CN113679878A - Injectable temperature-sensitive hydrogel and preparation method thereof - Google Patents
Injectable temperature-sensitive hydrogel and preparation method thereof Download PDFInfo
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Abstract
The embodiment of the invention provides an injectable temperature-sensitive hydrogel and a preparation method thereof, relating to biomedical materials. Aims at providing a preparation method of injectable temperature-sensitive hydrogel with low cost. Dissolving temperature-sensitive cellulose and a water-soluble antibacterial high polymer material in a body fluid simulation solution to obtain a first solution; and (3) carrying out defoaming treatment on the first solution to obtain the injectable temperature-sensitive hydrogel. The injectable temperature-sensitive hydrogel is obtained by a preparation method of the injectable temperature-sensitive hydrogel. The mixing sequence of the temperature-sensitive cellulose, the water-soluble antibacterial high polymer material and the body fluid simulation liquid is not limited, and the preparation method is simple; the raw materials are wide in source and low in price; the obtained injectable temperature-sensitive hydrogel has good biocompatibility and biodegradability, and also has antibacterial property, good effect and low cost.
Description
Technical Field
The invention relates to a biomedical material, in particular to an injectable temperature-sensitive hydrogel and a preparation method thereof.
Background
Wound repair and wound therapy are one of the basic medical problems of biomedical materials. To date, there are many biomaterials to promote wound healing, such as electrospun fibers, porous foams, and functionalized hydrogels. The hydrogel dressing material has excellent soft and wet characteristics and biocompatibility similarity, can be used as a good carrier of bioactive factors or cells, and can better simulate the skin extracellular matrix structure. The injectable hydrogel can realize in-situ gelation under the condition of external stimulation, and can be attached to tissues at the focus of the wound surface, so that irregular wound surfaces can be filled to the maximum extent and surrounding tissues are not damaged. The temperature-sensitive cross-linked hydrogel is mainly subjected to sol-gel conversion through temperature change, and the biological activity of target cells or drugs can be maintained to the maximum extent under the mild gelation condition. Based on the structure, the temperature-sensitive gel material has important application prospect in the field of wound dressing materials.
However, the traditional temperature-sensitive hydrogel has the problems of complex preparation process, poor biocompatibility, difficult degradation and the like.
Disclosure of Invention
The object of the present invention includes, for example, providing a method for preparing an injectable temperature-sensitive hydrogel, which can provide a low-cost method for preparing an injectable temperature-sensitive hydrogel.
The invention also aims to provide an injectable temperature-sensitive hydrogel, which can provide the injectable temperature-sensitive hydrogel with low cost.
Embodiments of the invention may be implemented as follows:
the embodiment of the invention provides a preparation method of an injectable temperature-sensitive hydrogel, which comprises the following steps:
dissolving temperature-sensitive cellulose and a water-soluble antibacterial high polymer material in a body fluid simulation solution to obtain a first solution;
and carrying out defoaming treatment on the first solution to obtain the injectable temperature-sensitive hydrogel.
In addition, the preparation method of the injectable temperature-sensitive hydrogel provided by the embodiment of the invention can also have the following additional technical characteristics:
optionally, the temperature-sensitive cellulose is any one of methyl cellulose, hydroxypropyl cellulose or hydroxypropyl methyl cellulose.
Optionally, the water-soluble antibacterial high polymer material is quaternary ammonium salt chitosan or polylysine.
Optionally, the body fluid simulant is a phosphate buffered saline solution or a simulant body fluid.
Optionally, the mass ratio of the temperature-sensitive cellulose is 6-10%.
Optionally, the water-soluble antibacterial high polymer material is 0.1-2% by mass.
Optionally, the step of dissolving the temperature-sensitive cellulose and the water-soluble antibacterial polymer material in the body fluid simulation solution to obtain a first solution includes:
dissolving the water-soluble antibacterial high polymer material in the body fluid simulation liquid to obtain a first mixed liquid;
and dissolving the temperature-sensitive cellulose in the first mixed solution to obtain the first solution.
Optionally, the step of dissolving the temperature-sensitive cellulose and the water-soluble antibacterial polymer material in the body fluid simulation solution to obtain a first solution includes:
dissolving the temperature-sensitive cellulose in the body fluid simulation solution to obtain a second mixed solution;
and dissolving the water-soluble antibacterial high polymer material in the second mixed solution to obtain the first solution.
Optionally, the step of dissolving the temperature-sensitive cellulose in the body fluid simulation solution to obtain a second mixed solution includes:
and adding the temperature-sensitive cellulose into the body fluid simulation solution, and stirring and mixing at the temperature of 50-60 ℃ to obtain the second mixed solution.
The embodiment of the invention also provides an injectable temperature-sensitive hydrogel. The injectable temperature-sensitive hydrogel is obtained by a preparation method of the injectable temperature-sensitive hydrogel.
The injectable temperature-sensitive hydrogel and the preparation method thereof provided by the embodiment of the invention have the beneficial effects of, for example:
the preparation method of the injectable temperature-sensitive hydrogel comprises the steps of dissolving temperature-sensitive cellulose and a water-soluble antibacterial high polymer material in a body fluid simulation solution to obtain a first solution; and (3) carrying out defoaming treatment on the first solution to obtain the injectable temperature-sensitive hydrogel. The mixing sequence of the temperature-sensitive cellulose, the water-soluble antibacterial high polymer material and the body fluid simulation liquid is not limited, and the preparation method is simple; the raw materials are wide in source and low in price; the obtained injectable temperature-sensitive hydrogel has good biocompatibility and biodegradability and also has antibacterial property. Provides a preparation method of low-cost injectable temperature-sensitive hydrogel.
The injectable temperature-sensitive hydrogel is prepared by the preparation method of the injectable temperature-sensitive hydrogel, the mixing sequence of the temperature-sensitive cellulose, the water-soluble antibacterial high polymer material and the body fluid simulation liquid is not limited, and the preparation method is simple. The raw materials have wide sources and low price.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a flowchart of a method for preparing an injectable temperature-sensitive hydrogel according to an embodiment of the present invention;
FIG. 2 is a flow chart of one embodiment of a method for preparing an injectable temperature-sensitive hydrogel according to an embodiment of the present invention;
FIG. 3 is a graph showing transition temperature curves of a first component of an injectable temperature-sensitive hydrogel according to an embodiment of the present invention;
fig. 4 is a graph illustrating transition temperature curves of a second component of an injectable temperature-sensitive hydrogel according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that if the terms "upper", "lower", "inside", "outside", etc. indicate an orientation or a positional relationship based on that shown in the drawings or that the product of the present invention is used as it is, this is only for convenience of description and simplification of the description, and it does not indicate or imply that the device or the element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention.
Furthermore, the appearances of the terms "first," "second," and the like, if any, are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
It should be noted that the features of the embodiments of the present invention may be combined with each other without conflict.
The preparation method of the injectable temperature-sensitive hydrogel provided in this embodiment is described in detail below with reference to fig. 1 to 2.
Referring to fig. 1, an embodiment of the present invention provides a method for preparing an injectable temperature-sensitive hydrogel, including: dissolving temperature-sensitive cellulose and a water-soluble antibacterial high polymer material in a body fluid simulation solution to obtain a first solution; and (3) carrying out defoaming treatment on the first solution to obtain the injectable temperature-sensitive hydrogel. Specifically, the injectable temperature-sensitive hydrogel can be obtained by standing for 6-12 hours at 4 ℃ for bubble treatment.
In the embodiment, the injectable temperature-sensitive hydrogel is prepared by taking temperature-sensitive cellulose as a temperature-sensitive carrier, taking a water-soluble antibacterial high polymer material as an antibacterial component and a gel component, and taking a body fluid simulation solution as a solvent and a coagulant aid.
The mixing sequence of the temperature-sensitive cellulose, the water-soluble antibacterial polymer material and the body fluid simulation liquid is not limited, and the preparation method is simple. The temperature-sensitive cellulose, the water-soluble antibacterial polymer material and the body fluid simulation liquid are adopted, so that the raw materials are wide in source, low in price and simple in preparation process. Cellulose is used as macromolecular polysaccharide, is easy to degrade, the injectable temperature-sensitive hydrogel has very good biocompatibility and biodegradability, and when the temperature-sensitive hydrogel is injected to a wound surface, the gel can be adhered to the wound surface and can be well attached to the wound and release medicines; the antibacterial property is achieved; has excellent temperature sensitivity, can quickly form white gel when the temperature is between 30 and 37 ℃, and the process is reversible. Good effect and low cost.
In this embodiment, the mass ratio of the temperature-sensitive cellulose is 6 to 10%. Specifically, the mass ratio may be 6%, 7%, 8%, 9%, 10%.
In this example, the mass ratio of the water-soluble antibacterial polymer material is 0.1 to 2%. Specifically, the mass ratio is 0.1%, 0.5%, 0.8%, 1%, 1.2%, 2%.
In this embodiment, the temperature-sensitive cellulose is any one of methyl cellulose, hydroxypropyl cellulose, and hydroxypropyl methyl cellulose.
Methylcellulose is a methyl ether of cellulose, the simplest form of cellulose ethers, and has good biocompatibility. In the state of methylcellulose solution, methylcellulose molecules are hydrated, and only simple chain winding effect exists among the molecules; when the temperature is increased, gel formation occurs due to the hydrophobic interaction of the methoxy groups.
In this embodiment, the water-soluble antibacterial polymer material is quaternary ammonium salt chitosan or polylysine.
In this embodiment, the body fluid simulant is phosphate buffered saline or a simulant body fluid.
In this embodiment, the step of dissolving the temperature-sensitive cellulose and the water-soluble antibacterial polymer material in the body fluid simulant to obtain the first solution includes:
dissolving a water-soluble antibacterial high polymer material in a body fluid simulation solution to obtain a first mixed solution;
dissolving the temperature-sensitive cellulose in the first mixed solution to obtain a first solution.
Specifically, a water-soluble antibacterial high polymer material is added into a body fluid simulation solution, and a first mixed solution is obtained by stirring and mixing; and then adding the temperature-sensitive cellulose into the first mixed solution, and stirring and mixing at the temperature of 50-60 ℃ to obtain a first solution. The temperature can be 50 deg.C, 51 deg.C, 52 deg.C, 55 deg.C, 56 deg.C, 60 deg.C.
In another embodiment, the step of dissolving the temperature-sensitive cellulose and the water-soluble antibacterial polymer material in the body fluid simulant to obtain the first solution includes:
dissolving temperature-sensitive cellulose in body fluid simulation liquid to obtain second mixed liquid;
and dissolving the water-soluble antibacterial high polymer material in the second mixed solution to obtain a first solution.
Specifically, the temperature-sensitive cellulose is added into the body fluid simulation solution, and is stirred and mixed at the temperature of 50-60 ℃ to obtain a second mixed solution. And dissolving the water-soluble antibacterial high polymer material in the second mixed solution to obtain a first solution.
Specifically, referring to fig. 2, 6-10 wt% of methylcellulose is dissolved in phosphate buffered saline solution to obtain a second mixed solution; dissolving 0.1-2 wt% of quaternary ammonium salt chitosan in the second mixed solution to obtain a first solution; and (3) defoaming the first solution to obtain the injectable temperature-sensitive hydrogel.
In another embodiment, the step of dissolving the temperature-sensitive cellulose and the water-soluble antibacterial polymer material in the body fluid simulant to obtain the first solution includes:
adding temperature sensitive cellulose and water soluble antibacterial polymer material into the body fluid simulation solution, and stirring and mixing at 50-60 deg.C to obtain first solution.
The temperature-sensitive cellulose and the water-soluble antibacterial polymer material are added into the body fluid simulation liquid in a non-sequential order. The dissolution of the temperature-sensitive cellulose in the body fluid simulation solution needs to be carried out at the temperature of 50-60 ℃, the temperature-sensitive cellulose can be heated after being added into the body fluid simulation solution, and the temperature-sensitive cellulose and the water-soluble antibacterial polymer material can be heated after being added into the body fluid simulation solution.
In this embodiment, the step of performing bubble removal treatment on the first solution to obtain the injectable temperature-sensitive hydrogel includes: and (3) carrying out defoaming treatment on the first solution in the modes of ultrasonic treatment, centrifugation, standing at 4 ℃ and the like to obtain the injectable temperature-sensitive hydrogel. The defoaming method is not limited to ultrasonic, centrifugal or 4 ℃ standing.
Example 1
Preparing a phosphate buffer salt solution standard solution as a solvent and a coagulant aid agent of gel;
taking a certain amount of phosphate buffer solution in a beaker, adding 6-10 wt% of methylcellulose (with the viscosity of 15mPas) into the beaker, and primarily stirring the mixture at room temperature to form viscous solution;
then 0.1-2 wt% of quaternary ammonium salt chitosan is added; sealing the beaker, and further fully and uniformly stirring at the temperature of 50-60 ℃ to obtain white viscous liquid;
cooling to room temperature, removing bubbles by means of ultrasound and the like, and obtaining the injectable temperature-sensitive hydrogel.
The hydrogel has a sol-gel transition temperature of 30-37 ℃. Therein, fig. 3 shows a sol-gel transition temperature profile of a hydrogel of 7% methylcellulose, 1% quaternary ammonium chitosan, with a transition temperature of 36.7 ℃. FIG. 4 shows a sol-gel transition temperature profile of a 10% methylcellulose, 1% quaternary ammonium salt chitosan hydrogel, with a transition temperature of 31.9 ℃.
Example 2
Taking 9.2g of standard solution of phosphate buffer salt solution in a beaker, adding 0.7g of methylcellulose into the beaker, and primarily stirring the beaker at room temperature;
adding 0.1g of quaternary ammonium salt chitosan, sealing by using a preservative film, placing in a water bath at 60 ℃, and magnetically stirring until the chitosan is completely dissolved to obtain a white viscous solution;
and cooling to room temperature, and centrifuging to remove bubbles in the hydrogel to obtain the injectable temperature-sensitive hydrogel.
The hydrogel had a sol-gel transition temperature of 36.5 ℃.
Example 3
Taking 9.2g of standard solution of phosphate buffer salt solution in a beaker, adding 0.2g of quaternary ammonium salt chitosan into the beaker, and primarily stirring at room temperature;
then 0.7g of methylcellulose is added, and the mixture is fully and evenly stirred at the temperature of 50 ℃ to obtain white viscous liquid;
and (3) standing at 4 ℃ to remove bubbles in the hydrogel, thus obtaining the injectable temperature-sensitive hydrogel.
The hydrogel had a sol-gel transition temperature of 35.4 ℃.
Example 4
Taking 10g of standard solution of phosphate buffered saline solution, adding 0.5g of polylysine into the beaker, and primarily stirring the mixture at room temperature;
then 0.8g of hydroxypropyl cellulose is added, and the mixture is fully and uniformly stirred at the temperature of 60 ℃ to obtain white viscous liquid;
removing bubbles in the hydrogel by ultrasonic to obtain the injectable temperature-sensitive hydrogel.
The hydrogel had a sol-gel transition temperature of 34.3 ℃.
Example 5
Taking 10g of phosphate buffer solution standard solution to a beaker, adding 0.8g of polylysine and 0.8g of hydroxypropyl methylcellulose into the beaker, and fully and uniformly stirring the mixture at the temperature of 55 ℃ to obtain white viscous liquid;
removing air bubbles in the hydrogel by centrifugation to obtain the injectable temperature-sensitive hydrogel.
The hydrogel had a sol-gel transition temperature of 33.1 ℃.
The preparation method of the injectable temperature-sensitive hydrogel provided by the embodiment at least has the following advantages:
the mixing sequence of the temperature-sensitive cellulose, the water-soluble antibacterial polymer material and the body fluid simulation liquid is not limited, and the preparation method is simple.
The temperature sensitive cellulose, the water soluble antibacterial polymer material and the body fluid simulation liquid are used as raw materials, and are low in price and easy to obtain.
The temperature-sensitive gel has good biocompatibility and biodegradability, and when the temperature-sensitive gel is injected to a wound surface, the gel can be adhered to the wound surface, so that the temperature-sensitive gel can be well attached to the wound and release medicines.
Has excellent temperature sensitivity, can quickly form white gel when the temperature is between 30 and 37 ℃, and has reversible process.
The embodiment of the invention also provides an injectable temperature-sensitive hydrogel. The injectable temperature-sensitive hydrogel is obtained by a preparation method of the injectable temperature-sensitive hydrogel. The mixing sequence of the temperature-sensitive cellulose, the water-soluble antibacterial polymer material and the body fluid simulation liquid is not limited, and the preparation method is simple. The raw materials have wide sources and low price.
The above description is only for the specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. A preparation method of an injectable temperature-sensitive hydrogel is characterized by comprising the following steps:
dissolving temperature-sensitive cellulose and a water-soluble antibacterial high polymer material in a body fluid simulation solution to obtain a first solution;
and carrying out defoaming treatment on the first solution to obtain the injectable temperature-sensitive hydrogel.
2. The method for preparing an injectable temperature-sensitive hydrogel according to claim 1, wherein:
the temperature-sensitive cellulose is any one of methyl cellulose, hydroxypropyl cellulose or hydroxypropyl methyl cellulose.
3. The method for preparing an injectable temperature-sensitive hydrogel according to claim 1, wherein:
the water-soluble antibacterial high polymer material is quaternary ammonium salt chitosan or polylysine.
4. The method for preparing an injectable temperature-sensitive hydrogel according to claim 1, wherein:
the body fluid simulation solution is phosphate buffer saline solution or simulation body fluid.
5. The method for preparing an injectable temperature-sensitive hydrogel according to claim 1, wherein:
the mass ratio of the temperature-sensitive cellulose is 6-10%.
6. The method for preparing an injectable temperature-sensitive hydrogel according to claim 1, wherein:
the mass ratio of the water-soluble antibacterial high polymer material is 0.1-2%.
7. The method for preparing an injectable temperature-sensitive hydrogel according to any one of claims 1 to 6, wherein:
the step of dissolving the temperature-sensitive cellulose and the water-soluble antibacterial polymer material in the body fluid simulated liquid to obtain the first solution comprises the following steps:
dissolving the water-soluble antibacterial high polymer material in the body fluid simulation liquid to obtain a first mixed liquid;
and dissolving the temperature-sensitive cellulose in the first mixed solution to obtain the first solution.
8. The method for preparing an injectable temperature-sensitive hydrogel according to any one of claims 1 to 6, wherein:
the step of dissolving the temperature-sensitive cellulose and the water-soluble antibacterial polymer material in the body fluid simulated liquid to obtain the first solution comprises the following steps:
dissolving the temperature-sensitive cellulose in the body fluid simulation solution to obtain a second mixed solution;
and dissolving the water-soluble antibacterial high polymer material in the second mixed solution to obtain the first solution.
9. The method for preparing an injectable temperature-sensitive hydrogel according to claim 8, wherein:
the step of dissolving the temperature-sensitive cellulose in the body fluid simulation solution to obtain a second mixed solution comprises the following steps:
and adding the temperature-sensitive cellulose into the body fluid simulation solution, and stirring and mixing at the temperature of 50-60 ℃ to obtain the second mixed solution.
10. An injectable temperature-sensitive hydrogel, which is characterized in that:
the injectable temperature-sensitive hydrogel is obtained by the preparation method of the injectable temperature-sensitive hydrogel according to any one of claims 1 to 9.
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| CN114344246A (en) * | 2021-12-06 | 2022-04-15 | 南京医科大学附属口腔医院 | Injectable temperature-sensitive hydrogel and preparation method and application thereof |
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| US20190015564A1 (en) * | 2017-07-14 | 2019-01-17 | Soonchunhyang University Industry Academy Cooperation Foundation | Adhesion prevention agent comprising injectable thermosensitive wood based-oxidized cellulose nanofiber |
| KR20200112746A (en) * | 2019-03-21 | 2020-10-05 | 순천향대학교 산학협력단 | Novel thermosensitive cellulose based hydrogel for post-surgical peritoneal adhesion prevention and preparation method thereof |
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| US20190015564A1 (en) * | 2017-07-14 | 2019-01-17 | Soonchunhyang University Industry Academy Cooperation Foundation | Adhesion prevention agent comprising injectable thermosensitive wood based-oxidized cellulose nanofiber |
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| CN114344246A (en) * | 2021-12-06 | 2022-04-15 | 南京医科大学附属口腔医院 | Injectable temperature-sensitive hydrogel and preparation method and application thereof |
| CN114344246B (en) * | 2021-12-06 | 2024-03-19 | 南京医科大学附属口腔医院 | Injectable temperature-sensitive hydrogel and preparation method and application thereof |
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