Preparation method of antibacterial composite emulsion gel and antibacterial dressing

Abstract

The present invention provides a preparation method of an antibacterial composite emulsion gel and an antibacterial dressing, and relates to the technical field of antibacterial dressings. The preparation method comprises: preparing a tri-zan gum solution, wherein the mass concentration of tri-zan gum is 0.5% to 1%; adding a bacterial cellulose suspension to the tri-zan gum solution, so that the mass concentration of bacterial cellulose in the composite suspension reaches 0.1% to 0.5%; mixing an antibacterial plant essential oil or a magnolol oil solution with the composite suspension, and processing with a homogenizer to produce an emulsified system; heating the emulsified system and adding water to make up for evaporation losses; the heated emulsified system is formed after cooling to obtain an antibacterial composite emulsion gel. The antibacterial composite emulsion gel obtained according to the preparation method provided by the present invention has the following advantages: the antibacterial active ingredients are evenly distributed in the dressing, the uniformity is extremely high, the antibacterial performance can be improved, and different states of emulsion gels can be obtained by changing the amount of tri-zan gum and bacterial cellulose added.

Description

Technical Field

[0001] The invention relates to the technical field of antibacterial dressings, and in particular to a preparation method of an antibacterial composite emulsion gel and an antibacterial dressing. Background Art

[0002] The skin is the largest organ in the human body and is susceptible to various injuries, such as cuts, burns, surgical trauma, etc., and skin injuries are very prone to wound infection, which slows down wound healing; especially large-area burns and scalds of the skin, which are more likely to cause inflammatory reactions, which are life-threatening in severe cases. The healing of skin tissue is often accompanied by bacterial infection, which can delay wound healing or even lead to death. Therefore, bacterial infection is a challenge that must be overcome in the treatment of skin wounds. Wound dressings have always been a common and effective method to resist external bacterial infection and promote skin tissue healing. To date, a variety of synthetic wound dressing substrates, including sponges, electrospun nanofibers and hydrogels, have been studied. Among them, hydrogel is the most ideal wound dressing because it has a three-dimensional network structure, high water content and good air permeability, which can absorb wound exudate and keep the wound environment moist. As a three-dimensional water-containing polymer network, hydrogel is very similar to the structure of the extracellular matrix, and the network structure of the hydrogel is adjustable, which is conducive to cell growth. Hydrogel is the most ideal wound dressing at present, but some hydrogel products contain airtight materials such as PE, PP and PVC, which affect the normal breathing of the skin. Long-term use of such materials will cause adverse reactions such as allergies. In addition, traditional hydrogel dressings generally use chemical crosslinking methods. Due to incomplete crosslinking agents or chemical crosslinking reactions, chemical crosslinking methods are prone to residual polymer monomers in the hydrogel network system. These monomers may be toxic to the human body, making it difficult to obtain high-purity crosslinked products. At the same time, uneven crosslinking will occur, and "burning" will occur locally. In addition, chemical crosslinking is difficult to control the degree of crosslinking, which affects the biocompatibility of hydrogels and restricts the application of hydrogels as multifunctional materials. At the same time, hydrogels can be loaded with active components. There are many functional natural antibacterial substances in nature, but a considerable part of them are water-insoluble, including some plant essential oils and plant fat-soluble active ingredients, so they cannot be evenly dispersed in water-based dressings. There is currently no effective way to solve this problem.

[0003] Therefore, how to optimize the biocompatibility and antibacterial properties of wound dressings becomes a technical problem that needs to be solved. Summary of the invention

[0004] The present invention aims to solve at least one of the technical problems existing in the above-mentioned prior art or related technology, and provides a method for preparing an antibacterial composite emulsion gel and an antibacterial dressing, which can form an antibacterial dressing on the skin surface by simple application or direct covering, and has good biocompatibility.

[0005] The first aspect of the present invention discloses a method for preparing an antibacterial composite emulsion gel, comprising: preparing a tri-gluconate solution: dissolving tri-gluconate in water to obtain a completely hydrated tri-gluconate solution, wherein the mass concentration of tri-gluconate in the tri-gluconate solution reaches 0.5% to 1%; adding bacterial cellulose: adding a bacterial cellulose suspension to the tri-gluconate solution, wherein the mass concentration of bacterial cellulose in the final composite suspension reaches 0.1% to 0.5%; adding antibacterial substances: mixing an antibacterial plant essential oil or a magnolol oil solution with the composite suspension, and processing with a homogenizer to produce an emulsified system; heating and hydrating: heating the emulsified system to a first temperature, and adding water to compensate for evaporation losses; cooling and molding: cooling the heated emulsified system to a second temperature to obtain an antibacterial composite emulsion gel.

[0006] In this technical solution, a composite emulsion gel is prepared by using triazole gum as an emulsifier and gelling agent, and nano bacterial cellulose as a suspending agent and dispersing agent in combination with natural plant active ingredients. Different amounts of triazole gum and bacterial cellulose added can obtain emulsion gel samples in different states, which are suitable for application as wound dressings or covering the skin surface.

[0007] According to the method for preparing the antibacterial composite emulsion gel provided by the present invention, preferably, the first temperature is 90°C and the second temperature is 4°C.

[0008] According to the method for preparing the antibacterial composite emulsion gel provided by the present invention, preferably, the mass concentration of Tri-Gel in the Tri-Gel solution is 0.5%, 0.75% or 1%.

[0009] According to the method for preparing the antibacterial composite emulsion gel provided by the present invention, preferably, the mass concentration of bacterial cellulose in the bacterial cellulose suspension is 1%; the mass concentration of bacterial cellulose in the composite suspension is 0.1%, 0.2% or 0.5%.

[0010] According to the method for preparing the antibacterial composite emulsion gel provided by the present invention, preferably, the mass concentration of the antibacterial plant essential oil or magnolol oil solution is 10% to 30%, and the plant essential oil is tea tree essential oil.

[0011] According to the method for preparing the antibacterial composite emulsion gel provided by the present invention, preferably, the step of preparing the tri-zan gum solution specifically comprises: dissolving tri-zan gum powder in deionized water at a temperature of 25° C., and stirring and standing to obtain the tri-zan gum solution.

[0012] According to the method for preparing the antibacterial composite emulsion gel provided by the present invention, preferably, in the step of heating and replenishing water, the water added is deionized water.

[0013] According to the method for preparing the antibacterial composite emulsion gel provided by the present invention, preferably, in the step of adding the antibacterial substance, a homogenizer is used to homogenize the mixture at a speed of 5 m / s for 3 minutes to produce an emulsified system.

[0014] The second aspect of the present invention further discloses an antibacterial composite emulsion gel, which is prepared according to the preparation method of the antibacterial composite emulsion gel disclosed in any of the above technical solutions.

[0015] The third aspect of the present invention also discloses an antibacterial dressing, comprising: applying the antibacterial composite emulsion gel provided by the above technical solution to the skin surface to form an antibacterial dressing by smearing or directly covering; or applying the antibacterial composite emulsion gel as an antibacterial dressing in a bandage product; or applying the antibacterial composite emulsion gel as an antibacterial dressing in surgical supplies.

[0016] The beneficial effects achieved by the present invention include at least: different amounts of trisammonium gum and bacterial cellulose added can obtain emulsion gel samples in different states, which is convenient for controlling the mechanical properties of the final product; the addition of bacterial cellulose significantly improves the hardness, gel strength and elasticity of the composite emulsion gel, indicating that the interaction between bacterial cellulose and trisammonium gum in the composite emulsion gel inhibits the deformation of the material and improves its mechanical properties; trisammonium gum has a good emulsifying effect on vegetable oil, and many oil droplets of different sizes can be obtained, and bacterial cellulose can evenly disperse these oil droplets in the emulsion gel, which helps to evenly distribute the plant antibacterial active ingredients in the dressing and improve the antibacterial properties. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 A schematic diagram showing the effect of different concentrations of bacterial cellulose on the texture properties of antibacterial composite emulsion gel according to an embodiment of the present invention is shown.

[0018] Figure 2 A schematic diagram showing the effect of different concentrations of trisammonia gum on the texture properties of antibacterial composite emulsion gel according to an embodiment of the present invention is shown. DETAILED DESCRIPTION

[0019] In order to more clearly understand the above-mentioned objects, features and advantages of the present invention, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0020] Example 1

[0021] According to one embodiment of the present invention, a method for preparing an antibacterial composite emulsion gel is disclosed, comprising: dissolving tri-glucoside powder in deionized water at 25°C and stirring overnight to ensure complete hydration to obtain a tri-glucoside solution, wherein the tri-glucoside concentration is 0.5% to 1% (w / w); adding a bacterial cellulose suspension (1%, w / w) to the tri-glucoside solution, wherein the bacterial cellulose concentration in the final composite suspension is 0.1% to 0.5% (w / w); mixing (10-30%, w / w) of an antibacterial plant essential oil (tea tree essential oil, etc.) or magnolol oil solution with a tri-glucoside-bacterial cellulose composite liquid, and homogenizing the mixture at a speed of 5 m / s for 3 minutes using a laboratory mixer (Bioprep-24 homogenizer) to produce an emulsified system; heating the emulsified system to 90°C, and adding deionized water to compensate for the weight loss due to evaporation; and finally rapidly cooling the emulsified system to 4°C to prepare an antibacterial composite emulsion gel.

[0022] In this embodiment, a composite emulsion gel is prepared by using triazole gum as an emulsifier and gelling agent, nano bacterial cellulose as a suspending agent and dispersing agent, and combining with natural plant active ingredients. Different amounts of triazole gum and bacterial cellulose added can obtain emulsion gel samples in different states, which are suitable for application as wound dressings or covering the skin surface.

[0023] Example 2

[0024] Another embodiment of the present invention also discloses a specific method for preparing an antibacterial composite emulsion gel, comprising: dissolving tri-glucoside powder in deionized water at 25°C and stirring overnight to ensure complete hydration to obtain a tri-glucoside solution, and testing three tri-glucoside concentrations: 0.5%, 0.75% and 1% (w / w); adding a bacterial cellulose suspension (1%, w / w) to the tri-glucoside solution, and the bacterial cellulose concentrations in the final composite suspension are: 0.1%, 0.2% and 0. .5% (w / w); (10-30%, w / w) antibacterial plant essential oil (tea tree essential oil, etc.) or magnolol oil solution was mixed with tri-zan gum-bacterial cellulose composite liquid, and the mixture was homogenized at a speed of 5m / s for 3min using a laboratory mixer (Bioprep-24 homogenizer) to produce an emulsified system; the emulsified system was heated to 90℃, and deionized water was added to make up for the weight loss due to evaporation; finally, the emulsified system was quickly cooled to 4℃ to prepare an antibacterial composite emulsion gel. The microstructure of the prepared antibacterial composite emulsion gel was observed using an optical microscope. The structure showed that tri-zan gum had a good emulsification effect on plant oil, and many oil droplets of different sizes could be obtained, and bacterial cellulose could evenly disperse these oil droplets in the emulsion gel, which was helpful for the uniform distribution of plant antibacterial active ingredients in the dressing.

[0025] Example 3

[0026] According to another embodiment of the present invention, the effects of different bacterial cellulose addition amounts on the texture properties of the antibacterial composite emulsion gel are disclosed. The gel was prepared as follows: the gum tri-gum powder was dissolved in deionized water at a controlled temperature (25°C) and stirred overnight to ensure complete hydration to obtain a gum tri-gum solution with a concentration of 0.5% (w / w); different proportions of bacterial cellulose suspension (1%, w / w) were added to the gum tri-gum solution to obtain three different bacterial cellulose concentrations in the final composite suspension: 0.1%, 0.2% and 0.5% (w / w); an appropriate amount (10-30%, w / w) of antibacterial plant essential oil (tea tree essential oil, etc.) or magnolol oil solution was mixed with the gum tri-gum-bacterial cellulose composite solution, and the mixture was homogenized at a speed of 5 m / s for 3 minutes using a laboratory mixer (Bioprep-24 homogenizer) to produce an emulsified system; thereafter, the emulsified system was heated to 90°C, and deionized water was added to compensate for the weight loss due to evaporation, and then the emulsified system was quickly cooled to 4°C to prepare an antibacterial composite emulsion gel.

[0027] like Figure 1 As shown, the texture properties of the composite emulsion gel were determined using a TA. XTC texture analyzer. A cylindrical probe (p / 0.5) was used to compress a 2×2 cm (height×width) cylindrical sample to 50%, with a speed of 2.00 mm / s before the test; a test speed of 1.00 mm / s; a speed of 1.00 mm / s after the test; a strain of 75%; and a trigger-type automatic -5g. The resulting full texture analysis (TPA) curve can characterize the hardness, gel strength, brittleness, gelling, adhesion, elasticity, and cohesion of each sample. 0.5%S means that the concentration of tri-zan gum is 0.5%; 0.1%B means that the concentration of bacterial cellulose is 0.1%; 0.2%B means that the concentration of bacterial cellulose is 0.2%; 0.5%B means that the concentration of bacterial cellulose is 0.5%;

[0028] It was found that adding bacterial cellulose at a final concentration of 0.1% (w / w) can significantly improve the hardness, gel strength, brittleness, adhesion and elasticity of the latex gel, but adding higher concentrations will reduce the above properties. In contrast, adhesion, resilience and cohesion are slightly reduced when adding bacterial cellulose at a final concentration of 0.1-0.2% (w / w), while they are improved to a certain extent when adding a final concentration of 0.5% (w / w). Hardness refers to the force required to compress the sample to achieve a given deformation, gel strength is usually related to fracture strength, and elasticity refers to the degree of "rubberiness" of the gel and the degree to which the gel structure breaks during initial compression. The addition of bacterial cellulose significantly improves the hardness, gel strength and elasticity of the composite latex gel, indicating that the interaction between bacterial cellulose and trisammonium gum in the composite latex gel inhibits the deformation of the material and improves its mechanical properties, but too much bacterial cellulose will destroy the original structure of the latex gel and increase the interaction between its two different structures. In general, compared with ordinary hydrogel dressings, the texture properties of the Sanzan gum-bacterial cellulose composite emulsion gel material can be regulated by the amount of bacterial cellulose added, and therefore has a wider range of application scenarios.

[0029] Example 4

[0030] According to another embodiment of the present invention, the effects of different amounts of trisammonium chloride added on the texture properties of the antibacterial composite emulsion gel are disclosed. The gel was prepared as follows: the gum succinate powder was dissolved in deionized water at a controlled temperature (25°C) and stirred overnight to ensure complete hydration to obtain a gum succinate solution, and three gum succinate concentrations were tested: 0.5%, 0.75%, and 1% (w / w); a bacterial cellulose suspension (1%, w / w) was added to the gum succinate solution to obtain a bacterial cellulose concentration of 0.1% (w / w) in the final composite suspension; an appropriate amount (10-30%, w / w) of antibacterial plant essential oil (tea tree essential oil, etc.) or magnolol oil solution was mixed with the gum succinate-bacterial cellulose composite solution, and the mixture was homogenized at a speed of 5 m / s for 3 minutes using a laboratory mixer (Bioprep-24 homogenizer) to produce an emulsified system; thereafter, the emulsified system was heated to 90°C, and deionized water was added to compensate for the weight loss due to evaporation, and then the emulsified system was quickly cooled to 4°C to prepare an antibacterial composite emulsion gel.

[0031] like Figure 2As shown, the texture properties of the composite emulsion gel were determined by a TA. XTC texture analyzer using a cylindrical probe (p / 0.5). The cylindrical sample of 2×2 cm (height×width) was compressed to 50%, with a speed of 2.00 mm / s before the test; a test speed of 1.00 mm / s; a speed of 1.00 mm / s after the test; a strain of 75%; and a trigger-type automatic-5g. The resulting full texture analysis (TPA) curve can characterize the hardness, gel strength, brittleness, gelling, adhesion, elasticity, and cohesion of each sample. 0.5%S means that the concentration of tri-zan gum is 0.5%; 0.75%S means that the concentration of tri-zan gum is 0.75%; 1%S means that the concentration of tri-zan gum is 1%; 0.1%B means that the concentration of bacterial cellulose is 0.1%;

[0032] It was found that adding 0.75% (w / w) tri-gluconate to a final concentration of 3% (w / w) can prepare a composite latex gel with the highest hardness, gel strength and brittleness. Its adhesiveness, adhesion, elasticity and cohesion all increase with the increase of tri-gluconate concentration, while the resilience decreases. The texture analysis of tri-gluconate hydrogels with different concentrations showed that its hardness, adhesiveness and elasticity increased significantly with the increase of concentration. When the concentration of tri-gluconate was >0.4%, the elasticity of tri-gluconate hydrogel increased significantly. Therefore, it can be inferred that the concentration of tri-gluconate mainly has a certain effect on the three-dimensional network structure of the composite latex gel. As the concentration increases, the gel network structure is enhanced, its cohesion is increased, and the resilience is also reduced. In addition, the interaction between excessive tri-gluconate concentration and bacterial cellulose will also affect the structure of the composite latex gel.

[0033] Example 5

[0034] According to another embodiment of the present invention, the antibacterial performance detection process of the antibacterial composite emulsion gel is disclosed: Staphylococcus aureus ATCC 29213 and Escherichia coli K-12 MG1655 are used to represent Gram-positive and Gram-negative bacteria, respectively, to test the antibacterial property of the Sanzan gum-bacterial cellulose composite emulsion gel dressing. Take 50 μL of Staphylococcus aureus and Escherichia coli from the glycerol tube and inoculate them into 5mL LB test tubes respectively, and shake (200rpm) and culture for 12h at 37°C. Add 1mL of bacterial suspension to 100mL of LB solid culture medium (1.5% agar) melted and cooled to a suitable temperature, mix well and pour into a culture dish. After the culture medium solidifies, place the composite emulsion gel dressing with a diameter of about 6mm on LB agar plates containing Staphylococcus aureus and Escherichia coli, respectively, and after culturing at 37°C for 12h, observe the antibacterial effect and measure the diameter of the antibacterial circle. Using this method for testing, it was found that the addition of magnolia officinalis or tea tree essential oil gave the tri-zan gum-bacterial cellulose composite emulsion gel dressing antibacterial activity, among which magnolia officinalis had a strong inhibitory effect on Gram-positive bacteria and a weak inhibitory effect on Gram-negative bacteria, while tea tree essential oil had no obvious inhibitory effect on Gram-positive bacteria and a weak inhibitory effect on Gram-negative bacteria. This shows that the strategy of using tri-zan gum as an emulsifier and gelling agent, nano bacterial cellulose as a suspending agent and dispersing agent, and combining them with natural plant active ingredients to obtain an antibacterial composite emulsion gel is successful.

[0035] In summary, the present invention proposes and confirms a technical solution of using tri-zan gum as an emulsifier and gelling agent, nano bacterial cellulose as a suspending agent and dispersing agent, and combining with natural plant active ingredients to obtain an antibacterial composite emulsion gel. The basic structure and mechanical properties of the tri-zan gum-bacterial cellulose composite emulsion gel dressing were characterized by microscopic observation and testing of texture properties, and its antibacterial activity against Gram-positive bacteria and Gram-negative bacteria was tested. The effectiveness of the new strategy for preparing composite emulsion gels has been demonstrated, and due to the widespread presence of fat-soluble natural products rich in different functions such as antibacterial, this technical solution has broad application prospects.

[0036] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for preparing an antibacterial composite emulsion gel, characterized in that: include: Preparing a trimethoprim solution: dissolving trimethoprim in water to obtain a completely hydrated trimethoprim solution, wherein the mass concentration of trimethoprim in the trimethoprim solution reaches 0.5% to 1%; Adding bacterial cellulose: adding bacterial cellulose suspension to the tri-zan gum solution, so that the mass concentration of the bacterial cellulose in the final composite suspension reaches 0.1% to 0.5%; Adding antibacterial substances: mixing the antibacterial plant essential oil or magnolol oil solution with the composite suspension, and processing with a homogenizer to produce an emulsified system; Heating and replenishing water: heating the emulsified system to a first temperature and adding water to compensate for evaporation loss; Cooling molding: cooling the heated emulsified system to a second temperature to obtain an antibacterial composite emulsion gel.

2. The method for preparing the antibacterial composite emulsion gel according to claim 1, characterized in that: The first temperature is 90°C, and the second temperature is 4°C.

3. The method for preparing the antibacterial composite emulsion gel according to claim 1, characterized in that: The mass concentration of Tri-gluconate in the Tri-gluconate solution is 0.5%, 0.75% or 1%.

4. The method for preparing the antibacterial composite emulsion gel according to claim 1, characterized in that: The mass concentration of bacterial cellulose in the bacterial cellulose suspension is 1%; the mass concentration of bacterial cellulose in the composite suspension is 0.1%, 0.2% or 0.5%.

5. The method for preparing the antibacterial composite emulsion gel according to claim 1, characterized in that: The mass concentration of the antibacterial plant essential oil or the magnolol oil solution is 10% to 30%, and the plant essential oil is tea tree essential oil.

6. The method for preparing the antibacterial composite emulsion gel according to claim 1, characterized in that: The step of preparing the tri-zan gum solution specifically comprises: At 25° C., the Sanzan gum powder was dissolved in deionized water, and stirred and allowed to stand to obtain the Sanzan gum solution.

7. The method for preparing the antibacterial composite emulsion gel according to claim 1, characterized in that: In the step of heating and replenishing water, the water added is deionized water.

8. The method for preparing the antibacterial composite emulsion gel according to claim 1, characterized in that: In the step of adding the antibacterial substance, the mixture is homogenized at a speed of 5 m / s for 3 minutes using a homogenizer to produce an emulsified system. 9 . The antibacterial composite emulsion gel obtained by the method for preparing the antibacterial composite emulsion gel according to claim 1 .

10. An antibacterial dressing, characterized in that: include: The antibacterial composite emulsion gel as claimed in claim 9.

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