CN114887108B - Preparation method of sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with gradient pore structure - Google Patents
Preparation method of sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with gradient pore structure Download PDFInfo
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- CN114887108B CN114887108B CN202210380231.4A CN202210380231A CN114887108B CN 114887108 B CN114887108 B CN 114887108B CN 202210380231 A CN202210380231 A CN 202210380231A CN 114887108 B CN114887108 B CN 114887108B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/425—Porous materials, e.g. foams or sponges
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/28—Polysaccharides or their derivatives
Abstract
The invention belongs to the technical engineering field of biological medical use, and relates to a preparation method of a sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with a gradient pore structure, which comprises the following steps: preparing a mixed solution of sodium alginate and chitosan quaternary ammonium salt; preventing the sodium alginate and the chitosan quaternary ammonium salt from forming precipitate by adopting chloride salt; adding calcium carbonate nucleating agents with different particle sizes; lyophilizing the solution to obtain a solid dressing; washing the solid sample by using the ethanol-acid mixed solution, preparing a gradient hole and generating a secondary crosslinking reaction; finally, washing the sample by absolute ethyl alcohol and freeze-drying to obtain the sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with the gradient pore structure. The dressing prepared by the invention has excellent antibacterial, hemostatic, imbibing and biocompatible capacities, and has good application prospect in the field of biomedical engineering.
Description
Technical Field
The invention relates to the field of biomedical technical engineering, in particular to a preparation method of a sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with a gradient pore structure.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The dressing is used as the most common nursing article when the skin is damaged, and the use amount of the dressing in daily life is huge. Due to the particularity of the dressing as a medical article, the waste treatment process is very complicated. At present, the main treatment means of the waste medical materials are sanitary landfill and high-temperature incineration. However, a considerable part of the medical dressing is prepared by non-degradable or difficultly degradable materials, and the subsequent treatment is easy to cause environmental pollution. Therefore, the use of degradable materials to make medical dressings is clearly important to create a sustainable society.
Sodium alginate and chitosan quaternary ammonium salt are used as natural polymers and derivatives thereof from the nature, are easy to degrade, have excellent bacteriostatic performance, hemostasis and healing promotion performance and biocompatibility, and are ideal matrix materials of medical dressings. However, most of the existing medical dressings prepared from single sodium alginate or chitosan quaternary ammonium salt have low strength, the medical performance cannot meet the use requirement, and the sodium alginate and the chitosan quaternary ammonium salt are very easy to generate precipitate when being blended, so that the preparation of the medical dressings is not facilitated. In addition, the medical dressing with a single pore structure has limited exudate absorption and drug slow release performance, and the medical dressing prepared by the conventional freeze-drying method has a difficult pore structure regulation and control, so that the dressing with gradient change of pores is difficult to prepare. Therefore, how to prepare the high-strength sodium alginate/chitosan quaternary ammonium salt medical dressing with a gradient pore structure by adopting a freeze-drying method is one of the key problems for improving the clinical medical effect of the conventional dressing.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the technical problem of the prior art and provides a preparation method of a sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with a gradient pore structure.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with a gradient pore structure, which comprises the following steps:
uniformly mixing a sodium alginate solution and a chitosan quaternary ammonium salt solution, adding chloride, and uniformly mixing to obtain a first mixed solution;
dispersing calcium carbonate with different particle sizes in the first mixed solution, uniformly mixing, performing ultrasonic treatment, and standing to obtain a second mixed solution;
lyophilizing the second mixed solution to obtain a crude dressing;
soaking the rough dressing in an ethanol-acid mixed solution for reaction to obtain a semi-finished dressing;
and (4) washing and freeze-drying the semi-finished dressing to obtain the dressing.
In a second aspect of the invention, the sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with the gradient pore structure prepared by the method is provided.
In a third aspect of the invention, there is provided the use of a medical dressing as described above in the field of medical hygiene.
The invention has the beneficial effects that:
(1) By adding the potassium chloride solid into the sodium alginate/chitosan quaternary ammonium salt solution, the interaction between anions in sodium alginate molecules and cations in chitosan quaternary ammonium salt is shielded, the generation of precipitates is avoided, the uniformity of the solution is ensured, the internal structure of the prepared dressing is uniform, meanwhile, the potassium chloride is very easy to dissolve in water, and the sodium alginate and the chitosan quaternary ammonium salt can be crosslinked again after being dissolved in water in the subsequent treatment;
(2) Calcium carbonate solid particles with different particle sizes are added into a sodium alginate/chitosan quaternary ammonium salt solution, and after the solution is kept stand for a period of time, under the combined action of buoyancy and gravity, the calcium carbonate with different particle sizes is distributed in different heights of the solution, so that conditions are created for subsequent freeze-drying and preparation of a gradient pore structure by pickling the calcium carbonate;
(3) Soaking the solid dressing subjected to primary freeze-drying in an ethanol-acid mixed solution, and crosslinking sodium alginate molecules by generated calcium ions while calcium carbonate and hydrogen ions react to generate pores to form primary crosslinking, wherein the porosity of the dressing is further improved by generated carbon dioxide in the overflowing process, and the shrinkage of the dressing is inhibited to a certain extent by the existence of ethanol in the solution, so that the dressing is kept in an initial shape as much as possible;
(4) In the ethanol-acid mixed solution, the chloride salt originally interacting with anions and cations of the dressing matrix is dissolved in water again, and then the anion and cation interaction between the sodium alginate and the chitosan quaternary ammonium salt is promoted, so that a secondary cross-linked network is formed inside the dressing.
(5) The operation method is simple, low in cost, universal and easy for large-scale production.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a process flow diagram of the present application;
FIG. 2 is a microscopic morphology of the sodium alginate/chitosan quaternary ammonium salt double-crosslinked medical dressing with a gradient pore structure prepared in example 1;
FIG. 3 is a graph showing the distribution of potassium ions and calcium ions before and after pickling in the dressing of example 1;
FIG. 4 is a graph showing the reduction ratio of the samples prepared in example 1 and comparative example 1 in the presence or absence of ethanol during pickling;
FIG. 5 is a comparison of the absorbance of the sample prepared in example 1 and comparative examples 2 and 3 within 20min of simulated wound exudate fetal bovine serum;
FIG. 6 is a graph showing the change in morphology of the samples prepared in example 1 and comparative examples 2 and 3 after absorption of an amount of simulated wound exudate fetal bovine serum.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
A method for preparing a sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with a gradient pore structure.
(1) Respectively dissolving sodium alginate and chitosan quaternary ammonium salt in deionized water, and fully stirring to obtain a solution of sodium alginate and chitosan quaternary ammonium salt;
(2) Mixing the sodium alginate solution obtained in the step (1) with the chitosan quaternary ammonium salt solution, adding the chloride salt solid, and fully stirring;
(3) Dispersing calcium carbonate with different particle sizes in the solution prepared in the step (2), fully stirring, performing ultrasonic treatment, and standing;
(4) Freezing the mixed solution prepared in the step (3) in liquid nitrogen and then freeze-drying;
(5) Placing the dressing obtained in the step (4) in an ethanol-acid mixed solution for soaking reaction;
(6) Washing the solid dressing obtained in the step (5) by adopting absolute ethyl alcohol;
(7) And (4) freeze-drying the dressing obtained in the step (6) again to obtain the sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with the gradient pore structure.
In some embodiments, the chitosan quaternary ammonium salt has a degree of substitution of 20% to 95%.
In some embodiments, the chloride salt solids are potassium chloride, sodium chloride, and the like.
In some embodiments, the acid is hydrochloric acid, acetic acid, or the like.
In some embodiments, the sodium alginate and chitosan quaternary ammonium salt concentration in step (1) is 1-3wt%; the stirring temperature is 40-80 ℃.
In some embodiments, the mass ratio of the sodium alginate solution to the chitosan quaternary ammonium salt solution in step (2) is 3/1 to 3/1, and the total mass ratio of the chloride salt to the sodium alginate and the chitosan quaternary ammonium salt is 3 to 10.
In some embodiments, the particle size of the calcium carbonate in the step (3) is 50-1000 meshes, the mass ratio of the calcium carbonate to the total mass of the solution is 5-20wt%, the ultrasonic defoaming time is 10-30min, and the standing time is 24-48h.
In some embodiments, the lyophilization environment in step (4) is at a pressure of 5-20pa, a temperature of- (40-60) ° c, and a lyophilization time of 36-60 hours.
In some embodiments, in the step (5), the soaking reaction time is 6-24h, and the ratio of the acid solution to the ethanol in the ethanol-acid mixed solution is 1/1 to 3/7.
In some embodiments, the number of washes with absolute ethanol in step (6) is 2 to 5;
in some embodiments, the lyophilization environment in step (7) is at a pressure of 5-20pa, a temperature of- (40-60) deg.C, and a lyophilization time of 24-48h.
The present invention is described in further detail below with reference to specific examples, which are intended to be illustrative of the invention and not limiting.
Example 1
(1) Respectively dissolving 2g of sodium alginate and chitosan quaternary ammonium salt in 98g of deionized water, and fully stirring at 50 ℃ to prepare a sodium alginate and chitosan quaternary ammonium salt solution with the concentration of 2 wt%;
(2) Mixing 20g of the sodium alginate solution obtained in the step 1 with 10g of the chitosan quaternary ammonium salt solution by stirring, adding 3g of potassium chloride solid, and fully stirring;
(3) Dispersing 0.5g of calcium carbonate with 50 meshes, 0.75g of calcium carbonate with 200 meshes and 1g of calcium carbonate with 500 meshes in the solution prepared in the step (2), fully stirring, ultrasonically removing bubbles for 20min, and standing for 24h;
(4) Freezing the mixed solution prepared in the step (3) in liquid nitrogen, and freeze-drying for 48 hours in an environment with the pressure of 10pa and the temperature of-50 ℃ to obtain a crude solid dressing;
(5) Placing the dressing obtained in the step (4) in a mixed solution of 5wt% hydrochloric acid solution and ethanol (the proportion of the hydrochloric acid solution to the ethanol solution is 2/3) to react for 12 hours;
(6) Washing the solid dressing obtained in the step (5) by using absolute ethyl alcohol for 3 times;
(7) And (4) freeze-drying the dressing obtained in the step (6) for 36 hours under the environment of pressure of 10pa and temperature of-50 ℃ to obtain the sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with the gradient pore structure.
Example 2
(1) Respectively dissolving 2g of sodium alginate and chitosan quaternary ammonium salt in 98g of deionized water, and fully stirring at 50 ℃ to prepare a sodium alginate and chitosan quaternary ammonium salt solution with the concentration of 2 wt%;
(2) Mixing 10g of the sodium alginate solution obtained in the step 1 with 10g of the chitosan quaternary ammonium salt solution by stirring, and adding 2g of sodium chloride solid by stirring fully;
(3) Dispersing 0.3g50 mesh, 0.45g200 mesh and 0.6g500 mesh calcium carbonate in the solution prepared in the step (2), fully stirring, ultrasonically treating for 20min to remove bubbles, and standing for 24h;
(4) Freezing the mixed solution prepared in the step (3) in liquid nitrogen, and freeze-drying for 48 hours in an environment with the pressure of 10pa and the temperature of-60 ℃ to obtain a rough solid dressing;
(5) Placing the dressing obtained in the step (4) in a mixed solution of 10wt% acetic acid solution and ethanol (the proportion of the two is 1/1) to react for 12 hours;
(6) Washing the solid dressing obtained in the step (5) for 3 times by adopting absolute ethyl alcohol;
(7) And (4) freeze-drying the dressing obtained in the step (6) for 36 hours under the environment of pressure of 10pa and temperature of-50 ℃ to obtain the sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with the gradient pore structure.
Example 3
(1) Respectively dissolving 3g of sodium alginate and chitosan quaternary ammonium salt in 97g of deionized water, and fully stirring at 70 ℃ to prepare a sodium alginate and chitosan quaternary ammonium salt solution with the concentration of 3wt%;
(2) Mixing 10g of the sodium alginate solution obtained in the step 1 with 20g of the chitosan quaternary ammonium salt solution by stirring, adding 5g of potassium chloride solid, and fully stirring;
(3) Dispersing 1g of calcium carbonate with 50 meshes, 1.5g200 meshes and 2g of calcium carbonate with 500 meshes in the solution prepared in the step (2), fully stirring, ultrasonically treating for 20min to remove bubbles, and standing for 24h;
(4) Freezing the mixed solution prepared in the step (3) in liquid nitrogen, and freeze-drying for 48 hours in an environment with the pressure of 10pa and the temperature of-50 ℃ to obtain a crude solid dressing;
(5) Placing the dressing obtained in the step (4) in a 7wt% hydrochloric acid solution and ethanol mixed solution (the proportion of the hydrochloric acid solution and the ethanol mixed solution is 2/3) to react for 12 hours;
(6) Washing the solid dressing obtained in the step (5) for 3 times by adopting absolute ethyl alcohol;
(7) And (4) freeze-drying the dressing obtained in the step (6) for 36 hours under the environment of pressure of 10pa and temperature of-50 ℃ to obtain the sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with the gradient pore structure.
Comparative example 1
The difference from example 1 is that only 5% hydrochloric acid solution, not ethanol, is used in step (5).
Comparative example 2
The difference from example 1 is that without addition of calcium carbonate, i.e.without step (3), the sample prepared only gave 1 cross-linking;
comparative example 3
The difference from example 1 is that no sodium alginate solution is added, i.e.no significant cross-linking is present inside the prepared sample.
And (3) performance test results:
the dressing obtained as shown in fig. 2 has a clear pore diameter distribution from small to large in the vertical direction, and shows a gradient distribution.
FIG. 3 shows the distribution of potassium ions and calcium ions before and after pickling. By comparison, potassium ions are densely distributed in the dressing before the dressing is immersed in the ethanol-acid mixed solution, and carbon ions are particularly less. After acid washing, calcium ions in the dressing become more obviously, the existence of the calcium ions is beneficial to crosslinking the sodium alginate, and a crosslinking network is formed to improve the overall strength of the dressing; and the number of potassium ions is obviously reduced, which shows that part of potassium ions are lost into an acid solution, provides conditions for the interaction between the anions of the sodium alginate and the cations of the chitosan quaternary ammonium salt, and is beneficial to the formation of a secondary cross-linked network.
Fig. 4 shows the comparison of the wrinkle ratios of the samples prepared in example 1 and comparative example 1 in the presence or absence of ethanol during acid washing, and the results show that the presence of ethanol can significantly reduce the wrinkle phenomenon of the samples, which is very beneficial for the subsequent application of the samples.
Fig. 5 is a comparison of the absorption rates of the sample prepared in example 1 and the samples prepared in comparative examples 2 and 3 to the simulated exudate fetal bovine serum within 20min, and it can be seen from the results that the sample prepared in comparative example 1 has a very strong exudate absorption capacity.
FIG. 6 is a graph showing the change of appearance of the samples prepared in example 1 and comparative examples 2 and 3 after absorbing a certain amount of fetal calf serum simulating wound exudate, and it can be clearly seen from fig. 5 that the sample prepared in example 1 still maintains shape stability after absorbing exudate, while the sample prepared in comparative example 2 with only 1 kind of crosslinking action gradually becomes loose and has a tendency of breakage; whereas the sample prepared in comparative example 3, which had no crosslinking, had started to break. This demonstrates that the strength of the sample prepared in example 1 is significantly higher than the other samples.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or equivalents thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with a gradient pore structure is characterized by comprising the following steps:
uniformly mixing a sodium alginate solution and a chitosan quaternary ammonium salt solution, adding chloride, and uniformly mixing to obtain a first mixed solution;
dispersing calcium carbonate with different particle sizes in the first mixed solution, uniformly mixing, performing ultrasonic treatment, and standing to obtain a second mixed solution;
lyophilizing the second mixed solution to obtain a crude dressing;
soaking the rough dressing in an ethanol-acid mixed solution for reaction to obtain a semi-finished dressing;
washing and freeze-drying the semi-finished dressing to obtain the dressing;
the total mass ratio of the chloride salt to the sodium alginate to the chitosan quaternary ammonium salt is 3-10.
2. The preparation method of the sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with the gradient pore structure as claimed in claim 1, wherein the degree of substitution of the chitosan quaternary ammonium salt is 20% -95%.
3. The method for preparing the sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with the gradient pore structure as claimed in claim 1, wherein the solid chloride salt is potassium chloride or sodium chloride.
4. The method for preparing the sodium alginate/chitosan quaternary ammonium salt double-crosslinked medical dressing with the gradient pore structure as claimed in claim 1, wherein the acid is hydrochloric acid or acetic acid.
5. The preparation method of the sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with the gradient pore structure as claimed in claim 1, wherein the concentration of the sodium alginate and the chitosan quaternary ammonium salt is 1-3wt%.
6. The preparation method of the sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with the gradient pore structure as claimed in claim 1, wherein the mass ratio of the sodium alginate solution to the chitosan quaternary ammonium salt solution is 3/1-3/1.
7. The preparation method of the sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with the gradient pore structure as claimed in claim 1, wherein the particle size of the calcium carbonate is 50-1000 meshes, and the mass ratio of the calcium carbonate to the total mass of the solution is 5-20wt%;
or, the ultrasonic defoaming time is 10-30min, and the standing time is 24-48h.
8. The preparation method of the sodium alginate/chitosan quaternary ammonium salt double-crosslinked medical dressing with the gradient pore structure as claimed in claim 1, wherein the freeze-drying ambient pressure is 5-20pa, the temperature is-40 to-60 ℃, and the freeze-drying time is 36-60h or 24-48h.
9. The preparation method of the sodium alginate/chitosan quaternary ammonium salt double-crosslinked medical dressing with the gradient pore structure as claimed in claim 1, wherein in the ethanol-acid mixed solution, the ratio of the acid solution to the ethanol is 1/1-3/7, and the soaking reaction time is 6-24h;
the washing times of the absolute ethyl alcohol are 2-5 times.
10. The sodium alginate/chitosan quaternary ammonium salt double-crosslinking medical dressing with a gradient pore structure prepared by the method of any one of claims 1 to 8.
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