CN113476640B - Preparation method of antibacterial hydrogel dressing containing heterogeneous ion doped metal sulfide - Google Patents
Preparation method of antibacterial hydrogel dressing containing heterogeneous ion doped metal sulfide Download PDFInfo
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- 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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- 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
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- 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
- A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
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- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0004—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form containing inorganic materials
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- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0061—Use of materials characterised by their function or physical properties
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- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0061—Use of materials characterised by their function or physical properties
- A61L26/008—Hydrogels or hydrocolloids
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/41—Anti-inflammatory agents, e.g. NSAIDs
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- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
A preparation method of an antibacterial hydrogel dressing containing heterogeneous ions doped with metal sulfides comprises the following steps: uniformly mixing a metal salt solution and a sulfur source, then carrying out hydrothermal reaction, filtering, washing and drying after the reaction is finished, and obtaining the heterogeneous ion doped metal sulfide nano-particles; the metal salt is selected from at least two of copper chloride, zinc chloride, ferric chloride, cadmium chloride, molybdenum tetrachloride, magnesium chloride and bismuth nitrate; adding the xenogenic ion doped metal sulfide nanoparticles into the aescin sodium solution and uniformly stirring to obtain a mixed solution; and (3) soaking the dressing base material in the mixed solution, and taking out to obtain the antibacterial hydrogel dressing containing the heterogeneous ion doped metal sulfide. According to the invention, the heterogeneous ion doped metal sulfide is used as the antibacterial material of the hydrogel dressing, the prepared hydrogel has good heat resistance, stability and lasting antibacterial property, and the obtained product has obvious bioactivity, biocompatibility and antibacterial effect.
Description
Technical Field
The invention belongs to the technical field of medical materials, and particularly relates to a preparation method of an antibacterial hydrogel dressing containing heterogeneous ions and doped with metal sulfides.
Background
The hydrogel is a polymer with a three-dimensional network structure, can absorb a large amount of water without dissolving, has good flexibility, biocompatibility and the like, and has wide application prospect in the biomedical fields of drug sustained release, tissue engineering, wound repair and the like. In order to prevent bacterial infection, it is important how to prepare hydrogel with antibacterial property.
The patent application with publication number CN 111481735A discloses a medical antibacterial wound-protecting hydrogel dressing and a preparation method thereof, wherein a liquid matrix adhesive and an acrylamide solution are added into a chitosan derivative, then a cross-linking agent, an initiator and an accelerator are sequentially added to form gel, and the excessive cross-linking agent is removed to obtain the hydrogel dressing. Patent application publication No. CN 111363171A discloses an antibacterial hydrogel and a preparation method and application thereof, wherein a cross-linking agent is adopted to chemically cross-link hyaluronic acid to obtain the hydrogel, then hyaluronic acid hydrogel powder is dissolved in PBS to obtain hyaluronic acid microspheres, and the hyaluronic acid microspheres are mixed with a polylysine solution according to a proportion. The patent application with publication number CN 107028919A discloses a compound aescin A, B liposome hydrogel patch, which is composed of aescin A or its salt, aescin B or its salt, and diethylamine salicylate in the proportion of 0.3-1.5: 0.5-1: 2-5, and has better transdermal absorption effect, anti-swelling effect and safety compared with the prior art. Application with publication number CN111249226A discloses an aescin injectable hydrogel, a preparation method and application thereof, chemical modification and auxiliary additives are not needed, the aescin injectable hydrogel can be directly injected for administration, and the sustained release property is good.
In the prior art, antibiotics and natural or organic antibacterial materials are used as antibacterial agents to prepare the antibacterial hydrogel. However, microorganisms are easy to generate drug resistance under the long-term action of antibiotics, although natural antibacterial materials have high safety, the heat resistance is poor, the sterilization rate is low, the antibacterial effect is easy to influence, the heat resistance and the stability of organic antibacterial materials are generally poor, the effective period is short, the organic antibacterial materials are not suitable for a long-term antibacterial process, and the escin sodium hydrogel has a good anti-inflammatory effect but does not have antibacterial property.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background technology and provide a preparation method of an antibacterial hydrogel dressing containing a dissimilar ion doped metal sulfide.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of an antibacterial hydrogel dressing containing a dissimilar ion doped metal sulfide comprises the following steps:
(1) Uniformly mixing a metal salt solution and a sulfur source, then carrying out hydrothermal reaction, filtering, washing and drying after the reaction is finished, and obtaining the heterogeneous ion doped metal sulfide nano-particles; the metal salt is selected from at least two of copper chloride, zinc chloride, ferric chloride, cadmium chloride, molybdenum tetrachloride, magnesium chloride and bismuth nitrate;
(2) Adding the heterogeneous ion doped metal sulfide nanoparticles into the aescine sodium solution and uniformly stirring to obtain a mixed solution;
(3) And (3) soaking the dressing base material in the mixed solution obtained in the step (2), and taking out to obtain the antibacterial hydrogel dressing containing the heterogeneous ion doped metal sulfide.
In the above preparation method, preferably, in the step (1), the sulfur source is one or more selected from thiourea, thioacetamide, sodium sulfide and sulfur powder.
In the preparation method, preferably, in the step (1), the temperature of the hydrothermal reaction is 120-200 ℃, and the time of the hydrothermal reaction is 12-24h.
In the above preparation method, preferably, in the step (1), the concentration of the metal salt solution is 0.01 to 0.5mol/L; the molar ratio of the metal salt to the sulfur source is 1.
In the above preparation method, preferably, in the step (2), the mass concentration of the sodium aescinate solution is 0.1 to 10wt%, and the sodium aescinate solution is obtained by dissolving sodium aescinate powder in 0.1M tris buffer with pH =7.5 to 10.
In the above production method, preferably, in the step (2), the stirring is carried out at 35 to 50 ℃.
In the preparation method, preferably, in the step (3), the soaking time is 15-45min.
In the above preparation method, preferably, in the step (1), the metal salt solution is a mixed solution of a metal salt a and a metal salt B, wherein the metal salt a is any one of copper chloride, zinc chloride, ferric chloride, cadmium chloride, molybdenum tetrachloride, magnesium chloride and bismuth nitrate, and the metal salt B is at least one selected from the group consisting of copper chloride, zinc chloride, ferric chloride, cadmium chloride, molybdenum tetrachloride, magnesium chloride and bismuth nitrate; and the metal salt A and the metal salt B are different.
In the above production method, preferably, the molar ratio of the metal salt a to the metal salt B is (5-10): 1, metal salt a provides the main metal and metal salt B provides the dopant metal.
In the preparation method, preferably, in the step (2), the addition amount of the heteroionic doped metal sulfide nanoparticles accounts for 5-15% of the mass of the aescine sodium.
The metal ions in the antibacterial hydrogel dressing containing the heterogeneous ion doped metal sulfide can be continuously dissolved out, the dissolution rate of the heterogeneous ion doped metal sulfide can be improved, and the antibacterial effect of the hydrogel dressing is ensured to have durability.
Compared with the prior art, the invention has the advantages that:
(1) According to the invention, the metal sulfide doped with the heterogeneous ions is used as the antibacterial material of the hydrogel dressing, the prepared hydrogel has good heat resistance, stability and lasting antibacterial property, and the obtained product has obvious bioactivity, biocompatibility and antibacterial effect.
(2) According to the invention, the metal sulfide doped with the heterogeneous ions is used as the antibacterial material of the hydrogel dressing, the metal sulfide can improve the dissolution rate of the metal ions in a doping modification mode, the antibacterial performance of the material is effectively enhanced, and the antibacterial rate of the antibacterial hydrogel dressing can reach 99.9% by adding less heterogeneous ion doped metal sulfide.
(3) The antibacterial hydrogel dressing can be applied to various skin wounds and has the functions of antibiosis and antiphlogosis.
Drawings
Fig. 1 is an XRD diffractogram of the zinc-doped copper sulphide nanoparticles prepared in example 1 of the present invention.
Fig. 2 is an SEM image of the antibacterial hydrogel dressing prepared in example 1 of the present invention after soaking in the SBF solution for 7 days.
Fig. 3 is an SEM image of the antibacterial hydrogel dressing prepared in comparative example 1 of the present invention after soaking in SBF solution for 7 days.
Fig. 4 is an SEM image of the antibacterial hydrogel dressing prepared in example 2 of the present invention after soaking in the SBF solution for 7 days.
Fig. 5 is an SEM image of the antibacterial hydrogel dressing prepared in comparative example 3 of the present invention after soaking in the SBF solution for 7 days.
Fig. 6 is an SEM image of the antibacterial hydrogel dressing prepared in example 3 of the present invention after soaking in the SBF solution for 7 days.
FIG. 7 is a graph showing the results of the cell compatibility test of the antibacterial hydrogel dressings of examples 1 to 3, the blank control group, and comparative examples 1 and 3.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically indicated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the invention relates to a preparation method of an antibacterial hydrogel dressing containing a dissimilar ion doped metal sulfide, which comprises the following steps:
(1) Preparing zinc-doped copper sulfide nano particles: adding zinc chloride into a copper chloride aqueous solution with the concentration of 0.1mol/L, wherein the molar ratio of the zinc chloride to the copper chloride is 1; the XRD pattern is shown in figure 1, the peaks in the pattern are consistent with the characteristic peak of copper sulfide (JCPDF No. 06-0464), and impurity phases such as zinc sulfide and the like are not generated;
(2) Preparing the antibacterial hydrogel dressing: dissolving 0.2g of sodium aescinate powder in 10mL of 0.1M Tris buffer solution with pH =8, adding 10mg of zinc-doped copper sulfide nanoparticles, and stirring at 35 ℃ to uniformly mix the zinc-doped copper sulfide nanoparticles;
(3) And (3) soaking medical gauze in the mixed solution obtained in the step (2), standing and soaking for 30 minutes, and taking out to obtain the zinc-doped copper sulfide-containing antibacterial hydrogel dressing.
The zinc-doped copper sulfide-containing antibacterial hydrogel dressing prepared in the embodiment is soaked in an SBF solution, the concentrations of calcium ions and phosphorus ions in the solution are reduced after the soaking for 7 days, and as shown in fig. 2, osteoid apatite is deposited on the surface of a sample, so that the dressing has good in-vitro biological activity.
The antibacterial hydrogel dressing containing zinc and copper sulfide is subjected to antibacterial test, target strains are escherichia coli and staphylococcus aureus, after 24 hours of culture, a bacteriostatic ring is formed around a sample, and the bacteriostatic rate reaches 99.6%.
Cell compatibility tests are carried out on the zinc-doped copper sulfide-containing antibacterial hydrogel dressing prepared in the embodiment, the results are shown in fig. 7, the used cells are human osteogenic sarcoma MG-63 cells, and the cell adhesion rate after 24-hour culture is higher than that of a blank control group, which shows that the antibacterial dressing has no toxicity to MG-63 cells.
Comparative example 1:
the comparative example prepared the preparation method of the antibacterial hydrogel dressing containing copper sulfide nanoparticles, which is different from the preparation method of example 1 in that the copper sulfide nanoparticles are prepared in the step (1), and other processes are the same and specifically as follows:
(1) Preparing copper sulfide nanoparticles: adding 0.1mol/L thiourea aqueous solution into 0.1mol/L copper chloride aqueous solution, stirring and mixing uniformly, carrying out hydrothermal reaction for 18 hours at 160 ℃, filtering and collecting a product, washing and drying to obtain copper sulfide nanoparticles;
(2) Preparing the antibacterial hydrogel dressing: dissolving 0.2g of aescine sodium powder in 10mL of 0.1M PBS buffer solution, adding 10mg of the copper sulfide nano-particles prepared in the step (1), and stirring at 35 ℃ to uniformly mix the copper sulfide nano-particles;
(3) And (3) soaking medical gauze in the mixed solution obtained in the step (2), standing and soaking for 30 minutes, and taking out to obtain the copper sulfide-containing antibacterial hydrogel dressing.
After the antibacterial hydrogel dressing prepared in the comparative example is soaked in the SBF solution for 7 days, the deposition of bone-like apatite on the surface of the sample can be observed in figure 3, and the in vitro biological activity of the dressing is proved to be good.
The antibacterial hydrogel dressing containing copper sulfide prepared in the comparative example is subjected to an antibacterial test, the target strains are escherichia coli and staphylococcus aureus, and the antibacterial rate after 24-hour culture is 98.2% and is smaller than that of the sample in example 1.
Cell compatibility tests are carried out on the antibacterial hydrogel dressing prepared by the comparative example, the results are shown in figure 7, the used cells are human osteogenic sarcoma MG-63 cells, and the cell adhesion rate is higher than that of a blank control group after 24-hour culture, namely the antibacterial dressing has no toxicity to MG-63 cells.
Comparative example 2:
the comparison example verifies that the antibacterial performance of the copper sulfide can be improved by doping modification, and the specific process comprises the following steps:
(1) Preparing copper sulfide nanoparticles: adding 0.1mol/L thiourea aqueous solution into 0.1mol/L copper chloride aqueous solution, stirring and mixing uniformly, carrying out hydrothermal reaction for 18 hours at 160 ℃, filtering and collecting a product, washing and drying to obtain copper sulfide nanoparticles;
(2) Preparing zinc-doped copper sulfide nano particles: adding zinc chloride into a copper chloride aqueous solution with the concentration of 0.1mol/L, wherein the molar ratio of the zinc chloride to the copper chloride is 1;
the prepared copper sulfide and zinc-doped copper sulfide are respectively subjected to antibacterial tests, target strains are escherichia coli and staphylococcus aureus, the culture time is 24 hours, when the test concentrations of samples are all 0.05mg/mL, the bacteriostatic rates of the copper sulfide and zinc-doped copper sulfide are respectively 98.7% and 100%, and when the test concentration of the copper sulfide is increased to 0.1mg/mL, the bacteriostatic rate can reach 99.9%. The comparison proves that the antibacterial performance of the copper sulfide can be improved by doping modification.
Example 2:
the preparation method of the antibacterial hydrogel dressing containing the xenogenous ion doped metal sulfide comprises the following steps:
(1) Preparing magnesium-doped zinc sulfide nanoparticles: adding magnesium chloride into a zinc chloride aqueous solution with the concentration of 0.1mol/L, wherein the molar ratio of the magnesium chloride to the zinc chloride is 1.
(2) Preparing the antibacterial hydrogel dressing: dissolving 0.5g sodium aescinate powder in 10mL of 0.1M Tris buffer (pH = 8), adding 50mg magnesium-doped zinc sulfide nanoparticles, and stirring at 50 ℃ to mix them uniformly;
(3) And (3) soaking the medical bandage in the mixed solution obtained in the step (2), standing for 40 minutes, and taking out to obtain the magnesium-doped zinc sulfide-containing antibacterial hydrogel dressing.
The antibacterial hydrogel dressing containing magnesium and zinc sulfide is soaked in the SBF solution for 7 days, the concentration of calcium and phosphorus ions in the solution is reduced, and as shown in figure 4, osteoid apatite is deposited on the surface of the sample, so that the in vitro bioactivity of the dressing is proved to be good.
The magnesium-doped zinc sulfide-containing antibacterial hydrogel dressing prepared in the embodiment is subjected to an antibacterial test, target strains are escherichia coli and staphylococcus aureus, after 24 hours of culture, a bacteriostatic ring is formed around a sample, and the bacteriostatic rate reaches 99.9%.
Cell compatibility tests are carried out on the magnesium-doped zinc sulfide antibacterial hydrogel dressing prepared in the embodiment, the results are shown in fig. 7, the used cells are human osteogenic sarcoma MG-63 cells, and the cell adhesion rate after 24-hour culture is higher than that of a blank control group, which shows that the antibacterial dressing has no toxicity to MG-63 cells.
Comparative example 3:
the preparation method of the antibacterial hydrogel dressing of the comparative example comprises the following steps:
(1) Respectively preparing magnesium sulfide and zinc sulfide nanoparticles: adding 0.1mol/L aqueous solution of sodium sulfide (the molar ratio of zinc chloride to sodium sulfide is 1.
(2) Preparing the antibacterial hydrogel dressing: dissolving 0.5g of aescine sodium powder in 10mL of 0.1M PBS buffer solution (pH = 8), adding 4.5mg of magnesium sulfide nanoparticles and 45.5mg of zinc sulfide nanoparticles, and stirring at 50 ℃ to mix them uniformly;
(3) And (3) soaking the medical bandage in the mixed solution obtained in the step (2), standing for 40 minutes, and taking out to obtain the antibacterial hydrogel dressing containing magnesium sulfide and zinc sulfide.
The antibacterial hydrogel dressing obtained in the comparative example is soaked in the SBF solution for 7 days, the concentrations of calcium and phosphorus ions in the solution are reduced, and as shown in figure 5, the osteoid apatite is deposited on the surface of the sample, which proves that the dressing has good in vitro biological activity.
The antibacterial hydrogel dressing prepared by the comparative example is subjected to an antibacterial test, the target strains are escherichia coli and staphylococcus aureus, and the bacteriostasis rate reaches 98.8 percent after the dressing is cultured for 24 hours and is less than that of the sample in example 2.
The cell compatibility test is carried out on the antibacterial hydrogel dressing prepared by the comparative example, the result is shown in figure 7, the used cells are human osteogenic sarcoma MG-63 cells, the cell adhesion rate after 24h culture is higher than that of a blank control group, and the antibacterial hydrogel dressing has no toxicity to MG-63 cells.
Example 3:
the invention relates to a preparation method of an antibacterial hydrogel dressing containing a dissimilar ion doped metal sulfide, which comprises the following steps:
(1) Preparing copper-zinc doped cadmium sulfide nanoparticles: water in a volume ratio of 1: the ethanol mixed solution is used as a solvent to prepare a cadmium chloride solution with the concentration of 0.1mol/L, then zinc chloride and copper chloride are added into the solution, the molar ratio of the zinc chloride to the copper chloride to the cadmium chloride is 1.
(2) Preparing the antibacterial hydrogel dressing: dissolving 1g of aescine sodium powder in 10mL of 0.1M Tris buffer solution (pH = 8), adding 50mg of copper-zinc doped cadmium sulfide nanoparticles, stirring at 35 ℃ to uniformly mix, then soaking gauze in the mixed solution, standing and soaking for 30 minutes, and taking out the gauze to obtain the copper-zinc doped cadmium sulfide-containing antibacterial hydrogel dressing.
The obtained antibacterial hydrogel dressing is soaked in SBF solution for 7 days, the concentration of calcium and phosphorus ions in the solution is reduced, and osteoid apatite is deposited on the surface of a sample as shown in figure 6, so that the dressing has good in-vitro biological activity.
The antibacterial hydrogel dressing prepared in the embodiment is subjected to an antibacterial test, target strains are escherichia coli and staphylococcus aureus, after the target strains are cultured for 24 hours, a bacteriostatic ring is formed around a sample, and the bacteriostatic rate reaches 99.9%.
Cell compatibility tests are carried out on the antibacterial hydrogel dressing prepared in the embodiment, the results are shown in figure 7, the used cells are human osteosarcoma MG-63 cells, and the cell adhesion rate is higher than that of a blank control group after 24h of culture, namely the antibacterial hydrogel dressing has no toxicity on MG-63 cells.
Claims (8)
1. A preparation method of an antibacterial hydrogel dressing containing heterogeneous ions doped with metal sulfides is characterized by comprising the following steps:
(1) Uniformly mixing a metal salt solution and a sulfur source, then carrying out hydrothermal reaction, filtering, washing and drying after the reaction is finished, and obtaining the heterogeneous ion doped metal sulfide nano-particles; the metal salt is selected from at least two of copper chloride, zinc chloride, ferric chloride, cadmium chloride, molybdenum tetrachloride, magnesium chloride and bismuth nitrate; the metal salt solution is a mixed solution of a metal salt A and a metal salt B, wherein the metal salt A is any one of copper chloride, zinc chloride, ferric chloride, cadmium chloride, molybdenum tetrachloride, magnesium chloride and bismuth nitrate, the metal salt B is at least one selected from the group consisting of copper chloride, zinc chloride, ferric chloride, cadmium chloride, molybdenum tetrachloride, magnesium chloride and bismuth nitrate, and the molar ratio of the metal salt A to the metal salt B is (5-10): 1;
(2) Adding the heterogeneous ion doped metal sulfide nanoparticles into the aescine sodium solution and uniformly stirring to obtain a mixed solution;
(3) And (3) soaking the dressing base material in the mixed solution obtained in the step (2), and taking out to obtain the antibacterial hydrogel dressing containing the dissimilar ion doped metal sulfide.
2. The method according to claim 1, wherein in the step (1), the sulfur source is one or more selected from the group consisting of thiourea, thioacetamide, sodium sulfide and sulfur powder.
3. The preparation method according to claim 1, wherein in the step (1), the temperature of the hydrothermal reaction is 120 to 200 ℃ and the time of the hydrothermal reaction is 12 to 24 hours.
4. The production method according to claim 1, wherein in the step (1), the concentration of the metal salt solution is 0.01 to 0.5mol/L; the molar ratio of the metal salt to the sulfur source is 1.
5. The method according to any one of claims 1 to 4, wherein in the step (2), the concentration by mass of the sodium aescinate solution is 0.1 to 10wt%, and the sodium aescinate solution is obtained by dissolving sodium aescinate powder in 0.1M Tris buffer with pH =7.5 to 10.
6. The method according to any one of claims 1 to 4, wherein in the step (2), the stirring is carried out at 35 to 50 ℃.
7. The method according to any one of claims 1 to 4, wherein in the step (3), the soaking time is 15 to 45min.
8. The preparation method according to any one of claims 1 to 4, wherein in the step (2), the amount of the heteroionic doped metal sulfide nanoparticles added is 5 to 15% by mass of the sodium aescinate.
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