A puncture needle with a nano-silver coating and a preparation method thereof

Abstract

The application provides a puncture needle with a nano-silver coating and a preparation method thereof, and belongs to the technical field of biomaterial processing, and comprises the following steps: (1) preparing a graphene solution, adding catechin and tannic acid to obtain a mixed graphene solution; (2) preparing a silver-ammonia solution, mixing the silver-ammonia solution with the mixed graphene solution, and then irradiating under ultraviolet light to obtain a graphene-nano-silver solution; (3) etching the puncture needle, then immersing the etched puncture needle into a dopamine solution, and water-bath heating to form a thin film on the surface of the puncture needle; and (4) immersing the puncture needle with the dopamine thin film into the graphene-nano-silver solution, and stirring to obtain a puncture needle with a nano-silver antibacterial coating. The method can form a nano-silver coating with uniform thickness, the treated puncture needle has good antibacterial performance, can effectively inhibit escherichia coli and staphylococcus aureus, reduces the occurrence of bacterial infection, and has high safety.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of biological material processing, and particularly relates to a puncture needle with a nano-silver coating and a preparation method thereof. BACKGROUND

[0002] The puncture needle is a medical instrument for sampling and injection treatment of tissues of various organs such as kidney, liver, lung, breast, thyroid, prostate, pancreas, testis, uterus, ovary and body surface in minimally invasive surgery. In the detection and treatment of different diseases, the puncture needle can play a good auxiliary role. However, as a full-metal product, the puncture needle belongs to an invasive treatment method, and is prone to cause local skin redness, swelling and pain and bacterial infection or related complications, so it is desirable to improve the safety of the puncture needle.

[0003] Silver is a traditional bacteriostatic agent. Compared with ordinary silver particles, the specific surface area of nano-silver particles increases sharply, the contact area with bacteria increases, and the antibacterial performance also increases sharply. However, nano-materials generally have the characteristics of easy agglomeration, and it is difficult to form a uniform coating, which affects the bacteriostatic performance of nano-silver.

[0004] Therefore, it is desirable to provide a treatment method for a puncture needle, which improves the bacteriostatic property and stability of the coating of the puncture needle, reduces the risk of bacterial infection, and improves the safety of the puncture needle. SUMMARY

[0005] The present application aims to provide a puncture needle with a nano-silver antibacterial coating, which improves the antibacterial performance and safety of the puncture needle.

[0006] In order to achieve the above-mentioned application purposes, the present application provides the following technical solutions:

[0007] The present application provides a preparation method of a puncture needle with a nano-silver antibacterial coating, comprising the following steps:

[0008] (1) preparing a graphene solution, adding catechin and tannic acid to obtain a mixed graphene solution;

[0009] (2) preparing a silver-ammonia solution, mixing the silver-ammonia solution with the mixed graphene solution and then irradiating under ultraviolet light to obtain a graphene-nano-silver solution;

[0010] (3) etching the puncture needle, then immersing the etched puncture needle in a dopamine solution and water-bath heating to form a thin film on the surface of the puncture needle;

[0011] (4) immersing the puncture needle with the dopamine thin film in the graphene-nano-silver solution and stirring to obtain a puncture needle with a nano-silver antibacterial coating.

[0012] Preferably, the mass concentration of the graphene solution in step (1) is 0.8-1.2 mg / mL, the addition amount of catechin is 5-10 mg / mL, and the addition amount of tannic acid is 20-30 mg / mL.

[0013] Preferably, the graphene in step (1) is graphene oxide.

[0014] Preferably, the preparation method of the silver ammine solution in step (2) is as follows: 250-300 mg of silver nitrate is placed in 100-150 mL of water, and then 5-10% ammonia water by mass fraction is added dropwise until the silver nitrate solid completely disappears, to obtain the silver ammine solution.

[0015] Preferably, the mixing ratio of the silver ammine solution to the graphene solution in step (2) is 1-3:1-3.

[0016] Preferably, the wavelength range of the ultraviolet light in step (2) is 260-280 nm, and the irradiation time is 1.0-1.5 h.

[0017] Preferably, the etching in step (3) is chemical etching, and the etching method is as follows: the puncture needle is soaked in a hydrofluoric acid solution with a concentration of 40-50 wt% for 0.5-1 h, and then dried.

[0018] Preferably, the concentration of the dopamine solution in step (3) is 2-3 mg / mL.

[0019] Preferably, the temperature of the water bath heating is 60-80℃, and the time is 4-6 h.

[0020] Preferably, the immersion time in step (4) is 3-6 h, the temperature is 25-30℃, and the stirring speed is 100-200 rpm.

[0021] The application also provides a puncture needle with a nano-silver antibacterial coating prepared by the above preparation method.

[0022] The application uses graphene as a carrier and an antibacterial material, which is beneficial to increase the dispersion stability of nano-silver particles and form a uniform nano-silver coating. Meanwhile, graphene is also an antibacterial material. After graphene oxide and nano-silver are mixed as coating materials in a suitable ratio, the two can further increase the antibacterial effect by mutual cooperation. In the application, catechin and tannic acid are used in combination and subjected to appropriate ultraviolet irradiation, which is helpful to reduce and chelate the dispersed nano-silver particles, form a coating with uniform texture, and improve the antibacterial capacity.

[0023] The puncture needle with nano-silver antibacterial coating provided by the present invention has a uniform coating thickness of 0.01 to 0.02 mm and good antibacterial performance. The antibacterial rate of Escherichia coli is 97 to 99%, and the antibacterial rate of Staphylococcus aureus is 96 to 98%. It can effectively reduce the occurrence of bacterial infection and has high safety. DETAILED DESCRIPTION

[0024] The technical solutions provided by the present invention are described in detail below with reference to the embodiments, but they should not be construed as limiting the scope of protection of the present invention.

[0025] Example 1

[0026] A method for preparing a puncture needle with a nano-silver antibacterial coating comprises the following steps:

[0027] (1) preparing a 1 mg / mL graphene oxide solution, adding catechin and tannic acid to the graphene oxide solution, wherein the amount of catechin added is 10 mg / mL and the amount of tannic acid added is 25 mg / mL to obtain a mixed graphene oxide solution;

[0028] (2) taking 250 mg of silver nitrate and placing it in 100 mL of water, then adding 10% ammonia water by mass until the silver nitrate solid completely disappears to obtain a silver ammonia solution, mixing the silver ammonia solution and the mixed graphene oxide solution in a volume ratio of 1:1, pouring the silver ammonia solution into the mixed graphene oxide solution while stirring while pouring, and stirring at a speed of 100 rpm, and then irradiating the mixed solution under 270 nm ultraviolet light for 1.0 h to obtain a graphene-nanosilver solution;

[0029] (3) The puncture needle was immersed in a 50 wt% hydrofluoric acid solution and etched for 1 h, and then dried in an 80°C oven; dopamine crystals were dissolved in a tris buffer solution with a pH of 8.5 to obtain a dopamine solution with a concentration of 2 mg / ml, and the etched puncture needle was then immersed in the dopamine solution and heated in an 80°C water bath for 6 h to form a thin film on the surface of the puncture needle;

[0030] (4) Immerse the puncture needle with the dopamine film in the graphene-nanosilver solution and stir at 30° C. and 100 rpm for 6 h to obtain a puncture needle with a nanosilver antibacterial coating. The nanosilver antibacterial coating has a thickness of 0.017 mm.

[0031] Example 2

[0032] A method for preparing a puncture needle with a nano-silver antibacterial coating comprises the following steps:

[0033] (1) preparing a graphene oxide solution with a mass concentration of 1 mg / mL, adding catechin and tannic acid to the graphene oxide solution, wherein the amount of catechin added is 5 mg / mL and the amount of tannic acid added is 30 mg / mL, to obtain a mixed graphene oxide solution;

[0034] (2) taking 250 mg of silver nitrate and placing it in 150 mL of water, then adding ammonia water with a mass fraction of 10% until the silver nitrate solid completely disappears to obtain a silver ammonia solution, which is mixed with the mixed graphene oxide solution prepared in step (1) in a volume ratio of 1:1, pouring the silver ammonia solution into the mixed graphene oxide solution while stirring while pouring, and the stirring speed is 100 rpm, and then placing the mixed solution under 270 nm ultraviolet light for 1 hour to obtain a graphene-nanosilver solution;

[0035] (3) The puncture needle was immersed in a 50 wt% hydrofluoric acid solution and etched for 0.5 h, and then dried in an 80°C oven; dopamine crystals were dissolved in a tris buffer solution with a pH of 8.5 to obtain a dopamine solution with a concentration of 2 mg / ml, and the etched puncture needle was then immersed in the dopamine solution and heated in an 80°C water bath for 4 h to form a thin film on the surface of the puncture needle;

[0036] (4) Immerse the puncture needle with the dopamine film in the graphene-nanosilver solution and stir at 30° C. and 100 rpm for 5 h to obtain a puncture needle with a nanosilver antibacterial coating having a thickness of 0.015 mm.

[0037] Example 3

[0038] A method for preparing a puncture needle with a nano-silver antibacterial coating comprises the following steps:

[0039] (1) preparing a graphene oxide solution with a mass concentration of 1.2 mg / mL, adding catechin and tannic acid to the graphene oxide solution, wherein the amount of catechin added is 10 mg / mL and the amount of tannic acid added is 20 mg / mL, to obtain a mixed graphene oxide solution;

[0040] (2) taking 300 mg of silver nitrate and placing it in 150 mL of water, then adding 10% ammonia water by mass until the silver nitrate solid completely disappears, thereby obtaining a silver ammonia solution; mixing the prepared silver ammonia solution and the mixed graphene oxide solution prepared in step (1) in a volume ratio of 1:1, and then irradiating the mixture under 270 nm ultraviolet light for 1.5 h to obtain a graphene-nanosilver solution;

[0041] (3) The puncture needle was immersed in a 50 wt% hydrofluoric acid solution and etched for 1 h, and then dried in an 80°C oven; dopamine crystals were dissolved in a tris buffer solution with a pH of 8.5 to obtain a dopamine solution with a concentration of 2 mg / ml, and the etched puncture needle was then immersed in the dopamine solution and heated in an 80°C water bath for 6 h to form a thin film on the surface of the puncture needle;

[0042] (4) Immerse the puncture needle with the dopamine film in the graphene-nanosilver solution and stir at 30° C. and 150 rpm for 6 h to obtain a puncture needle with a nanosilver antibacterial coating having a thickness of 0.012 mm.

[0043] Comparative Example 1

[0044] The difference from Example 1 is that the amounts of catechin and tannic acid added in step (1) are:

[0045] A. Catechin 0 mg / mL, tannic acid 35 mg / mL;

[0046] B. Catechin 35 mg / mL, tannic acid 0 mg / mL;

[0047] C. Catechin 30mg / mL, tannic acid 30mg / mL.

[0048] Comparative Example 2

[0049] The difference from Example 1 is that the volume ratios of the mixed graphene solution and the silver ammonia solution in step (2) are:

[0050] A.0:1;

[0051] B.5:2;

[0052] C.2:5.

[0053] Comparative Example 3

[0054] Different from Example 1, the wavelength range and irradiation time of the ultraviolet light in step (2) are as follows:

[0055] A. The wavelength of ultraviolet light is 270nm and the irradiation time is 3h;

[0056] B. The wavelength of ultraviolet light is 300nm and the irradiation time is 1h;

[0057] C. The wavelength range of ultraviolet light is 200nm and the irradiation time is 1h.

[0058] Test Example 1 Antibacterial Properties

[0059] Test method: Escherichia coli (ATCC 8739) and Staphylococcus aureus (ATCC 6538) were used as test bacteria, and the concentration was 1×10 7 cfu / ml bacterial suspension; Place the puncture needles of different treatment groups (grouping is shown in Table 1, and each group is tested three times) on the culture dish, drip the bacterial suspension so that the bacterial suspension covers the puncture needle, cover it with sterile plastic film to ensure close contact between the bacterial liquid and the stainless steel surface and prevent the evaporation of the bacterial liquid and cause bacterial death, and then culture it in a 37°C incubator for 24 hours. Aspirate the bacterial liquid on the surface of the puncture needle, calculate the number of bacteria A in each group and the number of bacteria B in the control group according to the calculation method in GB 4789.2-2022, and calculate the antibacterial rate according to (1-A / B)×100%. The experimental results are shown in Table 1:

[0060] Table 1 Antibacterial rate of puncture needles treated with different coatings

[0061]

[0062]

[0063] As can be seen from the above examples, the puncture needle with nanosilver antibacterial coating provided by the present invention has good antibacterial properties, with an antibacterial rate of 97-99% against Escherichia coli and 94-98% against Staphylococcus aureus, which is significantly improved compared to Comparative Examples 1 to 3. By comparing Comparative Examples 1 and 3 with the examples of the present application, it is found that the combination of catechin and tannic acid and appropriate ultraviolet light irradiation can enhance the reducing ability of the reaction system, help to reduce and chelate the dispersed nanosilver particles, form a uniform coating, and enhance the antibacterial ability. By comparing Comparative Example 2 with the examples of the present application, it is found that the appropriate mixing ratio of graphene oxide and silver ammonia solution can enhance the dispersibility of nanosilver particles in the solution, reduce the aggregation of nanosilver particles, help to form a uniform coating, and further enhance the antibacterial performance.

[0064] Test Example 2 Acute systemic poisoning test

[0065] The puncture needles with nanosilver antibacterial coatings prepared in Examples 1-3 were immersed in 250 mL of 0.9% sterile sodium chloride solution and maintained at 40°C for 5 hours. The puncture needles were then removed to obtain a test solution. The test solution was then tested using the acute systemic toxicity test method (YBB00042003-2015 Acute Systemic Poisoning Test Method). It was found that no toxic symptoms were observed in Examples 1-3. This indicates that the puncture needles with nanosilver antibacterial coatings prepared in this application have no acute systemic toxicity to humans, and the nanosilver antibacterial coatings provided in this application are highly safe.

[0066] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.

Claims

1. A method for preparing a puncture needle with a nano-silver antibacterial coating, characterized in that: The following steps are involved: (1) preparing a graphene solution, adding catechin and tannic acid to obtain a mixed graphene solution; (2) preparing a silver ammonia solution, mixing the silver ammonia solution with the mixed graphene solution, and irradiating the mixture under ultraviolet light to obtain a graphene-nanosilver solution; (3) Etching the puncture needle, then immersing the etched puncture needle in a dopamine solution and heating it in a water bath to form a thin film on the surface of the puncture needle; (4) immersing the puncture needle with the dopamine film into the graphene-nanosilver solution and stirring to obtain a puncture needle with a nanosilver antibacterial coating; The mass concentration of the graphene solution in step (1) is 0.8-1.2 mg / mL, the amount of catechin added is 5-10 mg / mL, and the amount of tannic acid added is 20-30 mg / mL; The method for preparing the silver ammonia solution in step (2) is as follows: after adding silver nitrate in a ratio of (250-300 mg): (100-150 mL) to water, ammonia water with a mass fraction of 5-10% is added dropwise until the silver nitrate solid disappears completely, thereby obtaining the silver ammonia solution; The volume ratio of the silver ammonia solution to the graphene solution is: 1-3:1-3; The wavelength range of the ultraviolet light in step (2) is 260~280nm, and the irradiation time is: 1.0~1.5h.

2. The method for preparing the puncture needle according to claim 1, wherein: The graphene in step (1) is graphene oxide.

3. The method for preparing the puncture needle according to claim 2, wherein: The etching in step (3) is chemical etching, and the etching method is: immersing the puncture needle in a hydrofluoric acid solution with a concentration of 40-50 wt% for 0.5-1 h and drying.

4. The method for preparing the puncture needle according to claim 3, wherein: The concentration of the dopamine solution in step (3) is 2-3 mg / mL; The water bath is heated at a temperature of 60-80° C. for 4-6 hours.

5. The method for preparing the puncture needle according to claim 4, characterized in that: In step (4), the immersion time is 3 to 6 hours, the temperature is 25 to 30° C., and the stirring speed is 100 to 200 rpm.

6. A puncture needle with a nano-silver antibacterial coating prepared by the preparation method of a puncture needle according to any one of claims 1 to 5.

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