glucans (molecular weight 40,000) are dissolved in 8wt% is molten
In liquid, until completely dissolved, solution temperature is down to 55 DEG C, adds 5.6g pyridines, stirs 40min, 8.6g methyl-props are added dropwise
Olefin(e) acid acid anhydride, 5h is reacted, reaction is down to room temperature after terminating, precipitated in cold isopropanol, and by centrifugation, vacuum drying is modified
Glucan derivative.
2) modified glucan derivative obtained in 0.5g steps 1) is taken, 0.5g gelatin, 2g deionized waters, 1.1 × 10-3g
Darocur 2959, magnetic agitation is fully carried out at 40 DEG C, bubble is all separated out 1~2h of solution left standstill ultrasound can obtain
To the Electrospun solution of transparent and homogeneous.
3) the Electrospun solution prepared in step 2) is taken, large area electrospinning is carried out using multiple spray head static spinning machine, obtained
To glucan derivative and the composite fibre of gelatin.Spinning condition is：Temperature is 40 DEG C, voltage 25kV, and injection speed is
1.5mL/h, it is 10cm to receive distance.
4) electrospun fiber membrane obtained in step 3) is placed on away from uviol lamp (light intensity 400mW/cm2) irradiation 5h enters at 10cm
The photo-crosslinking on the positive and negative two sides of row, by the gamma ray radiation sterilization 8h of cobalt -60, cutting, packing obtain glucan derivative
Thing/gelatin composite nanofibers medical wound dressing.
Embodiment 2
1) in the case where 60 DEG C of nitrogen are protected, 3.0g konjaku glucomannans (molecular weight 200,000) are dissolved in 6wt%'s
In LiCl/DMF, until completely dissolved, solution temperature is down to 40 DEG C, adds 8.5g pyridines, stirs 20min, is added dropwise 13.0
Methacrylic anhydride, 24h is reacted, reaction is down to room temperature after terminating, precipitated in cold isopropanol, by centrifugation, vacuum drying
Obtain modified konjak portuguese gansu polyose sugar derivatives.
2) the modified konjac glucomannan derivative obtained in 0.2g steps 1), 0.8g hyaluronic acids, 3.0g deionizations are taken
Water, 5.5 × 10-4G Darocur 2959, magnetic agitation is fully carried out at 40 DEG C, 1~2h of solution left standstill ultrasound is made into bubble
All separate out the Electrospun solution that can obtain transparent and homogeneous.
3) the Electrospun solution prepared in step 2) is taken, large area electrospinning is carried out using multiple spray head static spinning machine, obtained
To konjak portuguese gansu polyose sugar derivatives and the composite fibre of hyaluronic acid.Spinning condition is：Temperature is 40 DEG C, voltage 25kV, note
Firing rate degree is 0.5mL/h, and it is 10cm to receive distance.
4) electrospun fiber membrane obtained in step 3) is placed on away from uviol lamp (light intensity 400mW/cm2) irradiation 5h enters at 10cm
The photo-crosslinking on the positive and negative two sides of row, by the gamma ray radiation sterilization 8h of cobalt -60, cutting, packing obtain konjaku glucomannan
Derivative/hyaluronic acid composite fibre medical wound dressing.
Embodiment 3
1) in the case where 70 DEG C of nitrogen are protected, 3.0g synanthrin (molecular weight 6,200) is dissolved in 5wt% LiCl/DMF, treated
After being completely dissolved, solution temperature is down to 40 DEG C, adds 5.6g pyridines, stirs 30min, 8.6g methacrylic anhydrides are added dropwise,
12h is reacted, reaction is down to room temperature after terminating, precipitated in cold isopropanol, and by centrifugation, vacuum drying obtains modified synanthrin
Derivative.
2) the modification synanthrin derivative obtained in 0.4g steps 1) is taken, 0.6g carboxymethyl celluloses, 3g deionized waters, 1.1
×10-3G Quantacure QTX, magnetic agitation is fully carried out at 40 DEG C, make bubble whole 1~2h of solution left standstill ultrasound
Separate out the Electrospun solution that can obtain transparent and homogeneous.
3) the Electrospun solution prepared in step 2) is taken, large area electrospinning is carried out using multiple spray head static spinning machine, obtained
To synanthrin derivative and the composite fibre of carboxymethyl cellulose.Spinning condition is：Temperature is 40 DEG C, voltage 15kV, injection speed
Spend for 0.1mL/h, it is 20cm to receive distance.
4) electrospun fiber membrane obtained in step 3) is placed on away from uviol lamp (light intensity 100mW/cm2) irradiation 1h enters at 5cm
The photo-crosslinking on the positive and negative two sides of row, by the gamma ray radiation sterilization 5h of cobalt -60, cutting, packing obtain synanthrin derivative/
Carboxymethyl cellulose composite fibre medical wound dressing.
Embodiment 4
1) in the case where 85 DEG C of nitrogen are protected, the LiCl/DMF that 3.0g glucans (molecular weight 20,000) are dissolved in 8wt% is molten
In liquid, until completely dissolved, solution temperature is down to 55 DEG C, adds 8.5g pyridines, stirs 30min, 13.0g methyl-props are added dropwise
Olefin(e) acid acid anhydride, 5h is reacted, reaction is down to room temperature after terminating, precipitated in cold isopropanol, and by centrifugation, vacuum drying is modified
Glucan derivative.
2) modified glucan derivative obtained in 0.4g steps 1) is taken, 0.6g sodium alginates, 2g deionized waters, 1.1 ×
10-3G Quantacure BTC, magnetic agitation is fully carried out at 40 DEG C, bubble is all analysed 1~2h of solution left standstill ultrasound
Go out to can obtain the Electrospun solution of transparent and homogeneous.
3) the Electrospun solution prepared in step 2) is taken, large area electrospinning is carried out using multiple spray head static spinning machine, obtained
To glucan derivative and the composite fibre of sodium alginate.Spinning condition is：Temperature is 40 DEG C, voltage 25kV, injection speed
For 1.5mL/h, it is 10cm to receive distance.
4) electrospun fiber membrane obtained in step 3) is placed on away from uviol lamp (light intensity 400mW/cm2) irradiation 5h enters at 10cm
The photo-crosslinking on the positive and negative two sides of row, by the gamma ray radiation sterilization 8h of cobalt -60, cutting, packing obtain glucan derivative
Thing/sodium alginate composite fiber medical wound dressing.
Embodiment 5
1) in the case where 60 DEG C of nitrogen are protected, 3.0g konjaku glucomannans (molecular weight 400,000) are dissolved in 6wt%'s
In LiCl/DMF, until completely dissolved, solution temperature is down to 40 DEG C, adds 5.6g pyridines, stirs 30min, 8.6 first are added dropwise
Base acrylic anhydride, reacts 24h, and reaction is down to room temperature after terminating, precipitates in cold isopropanol, by centrifugation, be dried in vacuo
To modified konjak portuguese gansu polyose sugar derivatives.
2) the modified konjac glucomannan derivative obtained in 0.3g steps 1) is taken, 0.7g gelatin, 3.0g deionized waters,
1.1×10-3G Quantacure BPQ, magnetic agitation is fully carried out at 40 DEG C, makes bubble complete 1~2h of solution left standstill ultrasound
Portion separates out the Electrospun solution that can obtain transparent and homogeneous.
3) the Electrospun solution prepared in step 2) is taken, large area electrospinning is carried out using multiple spray head static spinning machine, obtained
To konjak portuguese gansu polyose sugar derivatives and the composite fibre of gelatin.Spinning condition is：Temperature is 40 DEG C, voltage 20kV, injection speed
Spend for 1.0mL/h, it is 15cm to receive distance.
4) electrospun fiber membrane obtained in step 3) is placed on away from uviol lamp (light intensity 200mW/cm2) irradiation 2h enters at 8cm
The photo-crosslinking on the positive and negative two sides of row, by the gamma ray radiation sterilization 6h of cobalt -60, cutting, packing obtain konjaku glucomannan
Derivative/gelatin composite nanofibers medical wound dressing.
Embodiment 6
1) in the case where 65 DEG C of nitrogen are protected, 3.0g synanthrin (molecular weight 6,200) is dissolved in 5wt% LiCl/DMF, treated
After being completely dissolved, solution temperature is down to 40 DEG C, adds 11.3g pyridines, stirs 30min, 17.2g methacrylic acids are added dropwise
Acid anhydride, 10h is reacted, reaction is down to room temperature after terminating, precipitated in cold isopropanol, and by centrifugation, vacuum drying obtains modification
Synanthrin derivative.
2) the modification synanthrin derivative obtained in 0.5g steps 1) is taken, 0.5g hyaluronic acids, 3g deionized waters, 1.1 × 10- 3G Quantacure ABP, magnetic agitation is fully carried out at 40 DEG C, bubble is all separated out 1~2h of solution left standstill ultrasound
It can obtain the Electrospun solution of transparent and homogeneous.
3) the Electrospun solution prepared in step 2) is taken, large area electrospinning is carried out using multiple spray head static spinning machine, obtained
To synanthrin derivative and the composite fibre of hyaluronic acid.Spinning condition is：Temperature is 40 DEG C, voltage 18kV, and injection speed is
0.5mL/h, it is 12cm to receive distance.
4) electrospun fiber membrane obtained in step 3) is placed on away from uviol lamp (light intensity 400mW/cm2) irradiation 3h enters at 6cm
The photo-crosslinking on the positive and negative two sides of row, by the gamma ray radiation sterilization 8h of cobalt -60, cutting, packing obtain synanthrin derivative/
Hyaluronic acid composite fibre medical wound dressing.
Claims (6)
1. the preparation method of natural polysaccharide derivative/natural polymer composite fibre medical wound dressing, it is characterised in that to day
Right polysaccharide carries out chemical modification, obtains modified natural polysaccharide derivative；Then by itself and natural polymer Combined Mining electrostatic
Spining technology prepares fiber, and composite fibre is irradiated under uviol lamp and crosslinked；The sterilization of the gamma ray radiation of cobalt -60 is carried out again
Sterilizing, cutting, packaging can obtain natural polysaccharide derivative/natural polymer composite fibre medical wound dressing；Specifically include
Following steps：
1) preparation of modified natural polysaccharide derivates：In the case where 60~85 DEG C of nitrogen are protected, by natural polysaccharide in 5~8wt%LiCl/
It is completely dissolved in DMF solution, solution temperature is down to 40~55 DEG C, is added pyridine and stir 20~40min, add metering system
Acid anhydrides carries out 5~24h of esterification, is cooled to room temperature；Then through precipitating, centrifuging, being dried in vacuo and obtain modified natural polysaccharide and spread out
Biology；
2) preparation of Electrospun solution：Modified natural polysaccharide derivates, natural polymer, light trigger are pressed into certain quality hundred
Point than soluble in water, it is sufficiently stirred, so that being completely dissolved, bubble is all separated out 1~2h of solution left standstill ultrasound and can obtain
The Electrospun solution of transparent and homogeneous；
3) preparation of composite fibre：The Electrospun solution prepared in step 2) is used into multi-nozzle electrospinning device, passes through tune
The condition of whole electrostatic spinning carries out large area electrospinning, you can obtains composite fibre；
4) photo-crosslinking of composite fibre：Electrospinning composite fibre is irradiated to the crosslinking for carrying out positive and negative two sides under uviol lamp, handed over
There is the composite fibre of some strength after connection；
5) preparation of medical wound dressing：Composite fibre after crosslinking is subjected to the gamma ray radiation sterilization of cobalt -60, by
Cutting, packing obtain natural polysaccharide derivative/natural polymer composite fibre medical wound dressing.
2. preparation method according to claim 1, it is characterised in that 1), 2) described in natural polysaccharide for glucan, synanthrin, konjaku
One kind in Glucomannan；Described natural polymer is one in gelatin, hyaluronic acid, sodium alginate, carboxymethyl cellulose
Kind；Described light trigger is Quantacure BTC, Quantacure ABP, Quantacure BPQ, Quantacure
One kind in QTX, Darocur 2959.
3. preparation method according to claim 1, it is characterised in that the mass percentage content of each component described in 2) is：It is modified
Natural polysaccharide derivative：10~30%；Natural polymer：10~40%；Light trigger：0.05%~0.1%；Surplus is water；
Wherein the mass ratio of modified natural polysaccharide derivates and natural polymer is 1:1~1:4.
4. preparation method according to claim 1, it is characterised in that the electrospinning device described in 3) is multi-nozzle electrospinning
Machine；Described spinning condition is：15~25kV of spinning voltage, it is 10~20cm to receive distance, and spinning speed is 0.1~1.5mL/
H, shower nozzle internal diameter are 0.6mm.
5. preparation method according to claim 1, it is characterised in that the uv light irradiation condition described in 4) is：The light intensity of uviol lamp
For 100~400mW/cm2, for auxiliary range from for 5~10cm, auxiliary according to the time is 1~5h.
6. preparation method according to claim 1, it is characterised in that the gamma ray radiation sterilization of cobalt -60 described in 5) when
Between be 5~8h, l.33 million electro-volt the gamma radiation energy that cobalt -60 is launched is 1.17 and.
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| CN113214503B (en) * | 2021-04-13 | 2022-06-10 | 北京科技大学 | Preparation and application of amino acid-based polyurethane supermolecule high-viscosity gel patch |
| CN113730640A (en) * | 2021-09-17 | 2021-12-03 | 苏州永沁泉智能设备有限公司 | Sponge dressing capable of being crosslinked in situ and preparation method thereof |
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