CN104069536B - A kind of preparation method preparing sodium alginate-chitosan nanoscale medical dressing - Google Patents

A kind of preparation method preparing sodium alginate-chitosan nanoscale medical dressing Download PDF

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CN104069536B
CN104069536B CN201410332254.3A CN201410332254A CN104069536B CN 104069536 B CN104069536 B CN 104069536B CN 201410332254 A CN201410332254 A CN 201410332254A CN 104069536 B CN104069536 B CN 104069536B
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sodium alginate
solution
chitosan
spinning
linking agent
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CN201410332254.3A
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CN104069536A (en
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孙开源
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江苏开源康达医疗器械有限公司
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Abstract

The present invention relates to a kind of preparation method preparing sodium alginate-chitosan nanoscale medical dressing and belong to native biopolymer Material Field.Step of the present invention: sodium alginate and synthetic polymer are scattered in alcoholic solution, the chitosan solution of preparation containing cross-linking agent is as receiving liquid, when sodium alginate fiber is received after in chitosan solution, it is crosslinked that cross-linking agent makes fiber occur, and the electrolyte attribute of chitosan makes it be adsorbed in sodium alginate fiber surface by electrostatic interaction, the sodium alginate-chitosan composite nano fiber obtained has good breathability and antibacterial anti hemorrhagic effect, use it for growth and regeneration that wound dressing is conducive to wound tissue, can the healing of accelerated in wounds.The method adopts natural polymer subbase to be raw material, and cost is low, nontoxic, good biocompatibility.

Description

A kind of preparation method preparing sodium alginate-chitosan nanoscale medical dressing

Technical field

The invention belongs to native biopolymer field of material technology, relate to a kind of preparation method preparing sodium alginate-chitosan nanoscale medical dressing

Technical background

Chitosan (Chitosan, CS) be a kind of abundant natural alkaline polysaccharide, at nature warp inferior to cellulosic second largest living resources, there is good biocompatibility, biodegradability, human body affinity and antibacterial, hemostasis and promote the excellent properties such as wound healing, can absorbed themselves after using, do not cause allergy, can also accelerating wound healing, there is protective effect to large-area burns, can skin regeneration be promoted; With the medical adhesive-bonded fabric that it is produced, can use in burn wound and skin donor site, not only play the effect of covering, protection wound surface, and antigenicity be low.Therefore, chitin biodressing is more and more being subject to people's attention in recent years, and applies in bio-medical field as artificial skin, operation suture thread.

Alginate (Alginate) is a kind of naturally occurring high molecular polymer, its quantity is various, can rough segmentation be the large class of red algae, Brown algae, chlorella and cyanophyceae four by color, alginate be used in Food & Drink industry the earliest, and it can be used as stabilizing agent, thickening agent and gellant.Because it has good biocompatibility and biological degradability, therefore more and more receive the concern of people in technical field of biology.

Sodium alginate is odorless, tasteless, faint yellow unsetting powder, pluripolarity, polyhydroxy macromolecular compound, have stronger affinity with water, gelatinizing is good, adds water expanded, hygroscopicity is strong, retentiveness is good, is insoluble to organic solvent, is 6 ~ 11 good stabilities at pH, lower than 6 time form alginic acid gel, water insoluble; Viscosity is maximum when pH value is 7, but significantly declines with the rising of temperature.Containing free carboxyl in sodium alginate, character is active, has very high ion exchanging function, adds Ca in sodium alginate aqueous solution 2+, Ba 2+after bivalent cation, the Na in sodium alginate +with bivalent cation generation ion-exchange reactions, form ionomer hydrogel.

Nanofiber has very high volume-surface ratio due to it, has higher value in fields such as organizational project, drug release, medical dressing.Electrostatic spinning technique prepares nanofiber simply effective method.It is that one makes charged polymer solution or melt jet stretch in electrostatic field, prepares polymer superfine fibre method.When extra electric field reaches certain marginal value, jet will be spouting from spinning nozzle, solvent volatilization simultaneously, and jet solidifies, and forms superfine fibre.Current medical dressing has inconvenience part in use, and some dressing uses nondegradable material as timbering material, causes iatrogenic pollution; Meanwhile, dressing absorb wound fluid simultaneously and wound surface stick together, cause damage cambium when removing, bring great misery to patient.And the medical dressing that nano fibrous membrane is made is conducive to the evaporation of wound fluid, be conducive to oxygen through, be also conducive to growth and the regeneration of wound tissue, thus can the healing of accelerated in wounds, in recent years, nano fiber non-woven fabric is used for medical dressing more and more extensive.

Summary of the invention

An object of the present invention design is a kind of can be used for the receiving system receiving alginic acid sodio electricity spinning fibre;

Two of object of the present invention utilizes electrical spinning method to prepare sodium alginate chitosan composite polyelectrolyte nanofibers;

Three of object of the present invention improve a kind of can the solution formula of Quick cross-linking sodium alginate, and to receive for spinning;

Four of object of the present invention utilizes crosslinker solution crossslinked sodium alginate, obtains the composite polyelectrolyte fiber with excellent mechanical performances;

Five of object of the present invention has prepared the application of a kind of natural product based, biodegradable micro/nano fibrous membrane material as medical dressing.

Principle of the present invention: sodium alginate is due to its strand stretching, extension in aqueous, and intermolecular chain entanglement is few, and intermolecular interaction is weak, causes it to utilize Electrospinning to be difficult to form nanofiber.The present invention, by sodium alginate and synthetic polymer co-blended spinning, utilizes polymer support effect, prepares sodium alginate nano fiber; When sodium alginate nano fiber falls into homemade chitosan receiving liquid, it is crosslinked that cross-linking agent in solution makes sodium alginate nano fiber occur, because chitosan is poly-positive electrolyte, sodium alginate is poly-cloudy electrolyte, mutual electrostatic interaction between the two, make chitosan be adsorbed on sodium alginate fiber surface, successfully prepare sodium alginate-chitosan composite nano fiber.

Receiving system of the present invention: the chitosan receiving liquid containing cross-linking agent is poured in the temperature control tank with drainage screen, in spinning process, temperature control tank can be regulated to change the temperature of receiving liquid, to obtain the sodium alginate-chitosan composite nano fiber of performance the best.

The present invention is a kind of preparation method preparing sodium alginate-chitosan nanoscale medical dressing, and its concrete steps are as follows:

1) preparation of sodium alginate spinning solution: sodium alginate powder and synthetic polymer blends being dissolved in volume fraction is in the ethanol water of 10% ~ 50%, be made into the solution that percentage by weight is 3 ~ 12wt%, then solution is fully stirred, so that dissolve completely, within 1 ~ 2 hour, make bubble all separate out solution left standstill ultrasound wave and namely obtain transparent sodium alginate Electrospun solution.

2) chitosan receives solution preparation: Chitosan powder being dissolved in volume fraction is in 1% ~ 3% acetic acid solution, be made into the solution that weight ratio is 4 ~ 10wt%, add cross-linking agent wherein, the content of cross-linking agent is 5 ~ 15wt%, stir, to dissolving completely, within 1 ~ 2 hour, making bubble all separate out solution left standstill ultrasound wave and namely obtaining transparent chitosan reception solution;

3) fiber preparation process: by step 1) in preparation sodium alginate spinning solution add (Fig. 1) in solution supplying device, adjustment voltage is 15 ~ 30kV; Spinning head is 15 ~ 20cm to the distance of receiving system, and described receiving system includes the temperature control tank with drainage screen, has the chitosan receiving liquid containing cross-linking agent in described temperature control tank; The flow of spinning head spinning solution is 0.5 ~ 2.0mL/h; Spinning temperature is 25 DEG C; Starting drive carries out electrostatic spinning, and at certain reception temperature, cross-linking agents sodium alginate nano fiber, chitosan is adsorbed onto sodium alginate fiber surface by electrostatic interaction, successfully obtains sodium alginate-chitosan composite nano fiber.

Step 1) described in synthetic polymer be polyethylene oxide (PEO), polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), polycaprolactone (PCL); Wherein the mass ratio of sodium alginate and synthetic polymer is 3: 7 ~ 7: 3;

Step 2) described in cross-linking agent be CaCl 2, MgCl 2, BaCl 2, glutaraldehyde, genipin, divinylsulfone, carbodiimides, one or more in sodium tripolyphosphate.

The advantage of the inventive method:

1) sodium alginate nano fiber has good intensity and water-retaining property after crosslinked;

2) the sodium alginate-chitosan composite nano fiber prepared has good antibacterial anti hemorrhagic effect, and good breathability can make it as wound dressing, is conducive to growth and the regeneration of wound tissue, can the healing of accelerated in wounds;

3) adopt natural polymer subbase to be raw material, cost is low, nontoxic, and cell compatibility is good.

Accompanying drawing explanation

Fig. 1 is the device schematic diagram that the present invention uses;

Fig. 2 is that the present invention prepares the scanning electron microscopic picture of gained fiber by embodiment 1;

Fig. 3 is that the present invention prepares the scanning electron microscopic picture of gained fiber by embodiment 2;

Detailed description of the invention

Embodiment 1

(1) dose volume mark is the aqueous solution of the ethanol of 20%; Dose volume mark is the second aqueous acid of 1%

(2) be distributed in the alcoholic solution of 20% at 3: 7 in mass ratio by sodium alginate and polyethylene oxide, solution concentration is 4wt%, then solution is fully stirred, so that dissolve completely, within 1 ~ 2 hour, make bubble all separate out solution left standstill ultrasound wave and namely obtain transparent sodium alginate Electrospun solution.

(3) be 5 × 10 by molecular weight 4the Chitosan powder of g/mol is distributed in the acetic acid solution of 1%, and solution concentration is 5wt%, in solution, add CaCl 2as cross-linking agent, concentration is 5%, stirs, so that dissolves completely, within 1 ~ 2 hour, makes bubble all separate out solution left standstill ultrasound wave and namely obtains transparent chitosan reception solution;

(4) add in solution supplying device by the sodium alginate spinning solution prepared, adjustment voltage is 20kV; Spinning head is 15cm to the distance of receiving system, and receiving system includes the temperature control tank with drainage screen, has the chitosan receiving liquid containing cross-linking agent in temperature control tank; The flow of spinning head spinning solution is 0.5mL/h; Spinning temperature is 25 DEG C; Receiving system temperature is 25 DEG C.Starting drive carries out electrostatic spinning, obtains sodium alginate-chitosan composite nano fiber in receiving system.By dry for fiber vacuum 24h, so that fully except desolventizing, the nanofiber of acquisition can use as wound dressing, and this fiber has good breathability, antibacterial anti hemorrhagic, is conducive to growth and the regeneration of wound tissue, can the healing of accelerated in wounds.

Embodiment 2

(1) dose volume mark is the aqueous solution of the ethanol of 20%; Dose volume mark is the second aqueous acid of 2%

(2) be distributed in the alcoholic solution of 20% at 3: 7 in mass ratio by sodium alginate and polyethylene oxide, solution concentration is 4wt%, then solution is fully stirred, so that dissolve completely, within 1 ~ 2 hour, make bubble all separate out solution left standstill ultrasound wave and namely obtain transparent sodium alginate Electrospun solution.

(3) be 1.0 × 10 by molecular weight 5the Chitosan powder of g/mol is distributed in the acetic acid solution of 2%, and solution concentration is 5wt%, in solution, add CaCl 2as cross-linking agent, concentration is 5%, stirs, so that dissolves completely, within 1 ~ 2 hour, makes bubble all separate out solution left standstill ultrasound wave and namely obtains transparent chitosan reception solution;

(4) add in solution supplying device by the sodium alginate spinning solution prepared, adjustment voltage is 20kV; Spinning head is 15cm to the distance of receiving system, and receiving system includes the temperature control tank with drainage screen, has the chitosan receiving liquid containing cross-linking agent in temperature control tank; The flow of spinning head spinning solution is 0.5mL/h; Spinning temperature is 25 DEG C; Receiving system temperature is 30 DEG C.Starting drive carries out electrostatic spinning, obtains sodium alginate-chitosan composite nano fiber in receiving system.By dry for fiber vacuum 24h, so that fully except desolventizing, the nanofiber of acquisition can use as wound dressing, and this fiber has good breathability, antibacterial anti hemorrhagic, is conducive to growth and the regeneration of wound tissue, can the healing of accelerated in wounds.

Embodiment 3

(1) dose volume mark is the aqueous solution of the ethanol of 30%; Dose volume mark is the second aqueous acid of 2%

(2) be distributed in the alcoholic solution of 30% at 4: 6 in mass ratio by sodium alginate and polyethylene oxide, solution concentration is 4wt%, then solution is fully stirred, so that dissolve completely, within 1 ~ 2 hour, make bubble all separate out solution left standstill ultrasound wave and namely obtain transparent sodium alginate Electrospun solution.

(3) be 1.0 × 10 by molecular weight 5the Chitosan powder of g/mol is distributed in the acetic acid solution of 2%, and solution concentration is 5wt%, in solution, add MgCl 2as cross-linking agent, concentration is 10%, stirs, so that dissolves completely, within 1 ~ 2 hour, makes bubble all separate out solution left standstill ultrasound wave and namely obtains transparent chitosan reception solution;

(4) add in solution supplying device by the sodium alginate spinning solution prepared, adjustment voltage is 25kV; Spinning head is 15cm to the distance of receiving system, and receiving system includes the temperature control tank with drainage screen, has the chitosan receiving liquid containing cross-linking agent in temperature control tank; The flow of spinning head spinning solution is 0.5mL/h; Spinning temperature is 25 DEG C; Receiving system temperature is 25 DEG C.Starting drive carries out electrostatic spinning, obtains sodium alginate-chitosan composite nano fiber in receiving system.By dry for fiber vacuum 24h, so that fully except desolventizing, the nanofiber of acquisition can use as wound dressing, and this fiber has good breathability, antibacterial anti hemorrhagic, is conducive to growth and the regeneration of wound tissue, can the healing of accelerated in wounds.

Embodiment 4

(1) dose volume mark is the aqueous solution of the ethanol of 30%; Dose volume mark is the second aqueous acid of 3%

(2) be distributed in the alcoholic solution of 30% at 4: 6 in mass ratio by sodium alginate and polyethylene oxide, solution concentration is 4wt%, then solution is fully stirred, so that dissolve completely, within 1 ~ 2 hour, make bubble all separate out solution left standstill ultrasound wave and namely obtain transparent sodium alginate Electrospun solution.

(3) be 2.0 × 10 by molecular weight 5the Chitosan powder of g/mol is distributed in the acetic acid solution of 2%, and solution concentration is 5wt%, in solution, add MgCl 2as cross-linking agent, concentration is 10%, stirs, so that dissolves completely, within 1 ~ 2 hour, makes bubble all separate out solution left standstill ultrasound wave and namely obtains transparent chitosan reception solution;

(4) add in solution supplying device by the sodium alginate spinning solution prepared, adjustment voltage is 25kV; Spinning head is 15cm to the distance of receiving system, and receiving system includes the temperature control tank with drainage screen, has the chitosan receiving liquid containing cross-linking agent in temperature control tank; The flow of spinning head spinning solution is 0.5mL/h; Spinning temperature is 25 DEG C; Receiving system temperature is 25 DEG C.Starting drive carries out electrostatic spinning, obtains sodium alginate-chitosan composite nano fiber in receiving system.By dry for fiber vacuum 24h, so that fully except desolventizing, the nanofiber of acquisition can use as wound dressing, and this fiber has good breathability, antibacterial anti hemorrhagic, is conducive to growth and the regeneration of wound tissue, can the healing of accelerated in wounds.

Claims (5)

1. prepare a preparation method for sodium alginate-chitosan nanoscale medical dressing, it is characterized in that comprising the following steps:
(1) preparation of sodium alginate spinning solution: sodium alginate powder and synthetic polymer blends being dissolved in volume fraction is in the ethanol water of 10% ~ 50%, be made into the solution that percentage by weight is 3 ~ 12wt%, then solution is fully stirred, so that dissolve completely, by ultrasonic for solution 1 ~ 2 hour, bubble is all separated out and namely obtain transparent sodium alginate Electrospun solution;
(2) chitosan receives solution preparation: Chitosan powder being dissolved in volume fraction is in 1% ~ 3% acetic acid solution, be made into the solution that weight ratio is 4 ~ 10wt%, add cross-linking agent wherein, stir, to dissolving completely, within 1 ~ 2 hour, making bubble all separate out solution left standstill ultrasound wave and namely obtaining transparent chitosan reception solution;
(3) fiber preparation process: add in solution supplying device by the sodium alginate spinning solution of preparation in step (1), adjustment voltage is 15 ~ 30kV; Spinning head is 15 ~ 20cm to the distance of receiving system, and described receiving system includes the temperature control tank with drainage screen, has the chitosan receiving liquid containing cross-linking agent in described temperature control tank; The flow of spinning head spinning solution is 0.5 ~ 2.0mL/h; Spinning temperature is 25 DEG C; Starting drive carries out electrostatic spinning, and at certain reception temperature, cross-linking agents sodium alginate nano fiber, chitosan is adsorbed onto sodium alginate fiber surface by electrostatic interaction, obtains sodium alginate-chitosan composite nano fiber.
2. method according to claim 1, it is characterized in that, in step (1), synthetic polymer is polyethylene oxide (PEO), polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), polycaprolactone (PCL); Wherein the mass ratio of sodium alginate and synthetic polymer is 3: 7 ~ 7: 3.
3. method according to claim 1, is characterized in that, in step (2), the molecular weight of chitosan is 5 × 10 4~ 2.5 × 10 5g/mol, deacetylation is>=90%.
4. method according to claim 1, is characterized in that, in step (2), cross-linking agent is CaCl 2, MgCl 2, BaCl 2, glutaraldehyde, genipin, divinylsulfone, carbodiimides, one or more in sodium tripolyphosphate, the content of cross-linking agent is 5 ~ 15wt%.
5. method according to claim 1, is characterized in that, in step (3), the temperature of receiving device is 25 ~ 60 DEG C.
CN201410332254.3A 2014-07-11 2014-07-11 A kind of preparation method preparing sodium alginate-chitosan nanoscale medical dressing CN104069536B (en)

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