Puncture needle with nano-silver coating and preparation method thereof

Abstract

The invention provides a puncture needle with a nano-silver coating and a preparation method thereof, and belongs to the technical field of biological material processing, the preparation method comprises the following steps: (1) preparing a graphene solution, and adding catechinic acid 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 under ultraviolet light to obtain a graphene-nano silver solution; (3) etching the puncture needle, immersing the etched puncture needle into a dopamine solution, and heating in a water bath to form a layer of film on the surface of the puncture needle; and (4) immersing a puncture needle with a dopamine film into the graphene-nano-silver solution, and stirring to obtain the puncture needle with the nano-silver antibacterial coating. According to the method, the nano-silver coating with the uniform thickness can be formed, the treated puncture needle is good in antibacterial performance, escherichia coli and staphylococcus aureus can be effectively inhibited, the situation of bacterial infection is reduced, and safety is high.

Description

Technical Field

[0001] The invention relates to the technical field of biomaterial processing, and in particular to a puncture needle with a nano silver coating and a preparation method thereof. Background Art

[0002] The puncture needle is a medical device used for tissue sampling and injection treatment of various organs such as kidney, liver, lung, breast, thyroid, prostate, pancreas, testicle, uterus, ovary, body surface, etc. in minimally invasive surgery. It can play a good auxiliary role in the detection and treatment of different diseases. However, as a full metal product, the puncture needle is an invasive treatment method, which is very likely to cause symptoms such as local skin redness, swelling and pain, and is also prone to bacterial infection or related complications. Therefore, it is hoped that the safety of the use of the puncture needle can be improved.

[0003] Silver is a traditional antibacterial agent. Compared with ordinary silver particles, the specific surface area of ​​nanosilver particles increases dramatically, which increases the contact area with bacteria and increases the antibacterial properties. However, nanomaterials generally have the characteristic of easy agglomeration and are not easy to form a uniform coating, which affects the antibacterial properties of nanosilver.

[0004] Therefore, it is hoped that a method for treating a puncture needle can be provided to reduce the risk of bacterial infection and improve the safety of the puncture needle by improving the antibacterial property and stability of the puncture needle coating. Summary of the invention

[0005] The purpose of the present invention is to provide a puncture needle with a nano-silver antibacterial coating to improve the antibacterial performance and safety of the puncture needle.

[0006] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0007] The present invention provides a method for preparing 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 irradiating the mixture under ultraviolet light to obtain a graphene-nanosilver solution;

[0010] (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;

[0011] (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.

[0012] Preferably, 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.

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

[0014] Preferably, the preparation method of the silver ammonia solution in step (2) is: taking 250-300 mg of silver nitrate and placing it in 100-150 mL of water, and then dripping ammonia water with a mass fraction of 5-10% until the silver nitrate solid disappears completely, thereby obtaining the silver ammonia solution.

[0015] Preferably, the mixing ratio of the silver ammonia solution and 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: immersing the puncture needle in a hydrofluoric acid solution with a concentration of 40 to 50 wt% for 0.5 to 1 hour, and drying.

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

[0019] Preferably, the water bath heating temperature is 60-80° C., and the heating time is 4-6 hours.

[0020] Preferably, 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.

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

[0022] The present invention uses graphene as a carrier and an antibacterial material, which is beneficial to increasing the dispersion stability of nanosilver particles and forming a uniform nanosilver coating. At the same time, graphene is also an antibacterial material. After graphene oxide and nanosilver are mixed in a suitable ratio as a coating material, the two can cooperate with each other to further increase the antibacterial effect. In the present invention, catechin and tannic acid are used in combination and properly irradiated with ultraviolet light, which is helpful to reduce and chelate the dispersed nanosilver particles, form a coating with uniform texture, and enhance the antibacterial ability.

[0023] The puncture needle with nano silver antibacterial coating provided by the present invention has a uniform coating thickness of 0.01-0.02 mm, good antibacterial performance, an antibacterial rate of 97-99% for Escherichia coli, and an antibacterial rate of 96-98% for Staphylococcus aureus, which 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 in conjunction with the embodiments, but they should not be construed as limiting the protection scope 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 dropping ammonia water with a mass fraction of 10% 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, and the stirring speed is 100 rpm, and then placing 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 for etching for 1 h, and then dried in an oven at 80°C; 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 then the etched puncture needle was immersed in the dopamine solution and heated in a water bath at 80°C 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, stir at 30° C. and 100 rpm for 6 hours, and obtain a puncture needle with a nanosilver antibacterial coating having 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, and mixing the silver ammonia solution with the mixed graphene oxide solution prepared in step (1) at a volume ratio of 1:1, pouring the silver ammonia solution into the mixed graphene oxide solution while stirring, and the stirring speed is 100 rpm, and then irradiating the mixed solution under 270 nm ultraviolet light for 1 h to obtain a graphene-nanosilver solution;

[0035] (3) The puncture needle was immersed in a 50 wt% hydrofluoric acid solution for etching for 0.5 h, and then dried in an oven at 80° C.; 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 then the etched puncture needle was immersed in the dopamine solution and heated in a water bath at 80° C. 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, stir at 30° C. and 100 rpm for 5 hours, and 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 for etching for 1 h, and then dried in an oven at 80°C; 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 then the etched puncture needle was immersed in the dopamine solution and heated in a water bath at 80°C 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, stir at 30° C. and 150 rpm for 6 hours, and 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 added amounts of catechin and tannic acid in step (1) are respectively:

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

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

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

[0048] Comparative Example 2

[0049] Different from Example 1, 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 range of ultraviolet light is 270nm, and the irradiation time is 3h;

[0056] B. The wavelength range 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 prepared at 1×10 7 cfu / ml bacterial suspension; place the puncture needles with different treatments (grouping is shown in Table 1, and each group is tested three times) on a culture dish, drip the bacterial suspension so that the bacterial suspension covers the puncture needle, cover it with a sterile plastic film to ensure that the bacterial liquid is in close contact with the stainless steel surface and prevent the evaporation of the bacterial liquid from causing 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] It can be seen from the above examples that the puncture needle with nanosilver antibacterial coating provided by the present invention has good antibacterial performance, the antibacterial rate of Escherichia coli is 97-99%, and the antibacterial rate of Staphylococcus aureus is 94-98%, which is significantly improved compared with 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 irradiation can improve the reducing ability of the reaction system, help to reduce and chelate the dispersed nanosilver particles, form a coating with uniform texture, and improve the antibacterial ability; by comparing Comparative Example 2 with the examples of the present application, it is found that the appropriate mixing ratio of mixed graphene oxide and silver ammonia solution can improve the dispersibility of nanosilver particles in the solution, reduce the aggregation of nanosilver particles, help to form a uniform coating, and further improve the antibacterial performance.

[0064] Test Example 2 Acute systemic poisoning test method

[0065] The puncture needle with nano-silver antibacterial coating prepared in Examples 1 to 3 was immersed in 250 mL of 0.9% sterile sodium chloride solution, kept at 40°C for 5 hours, and the puncture needle was taken out to obtain the test solution, which was measured by the acute systemic toxicity test method (YBB00042003-2015 Acute systemic poisoning test method) using the test solution. It was found that no toxic symptoms were observed in Examples 1 to 3. It can be seen that the puncture needle with nano-silver antibacterial coating prepared in this application has no acute systemic toxicity to the human body, and the nano-silver antibacterial coating provided in this application is relatively 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 principle of the present invention. These improvements and modifications should also be regarded as 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.

2. The method for preparing the puncture needle according to claim 1, characterized in that: 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.

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

4. The method for preparing the puncture needle according to claim 3, characterized in that: The preparation method of the silver ammonia 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 is added dropwise until the silver nitrate solid disappears completely, thereby obtaining the silver ammonia solution.

5. The method for preparing a puncture needle according to claim 4, characterized in that: The mixing ratio of the silver ammonia solution and the graphene solution in step (2) is 1-3:1-3.

6. The method for preparing the puncture needle according to claim 5, characterized in that: The wavelength range of the ultraviolet light in step (2) is 260-280 nm, and the irradiation time is 1.0-1.5 h.

7. The method for preparing a puncture needle according to claim 6, characterized in that: The etching in step (3) is chemical etching, and the etching method is: immerse the puncture needle in a hydrofluoric acid solution with a concentration of 40 to 50 wt% for 0.5 to 1 hour, and dry it.

8. The method for preparing a puncture needle according to claim 7, characterized in that: The concentration of the dopamine solution in step (3) is 2 to 3 mg / mL; The water bath heating temperature is 60-80° C., and the heating time is 4-6 hours.

9. The method for preparing a puncture needle according to claim 8, 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.

10. 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 9.

Images