CN114712553B - Preparation method of wound dressing based on shaddock ped pectin-oxidized chitosan composite hydrogel - Google Patents
Preparation method of wound dressing based on shaddock ped pectin-oxidized chitosan composite hydrogel Download PDFInfo
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Abstract
The invention relates to the field of biomedical materials, and discloses a preparation method of wound dressing based on shaddock ped pectin-oxidized chitosan composite hydrogel. The preparation method comprises the steps of firstly, respectively preparing naringin pectin and oxidized chitosan, and then preparing the naringin pectin and the oxidized chitosan into composite hydrogel; finally, the wound dressing is prepared after baking. The composite hydrogel prepared from the two materials of the naringin pectin and the oxidized chitosan has excellent biodegradability, biocompatibility and regenerability, is favorable for cell proliferation, and can be used as nutrient and waste for waste exchange in the healing process. The composite hydrogel disclosed by the invention is soft hydrogel, and can be easily removed from skin wounds without causing any secondary skin injury. Therefore, the dressing has good treatment effect on wound healing and wound surface large-area infection.
Description
Technical Field
The invention relates to the field of biomedical materials, in particular to a preparation method of wound dressing based on shaddock ped pectin-oxidized chitosan composite hydrogel.
Background
Skin injuries from wounds, burns and other external accidents often lead to a series of complications and even death. Wound healing of skin lesions is a fairly complex process involving several stages of hemostasis, inflammation, cell proliferation and tissue remodeling. To date, a number of advanced materials have been developed and are considered potential candidates for skin wound dressings, such as fibers, gauze, medical films, hydrogels, and the like. Among these materials, hydrogel wound dressings have several distinct advantages, such as hydrogels having a three-dimensional (3D) structure that can hold high levels of water to provide a suitably moist environment for wound healing. In addition, hydrogels with specific 3D structures similar to the natural extracellular matrix (ECM) are also critical to cell proliferation and as nutrient and waste exchange in the healing process. In addition, soft hydrogels can be easily removed from skin wounds without causing any secondary skin damage. Polysaccharide-based hydrogels, such as alginates, celluloses, pectins, hyaluronates, chitosan and carrageenan, have attracted considerable attention in wound healing and other biomedical applications due to their excellent biodegradability, biocompatibility, availability and reproducibility. However, practical applications of hydrogels in wound dressings are still limited at the present stage due to the poor mechanical strength and stability of hydrogels. Thus, the development of novel hydrogels with superior performance remains an urgent need to facilitate the application of wound dressings in the healing of skin wounds.
The grapefruit belongs to Rutaceae plants, and is the biggest one of citrus fruits. A large amount of shaddock peel is discarded after being eaten, so that resource waste and environmental pollution are caused. The shaddock peel accounts for 30 percent of the total weight of the fruit. The pomelo peel also contains rich chemical components such as pectin, essential oil, cellulose, flavonoid compounds, etc. Pectin production from the pomelo peel waste is comparable to or superior to other known sources of fruit processing waste.
Pectin is another polysaccharide, namely an anionic polysaccharide. It is a structural complex consisting of D-galacturonic acid, the carboxy terminus of which is esterified with methanol, in which a certain amount of neutral sugar is also present. The neutral sugar in pectin is D-galactose, L-rhamnose, L-arabinose and D-xylose, and the type and amount of neutral sugar are different depending on pectin source. In plant tissue, pectin is present in the middle sheet and primary cell walls. In most types of plants, pectin represents about one third of the dry matter of the cell wall and provides intercellular adhesion as well as mechanical strength of the cell wall, and appears to have a high gel forming capacity, being degradable in nature and thus a potential material suitable for making hydrogel wound dressings.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of wound dressing based on shaddock ped pectin-oxidized chitosan composite hydrogel. The preparation method comprises the steps of firstly, respectively preparing naringin pectin and oxidized chitosan, and then preparing the naringin pectin and the oxidized chitosan into composite hydrogel; finally, the wound dressing is prepared after baking. The composite hydrogel prepared from the two materials of the naringin pectin and the oxidized chitosan has excellent biodegradability, biocompatibility and regenerability, is favorable for cell proliferation, and can be used as nutrient and waste for waste exchange in the healing process. The composite hydrogel disclosed by the invention is soft hydrogel, and can be easily removed from skin wounds without causing any secondary skin injury. Therefore, the dressing has good treatment effect on wound healing and wound surface large-area infection.
The specific technical scheme of the invention is as follows:
a preparation method of wound dressing based on shaddock ped pectin-oxidized chitosan composite hydrogel comprises the following steps:
step 1: preparation of shaddock ped powder: cleaning fresh shaddock peel with water, peeling off shaddock peel, removing white pulp and reserving peel; cutting the peel into pieces, vacuum freeze drying, pulverizing, sieving to obtain pericarpium Citri Grandis powder, and storing.
The vacuum freeze drying technology can ensure that the dried powder has good dispersibility. Sieving can separate the powder obtained by mixing the coarse and fine powders, thereby ensuring uniformity of the composition of the naringin powder.
Step 2: extraction of shaddock ped pectin: mixing pericarpium Citri Grandis powder with water in a container, and placing the container in a hot water bath; adjusting pH to 1.5-1.7 with citric acid, and extracting; cooling the mixture in the container to room temperature, filtering, centrifuging, precipitating supernatant with ethanol solution, maintaining at room temperature for 10-15 hr, filtering, treating with ethanol solution to remove monosaccharide and disaccharide, and drying to obtain naringin pectin.
Citric acid is used to effectively reduce negative charge of the pomelo peel pectin, so that the pectin is combined with intermolecular hydrogen bonds to gel. Further, the present team found that adjusting the pH of the system to the above specified interval with citric acid enabled not only proper cleavage of the cellulose crystalline regions of the pectin molecules, but also no disruption of the structure of the pectin molecules. The first use of the ethanol solution is to precipitate the supernatant and the second use of the ethanol solution is to remove the mono-and disaccharides in pectin to a great extent.
Step 3: preparation of oxidized chitosan: adding chitosan into water, and stirring at room temperature; adding sodium periodate into the obtained chitosan suspension, stirring, and standing at room temperature; washing the precipitate for several times with water and fast freezing with liquid nitrogen; and finally, freeze-drying to obtain the oxidized chitosan.
The invention uses sodium periodate to oxidize chitosan, and improves the solubility of chitosan in solution when introducing aldehyde groups. Amine groups in the oxidized chitosan can effectively attract anionic erythrocytes through adsorbing platelet membrane glycoprotein, and promote platelet activation.
Step 4: preparation of shaddock Pi Guojiao-oxidized chitosan composite hydrogel: respectively dissolving shaddock ped pectin and oxidized chitosan in water to obtain shaddock ped pectin aqueous solution and oxidized chitosan aqueous solution; and then mixing the two materials to obtain a mixed solution, stirring and washing the mixed solution, and performing ultrasonic treatment to obtain the shaddock Pi Guojiao-oxidized chitosan composite hydrogel.
The invention initiates the free radical polymerization of the monomer in a short time by ultrasonic wave, namely, the-COOH in pectin molecules is partially deprotonated to form-COO － Can be combined with-NH in chitosan 3 + Ion crosslinking occurs to form-COO+NH 3 + Secondary valence bonds, forming polyelectrolyte complexes (PECs) by electrostatic action.
Step 5: preparation of wound dressing: pouring the prepared shaddock ped pectin-oxidized chitosan composite hydrogel into a container, and baking under ultraviolet irradiation to obtain the wound dressing.
The hydrogel is cured to form a hydrogel layer by sufficient heat radiation and ultraviolet radiation. Namely, the shaddock ped pectin-oxidized chitosan composite hydrogel is placed under ultraviolet radiation, and a polyelectrolyte complex (PEC) formed by the shaddock ped pectin-oxidized chitosan composite hydrogel and the shaddock ped pectin-oxidized chitosan composite hydrogel is subjected to crosslinking modification to prepare a crosslinked network-shaped solid polymer electrolyte complex, and the crosslinked network-shaped solid polymer electrolyte complex is in an crosslinked network structure, so that the mechanical property of the solid polymer electrolyte complex is improved.
Preferably, in step 1, the thickness of the outer skin is 2-4mm, and the vacuum freeze drying time is 10-12h.
Preferably, in step 1, the sieving range is 190-200 mesh sieve, the humidity of the storage environment is 55-65%, and the temperature is 20-30 ℃.
Preferably, in step 2, the mass ratio of the shaddock ped powder to the water in the container is 1:5-1:7, preparing a base material; the temperature of the hot water bath is 90-100 ℃, and the time of the hot water bath is 80-90min.
Preferably, in the step 2, the centrifugal speed is 7000-8000rpm, and the centrifugal time is 10-20min; the volume fraction of ethanol in the ethanol solution is 90-98%; the drying temperature is 45-55 ℃.
Preferably, in the step 3, the dosage ratio of chitosan to water in the chitosan suspension is 0.5-1.5g:50-70ml; the stirring time at room temperature is 0.5-1.5h.
Preferably, in the step 3, the mass ratio of the sodium periodate to the chitosan is 0.5-1.5:0.3-0.5, the stirring temperature is 50-55 ℃, and the stirring time is 1-3h; the standing time at room temperature is 40-50h; the freeze drying time is 1-3 days.
Preferably, in the step 4, the mass ratio of the naringin pectin, the oxidized chitosan and the water is 0.5-1.0:0.1-0.5:10-20.
Preferably, in the step 4, the stirring temperature is 35-40 ℃ and the stirring time is 2-6h; the amplitude of the ultrasonic wave is 34-45%, and the ultrasonic time is 20-40s.
Preferably, in step 45, the baking conditions are as follows: 40-50 ℃ and 40-50h.
Compared with the prior art, the invention has the following technical effects:
(1) The composite hydrogel prepared from the two materials of the naringin pectin and the oxidized chitosan has excellent biodegradability, biocompatibility and regenerability, is favorable for cell proliferation, and can be used as nutrient and waste for waste exchange in the healing process.
(2) The composite hydrogel disclosed by the invention is soft hydrogel, and can be easily removed from skin wounds without causing any secondary skin injury. Therefore, the dressing has good treatment effect on wound healing and wound surface large-area infection.
Detailed Description
The invention is further described below with reference to examples.
Example 1
1) Preparation of shaddock ped powder: washing fresh pericarpium Citri Grandis with distilled water, peeling off pericarpium Citri Grandis, removing white pulp on pericarpium Citri Grandis, and keeping the outer skin with thickness of 2 mm. Cutting the outer skin into pieces, vacuum freeze drying for 10h, and pulverizing the dried shaddock peel by a high-speed multifunctional pulverizer to obtain shaddock peel powder, and sieving the powder with a 190-mesh sieve to obtain the raw material required by experiments. The raw materials are put into a dampproof cabinet with the humidity of 60 percent and the temperature of 25 ℃ for storage for standby.
2) Extraction of shaddock ped pectin: a beaker containing 5g of grapefruit powder was kept in a hot water bath at 90℃for 80min with 25g of distilled water. The extraction process was performed by adjusting the pH of the solvent to 1.5 with the aid of citric acid, and the mixture in the beaker was then cooled to room temperature. After cooling, the solution was filtered using a scrim. After filtration, the resulting filtrate was centrifuged at 7000rpm for 10min. Then, precipitation of the supernatant was performed with 95% ethanol by volume fraction and maintained at 20 ℃ at room temperature. After 12 hours, the precipitate was filtered and treated with 95% ethanol by volume to remove mono-and disaccharides, and then dried in a tray dryer at 50 ℃ to extract the naringin pectin.
3) Preparation of oxidized chitosan: 0.5g of chitosan was suspended in 50ml of distilled water and stirred at room temperature for 1h. Then, 0.3g of sodium periodate was added to the chitosan suspension, and the mixture was stirred at 50℃for 2 hours. After that, the suspension was stored at room temperature for 48 hours. The precipitated product was then washed multiple times with deionized water and then flash frozen with liquid nitrogen. Finally, the mixture was lyophilized for 2 days using a water-cooled pilot-scale freeze dryer.
4) Preparation of shaddock Pi Guojiao-oxidized chitosan composite hydrogel: 0.5g of pomelo peel pectin and 0.1g of oxidized chitosan are respectively dissolved in 10ml of deionized water to prepare an aqueous solution of the pomelo peel pectin and the oxidized chitosan. The two were then mixed and stirred at 35℃for 2 hours, washed twice, and sonicated at 40% amplitude for 30s to prepare a hydrogel.
5) Preparation of a shaddock Pi Guojiao-oxidized chitosan composite hydrogel wound dressing: pouring the prepared shaddock ped pectin/oxidized chitosan hydrogel into a culture dish, and drying the shaddock ped pectin/oxidized chitosan hydrogel in an oven with an ultraviolet irradiation function at 45 ℃ for 48 hours to prepare the shaddock ped pectin/oxidized chitosan dressing.
Example 2
1) Preparation of shaddock ped powder: washing fresh pericarpium Citri Grandis with distilled water, peeling off pericarpium Citri Grandis, removing white pulp on pericarpium Citri Grandis, and keeping the outer skin with thickness of 3 mm. Cutting the outer skin into pieces, vacuum freeze drying for 11h, and pulverizing the dried shaddock peel by a high-speed multifunctional pulverizer to obtain shaddock peel powder, and sieving the powder with a 195-mesh sieve to obtain the raw material required by experiments. The raw materials are put into a dampproof cabinet with the humidity of 60 percent and the temperature of 25 ℃ for storage for standby.
2) Extraction of shaddock ped pectin: a beaker containing 7g of grapefruit powder was kept in a hot water bath at 95℃for 85min with 42g of distilled water. The extraction process was performed by adjusting the pH of the solvent to 1.6 with the aid of citric acid, and the mixture in the beaker was then cooled to room temperature. After cooling, the solution was filtered using a scrim. After filtration, the resulting filtrate was centrifuged at 7500rpm for 15min. Then, precipitation of the supernatant was performed with 95% ethanol by volume fraction and maintained at 20 ℃ at room temperature. After 12 hours, the precipitate was filtered and treated with 95% ethanol by volume to remove mono-and disaccharides, and then dried in a tray dryer at 50 ℃ to extract the naringin pectin.
3) Preparation of oxidized chitosan: 1.0g of chitosan was suspended in 60ml of distilled water and stirred at room temperature for 1h. Then, 0.4g of sodium periodate was added to the chitosan suspension, and the mixture was stirred at 52℃for 2 hours. After that, the suspension was stored at room temperature for 48 hours. The precipitated product was then washed multiple times with deionized water and then flash frozen with liquid nitrogen. Finally, the mixture was lyophilized for 2 days using a water-cooled pilot-scale freeze dryer.
4) Preparation of shaddock Pi Guojiao-oxidized chitosan composite hydrogel: 0.7g of pomelo peel pectin and 0.2g of oxidized chitosan are respectively dissolved in 15ml of deionized water to prepare an aqueous solution of the pomelo peel pectin and the oxidized chitosan. The two were then mixed and stirred at 37℃for 4 hours, washed twice, and sonicated at 40% amplitude for 30s to produce a hydrogel.
5) Preparation of wound dressing of shaddock Pi Guojiao-oxidized chitosan composite hydrogel: pouring the prepared shaddock ped pectin-oxidized chitosan composite hydrogel into a culture dish, and drying the shaddock ped pectin-oxidized chitosan composite hydrogel in an oven with an ultraviolet irradiation function at 45 ℃ for 48 hours to prepare the shaddock ped pectin/oxidized chitosan dressing.
Example 3
1) Preparation of shaddock ped powder: washing fresh pericarpium Citri Grandis with distilled water, peeling off pericarpium Citri Grandis, removing white pulp on pericarpium Citri Grandis, and keeping the outer skin with thickness of 4 mm. Cutting the outer skin into pieces, vacuum freeze drying for 12h, and pulverizing the dried shaddock peel by a high-speed multifunctional pulverizer to obtain shaddock peel powder, and sieving the powder with a 200-mesh sieve to obtain the raw material required by experiments. The raw materials are put into a dampproof cabinet with the humidity of 60 percent and the temperature of 25 ℃ for storage for standby.
2) Extraction of shaddock ped pectin: a beaker containing 9g of grapefruit powder was kept in a hot water bath with 63g of distilled water for 90min. The extraction process was performed by adjusting the pH of the solvent to 1.7 with the aid of citric acid, and the mixture in the beaker was then cooled to room temperature. After cooling, the solution was filtered using a scrim. After filtration, the resulting filtrate was centrifuged at 8000rpm for 20min. Then, precipitation of the supernatant was performed with 95% ethanol by volume fraction and maintained at 20 ℃ at room temperature. After 12 hours, the precipitate was filtered and treated with 95% ethanol by volume to remove mono-and disaccharides, and then dried in a tray dryer at 50 ℃ to extract the naringin pectin.
3) Preparation of oxidized chitosan: 1.5g of chitosan was suspended in 70ml of distilled water and stirred at room temperature for 1h. Then, 0.5g of sodium periodate was added to the chitosan suspension, and the mixture was stirred at 54℃for 2 hours. After that, the suspension was stored at room temperature for 48 hours. The precipitated product was then washed multiple times with deionized water and then flash frozen with liquid nitrogen. Finally, the mixture was lyophilized for 2 days using a water-cooled pilot-scale freeze dryer.
4) Preparation of shaddock Pi Guojiao-oxidized chitosan composite hydrogel: 0.9g of pomelo peel pectin and 0.4g of oxidized chitosan are respectively dissolved in 20ml of deionized water to prepare an aqueous solution of the pomelo peel pectin and the oxidized chitosan. The two were then mixed and stirred at 39℃for 6 hours, washed twice, and sonicated at 40% amplitude for 30s to prepare a hydrogel.
5) Preparation of wound dressing of shaddock Pi Guojiao-oxidized chitosan composite hydrogel: pouring the prepared naringin pectin/oxidized chitosan hydrogel into a culture dish, and drying in an oven with ultraviolet irradiation function at 45 ℃ for 48 hours to prepare the naringin pectin-oxidized chitosan composite hydrogel dressing.
The raw materials and equipment used in the invention are common raw materials and equipment in the field unless specified otherwise; the methods used in the present invention are conventional in the art unless otherwise specified.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any simple modification, variation and equivalent transformation of the above embodiment according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (9)
1. A preparation method of wound dressing based on shaddock ped pectin-oxidized chitosan composite hydrogel is characterized by comprising the following steps: the method comprises the following steps:
step 1: preparation of shaddock ped powder: cleaning fresh shaddock peel with water, peeling off shaddock peel, removing white pulp and reserving peel; cutting the outer skin into pieces, vacuum freeze-drying, pulverizing, sieving to obtain pericarpium Citri Grandis powder, and storing for use;
step 2: extraction of shaddock ped pectin: mixing pericarpium Citri Grandis powder with water in a container, and placing the container in a hot water bath; adjusting pH to 1.5-1.7 with citric acid, and extracting; cooling the mixture in the container to room temperature, filtering, centrifuging, precipitating supernatant with ethanol solution, maintaining at room temperature for 10-15 hr, filtering the precipitate, treating with ethanol solution to remove monosaccharide and disaccharide, and drying to obtain naringin pectin;
step 3: preparation of oxidized chitosan: adding chitosan into water, and stirring at room temperature; adding sodium periodate into the obtained chitosan suspension, stirring, and standing at room temperature; washing the precipitate for several times with water and fast freezing with liquid nitrogen; finally, freeze-drying is carried out to obtain oxidized chitosan; the mass ratio of the sodium periodate to the chitosan is 0.5-1.5:0.3-0.5;
step 4: preparation of shaddock Pi Guojiao-oxidized chitosan composite hydrogel: respectively dissolving shaddock ped pectin and oxidized chitosan in water to obtain shaddock ped pectin aqueous solution and oxidized chitosan aqueous solution; then mixing the two to obtain a mixed solution, stirring, washing, and performing ultrasonic treatment to obtain the shaddock Pi Guojiao-oxidized chitosan composite hydrogel; the mass ratio of the shaddock ped pectin to the oxidized chitosan to the water is 0.5-1.0:0.1-0.5:10-20; the amplitude of the ultrasonic wave is 34-45%, and the ultrasonic time is 20-40s;
step 5: preparation of wound dressing: pouring the prepared shaddock ped pectin-oxidized chitosan composite hydrogel into a container, and baking under ultraviolet irradiation to obtain the wound dressing.
2. The method of manufacturing according to claim 1, wherein: in the step 1, the thickness of the crust is 2-4mm, and the vacuum freeze drying time is 10-12h.
3. The method of manufacturing according to claim 1, wherein: in the step 1, the sieving range is 190-200 meshes, the humidity of the storage environment is 55-65%, and the temperature is 20-30 ℃.
4. The method of manufacturing according to claim 1, wherein: in the step 2, the mass ratio of the shaddock ped powder to the water in the container is 1:5-1:7; the temperature of the hot water bath is 90-100 ℃, and the time of the hot water bath is 80-90min.
5. The method of manufacturing according to claim 1, wherein: in the step 2, the centrifugal speed is 7000-8000rpm, and the centrifugal time is 10-20min; the volume fraction of ethanol in the ethanol solution is 90-98%; the drying temperature is 45-55 ℃.
6. The method of manufacturing according to claim 1, wherein: in the step 3, the dosage ratio of chitosan to water in the chitosan suspension is 0.5-1.5g:50-70ml; the stirring time at room temperature is 0.5-1.5h.
7. The method of manufacturing according to claim 6, wherein: in the step 3, the stirring temperature is 50-55 ℃ and the stirring time is 1-3h; the standing time at room temperature is 40-50h; the freeze drying time is 1-3 days.
8. The method of manufacturing according to claim 1, wherein: in the step 4, the stirring temperature is 35-40 ℃ and the stirring time is 2-6h.
9. The method of manufacturing according to claim 1, wherein: in step 5, the baking conditions are as follows: 40-50 ℃ and 40-50h.
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