CN116212095A - Preparation method of molybdenum disulfide nanofiber membrane dressing - Google Patents

Preparation method of molybdenum disulfide nanofiber membrane dressing Download PDF

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CN116212095A
CN116212095A CN202211607708.4A CN202211607708A CN116212095A CN 116212095 A CN116212095 A CN 116212095A CN 202211607708 A CN202211607708 A CN 202211607708A CN 116212095 A CN116212095 A CN 116212095A
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molybdenum disulfide
nanofiber membrane
aqueous solution
mos
stirring
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陈正荣
高明
郑立
雷豆豆
金玮茜
苏桂敏
何欣
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Guangxi Medical University
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Guangxi Medical University
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    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
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    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
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    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
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    • A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
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    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • 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
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    • A—HUMAN NECESSITIES
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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
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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
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
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    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
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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
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Abstract

The invention provides a preparation method of a molybdenum disulfide nanofiber membrane dressing, which comprises the following steps: s1, adding molybdenum disulfide into deionized water, uniformly dispersing, adding a sodium carboxymethyl cellulose aqueous solution, stirring, adding an ascorbic acid aqueous solution, and stirringAdding palladium chloride aqueous solution, stirring to obtain a mixture, washing the mixture with deionized water for 3 times, and vacuum drying in a vacuum drying oven to obtain MoS 2 A @ Pd nanomaterial; s2, performing MoS obtained in the step S1 2 Adding the@Pd nano material into hexafluoroisopropanol, uniformly dispersing, adding PLGA, and continuously stirring to obtain PLGA/MoS 2 A @ Pd solution; s3, PLGA/MoS obtained in the step S2 is processed 2 Filling the@Pd solution into an injector, preparing a nanofiber membrane through electrostatic spinning, and placing the nanofiber membrane into a vacuum drying oven for vacuum drying to obtain the molybdenum disulfide nanofiber membrane dressing. The molybdenum disulfide nanofiber membrane dressing prepared by the invention has strong photo-thermal effect, good antibacterial and wound repair promoting capabilities, and has wide application prospects in clinical wound repair.

Description

Preparation method of molybdenum disulfide nanofiber membrane dressing
Technical Field
The invention relates to a dressing, in particular to a preparation method of a molybdenum disulfide nanofiber membrane dressing.
Background
The skin serves as a first defense line of the human body and plays an important role in protecting against external damage and internal water loss. When the integrity of the skin is compromised, pathogens invade the body, leading to various complications, including pain, bleeding, inflammation, infection, and the like. The current clinical method for treating chronic skin wound is mainly to debridement and match with wound dressing, debridement takes longer time and has potential risk of secondary infection. Traditional wound dressing is usually sponge, bandage or gauze, which is cheap but easy to impregnate to cause exogenous infection, and has single function and poor antibacterial function for promoting wound healing. In order to reduce adhesion and enhance antibacterial performance, grease, vaseline, bactericides such as antibiotics, traditional Chinese medicines, quaternary ammonium salt, silver nano-particles and the like are added into early wound dressings. However, these dressings are poorly absorbent and may have difficulty healing of the infected wound due to local bacterial resistance, and even exhibit some degree of systemic or pathogenic properties. Therefore, the novel wound dressing with antibacterial and wound regeneration promoting synergistic effects and without medicines has larger development and application requirements. Compared with the traditional dressing and the dressing made of single material, the novel medical dressing made of the composite material can effectively inhibit bacteria and promote wound healing.
Photothermal therapy (PTT) has the advantages of being minimally invasive, efficient, small in toxic and side effects, and the like, and has been widely used in antibacterial treatment in the past few years. The photothermal preparation can convert light energy into heat energy when being exposed to Near Infrared (NIR) laser irradiation, and local high temperature is generated, so that the antibacterial effect is realized. The palladium nanoparticle (Pd) has the advantages of high stability, good biocompatibility, excellent photo-thermal performance, anti-inflammatory and antioxidant properties, simple preparation, environmental protection and the like, and is usually selected as a photo-thermal agent. Compared with other photo-thermal metal nano particles, the palladium sheet has higher photo-thermal conversion efficiency, ultrahigh thermal stability and good biosafety, and has wide biomedical application prospect. However, the palladium nanoparticles are easy to agglomerate, and researches show that palladium has toxicity, and excessive accumulation of palladium in human body can cause toxicity of organs such as liver, kidney, spleen and the like.
While the emerging two-dimensional material molybdenum disulfide (MoS 2 ) Because of its unique planar structure, excellent electronic and optical properties (such as thickness dependent band gap, strong near infrared absorbance and large surface area), etc., it has a certain application potential in drug carriers. Thus, palladium nano particles can be loaded on two-dimensional MoS 2 And the aggregation and toxicity of palladium nano particles are reduced, the photothermal anti-inflammatory and antibacterial properties of the palladium nano particles are better exerted, and wound repair is promoted.
Polylactic-co-glycolic acid (PLGA) is a biopolymer approved for clinical use by the United states Food and Drug Administration (FDA). PLGA has good biocompatibility, safety and controllable biodegradation activity, can be used as a drug carrier and a tissue engineering material, and has wide application prospect. Electrospun PLGA fiber membranes have proven to have the potential to support cell growth. The fibrous structure in wound electrospun membranes is similar to that in natural extracellular matrix (ECM), and the high micropores and high specific surface area provide good sites for cell adhesion and oxygen exchange, making it an excellent material for chronic wound dressings.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of the molybdenum disulfide nanofiber membrane dressing, and the prepared molybdenum disulfide nanofiber membrane dressing has a strong photo-thermal effect, good antibacterial and wound repair promoting capabilities, and has a wide application prospect in clinical wound repair.
In order to solve the technical problems, the technical scheme of the invention is as follows:
the preparation method of the molybdenum disulfide nanofiber membrane dressing comprises the following steps:
s1, adding molybdenum disulfide into deionized water, magnetically stirring until the molybdenum disulfide is uniformly dispersed, adding sodium carboxymethylcellulose aqueous solution, stirring for 25-35 minutes, adding ascorbic acid aqueous solution, stirring for 5-10 minutes, adding palladium chloride aqueous solution, stirring for 1-3 hours to obtain a mixture, washing the mixture with deionized water for 3 times, and then placing the mixture into a vacuum drying oven for vacuum drying for 24 hours to obtain MoS 2 A @ Pd nanomaterial;
s2, performing MoS obtained in the step S1 2 Adding the@Pd nano material into hexafluoroisopropanol, stirring for 8 hours until the mixture is uniformly dispersed, adding PLGA, and continuously stirring for 22-26 hours to obtain PLGA/MoS 2 A @ Pd solution;
s3, PLGA/MoS obtained in the step S2 is processed 2 Filling the@Pd solution into a syringe, preparing a nanofiber membrane through electrostatic spinning, and placing the nanofiber membrane into a vacuum drying oven for vacuum drying for 24 hours to obtain the molybdenum disulfide nanofiber membrane dressing.
Further, in the step S1, the mass concentration of the sodium carboxymethyl cellulose aqueous solution is 1-3%, the concentration of the ascorbic acid aqueous solution is 50-100 mg/mL, the concentration of the palladium chloride aqueous solution is 10-20 mg/mL, and the proportion of the molybdenum disulfide, the deionized water, the sodium carboxymethyl cellulose aqueous solution, the ascorbic acid aqueous solution and the palladium chloride aqueous solution is (0.5-2) g (200-500) mL (2-10) mL (30-50) mL (1-2) mL.
Further, in step S2 of the present invention, moS 2 The ratio of the @ Pd nano material, the hexafluoroisopropanol and the PLGA is (0.1-0.5) g (5-10) mL 1g.
Further, in the step S3 of the invention, the distance between the injector and the receiver is 15cm, the receiving speed is 50-100 rpm, the positive voltage is 15-18 kv, and the negative voltage is-3 to-5 kv during electrostatic spinning.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention loads palladium (Pd) nano particles on flaky molybdenum disulfide (MoS) 2 ) Adding the nano-fiber dressing into polylactic acid-glycolic acid copolymer (PLGA), and preparing the molybdenum disulfide nano-fiber film dressing by an electrostatic spinning technology, so that not only can palladium nano-particles be fully utilized to combine with photo-heat to achieve anti-inflammatory and antibacterial effects, but also agglomeration of nano-palladium can be reduced, and harm of the dressing to human body can be reduced, wherein sodium carboxymethyl cellulose used in the step S1 is used as an adhesive for adhering molybdenum disulfide and palladium, ascorbic acid is used as a reducing agent for reducing palladium chloride into palladium particles, and hexafluoroisopropanol used in the step S2 is used for dispersing MoS 2 @Pd nanomaterial and dissolved PLGA.
2. The invention is implemented by using MoS 2 The concentration of the@Pd nano material is controlled, so that MoS can be avoided 2 The content of the@Pd nano material is too low to achieve the antibacterial effect, and MoS can be avoided 2 The content of the@Pd nanomaterial is too high to cause MoS 2 The @ Pd nano material can be dispersed into surrounding tissues to generate toxic and side effects on the body, and the MoS 2 the@Pd nano material is of a two-dimensional black sheet structure, and the molybdenum disulfide nanofiber membrane dressing can generate high-temperature bacteria killing under the irradiation of near infrared light, so that wound healing is promoted.
3. The invention combines photo-heat to realize antibacterial effect, and Pd is loaded on MoS 2 The medicine does not contain medicines, but has strong sterilization, antioxidation, wound cell growth promotion and repair promotion effects, can avoid toxic and side effects of the medicines on patients to a certain extent, and can also effectively avoid drug resistance of wound bacteria.
4. The PLGA used in the invention has good biocompatibility, safety and controllable biodegradation activity, and the electrospun PLGA fiber membrane provides good sites for cell adhesion and oxygen exchange, thereby being beneficial to wound healing.
5. The preparation process is simple, the cost is low, the energy consumption is low, the large-scale production can be carried out, the prepared molybdenum disulfide nanofiber membrane dressing is convenient to use, the quality is good, the wound healing can be effectively prevented, the biodegradability is good, and the environment is protected, so that the environment pollution is avoided.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate and do not limit the invention, and together with the description serve to explain the principle of the invention:
FIG. 1 is a MoS obtained in example 1 of the present invention 2 A transmission electron microscope image of the@Pd nano material;
FIG. 2 shows a dressing of a molybdenum disulfide nanofiber membrane, PLGA+MoS, prepared in example 1 of the present invention 2 A temperature change condition diagram of PLGA under the irradiation of near infrared light;
fig. 3 is a diagram showing an experiment of bacteriostasis of a blank group and a dressing of a molybdenum disulfide nanofiber membrane prepared in example 1 of the present invention;
fig. 4 is a diagram showing repair of skin defects of SD rats in a blank group and molybdenum disulfide nanofiber membrane dressing prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples, wherein the exemplary embodiments and descriptions of the present invention are provided for the purpose of illustration and are not intended to be limiting.
Example 1
The molybdenum disulfide nanofiber membrane dressing is prepared according to the following steps:
s1, adding 1g of molybdenum disulfide into 300mL of deionized water, magnetically stirring until the molybdenum disulfide is uniformly dispersed, adding 10mL of sodium carboxymethylcellulose water solution with the mass concentration of 2%, stirring for 30 minutes, adding 50mL of ascorbic acid water solution with the concentration of 80mg/mL, stirring for 5 minutes, adding 2mL of palladium chloride water solution with the concentration of 20mg/mL, stirring for 2 hours to obtain a mixture, washing the mixture with deionized water for 3 times, and then placing the mixture into a vacuum drying oven for vacuum drying for 24 hours to obtain MoS 2 A @ Pd nanomaterial;
s2, mixing 0.1g of MoS obtained in the step S1 2 Adding the@Pd nano material into 10mL of hexafluoroisopropanol, stirring for 8 hours until the mixture is uniformly dispersed, adding 1g of PLGA, and continuously stirring for 24 hours to obtain PLGA/MoS 2 A @ Pd solution;
s3, PLGA/MoS obtained in the step S2 is processed 2 Filling the@Pd solution into a syringe, preparing a nanofiber membrane by electrostatic spinning, placing the nanofiber membrane into a vacuum drying oven, and drying for 24 hours to obtain the molybdenum disulfide nanofiber membrane dressing, wherein the distance between the syringe and a receiver is 15cm, the receiving speed is 100rpm, the positive voltage is 15kv, the negative voltage is-3 kv.
Example 2
S1, adding 0.5g of molybdenum disulfide into 200mL of deionized water, magnetically stirring until the molybdenum disulfide is uniformly dispersed, adding 2mL of sodium carboxymethyl cellulose water solution with the mass concentration of 3%, stirring for 25 minutes, adding 30mL of ascorbic acid water solution with the mass concentration of 100mg/mL, stirring for 8 minutes, adding 1mL of palladium chloride water solution with the mass concentration of 15mg/mL, stirring for 1 hour to obtain a mixture, washing the mixture with deionized water for 3 times, and then placing the mixture into a vacuum drying oven for vacuum drying for 24 hours to obtain MoS 2 A @ Pd nanomaterial;
s2, mixing 0.2g of MoS obtained in the step S1 2 Adding the@Pd nano material into 5mL hexafluoroisopropanol, stirring for 8 hours until the mixture is uniformly dispersed, adding 1g of PLGA, and continuously stirring for 22 hours to obtain PLGA/MoS 2 A @ Pd solution;
s3, PLGA/MoS obtained in the step S2 is processed 2 Filling the@Pd solution into a syringe, preparing a nanofiber membrane by electrostatic spinning, placing the nanofiber membrane into a vacuum drying oven, and drying for 24 hours to obtain the molybdenum disulfide nanofiber membrane dressing, wherein the distance between the syringe and a receiver is 15cm, the receiving speed is 50rpm, the positive voltage is 18kv, the negative voltage is-5 kv.
Example 3
The molybdenum disulfide nanofiber membrane dressing is prepared according to the following steps:
s1, adding 2g of molybdenum disulfide into 500mL of deionized water, magnetically stirring until the molybdenum disulfide is uniformly dispersed, adding 8mL of sodium carboxymethylcellulose water solution with the mass concentration of 1%, stirring for 35 minutes, adding 40mL of ascorbic acid water solution with the concentration of 50mg/mL, stirring for 10 minutes, adding 1.5mL of palladium chloride water solution with the concentration of 10mg/mL, stirring for 3 hours to obtain a mixture, washing the mixture with deionized water for 3 times, and then placing the mixture into a vacuum drying oven for vacuum drying for 24 hours to obtain MoS 2 A @ Pd nanomaterial;
s2, 0.5g of the product obtained in the step S1MoS 2 Adding the@Pd nano material into 9mL of hexafluoroisopropanol, stirring for 8 hours until the mixture is uniformly dispersed, adding 1g of PLGA, and continuously stirring for 26 hours to obtain PLGA/MoS 2 A @ Pd solution;
s3, PLGA/MoS obtained in the step S2 is processed 2 Filling the@Pd solution into a syringe, preparing a nanofiber membrane by electrostatic spinning, placing the nanofiber membrane into a vacuum drying oven, and drying for 24 hours to obtain the molybdenum disulfide nanofiber membrane dressing, wherein the distance between the syringe and a receiver is 15cm, the receiving speed is 80rpm, the positive voltage is 16kv, the negative voltage is-4 kv.
Bacteriostasis experiment
The molybdenum disulfide nanofiber membrane dressing prepared in example 1 was loaded into a 24-well plate, and then bacterial suspensions (10 μl,10 6 cfu/mL) was dropped into the dressing surface of the molybdenum disulfide nanofiber membrane for 6 hours, and the bacterial group incubated with 100 μl of PBS was used as a blank group, then the bacteria were resuspended with 100 μl of phosphate buffer, and then inoculated on a nutrient broth plate, cultured overnight, and photographed for bacteriostasis.
The test results are shown in fig. 3: the embodiment 1 shows a bacteriostasis ring, and proves that the molybdenum disulfide nanofiber membrane dressing prepared by the invention has good bacteriostasis performance.
Skin defect repair experiment
To evaluate the wound repair performance of molybdenum disulfide nanofiber membrane dressing, a full-thickness rat skin incision model was established using male SD rats (200-240 g). Briefly, SD rats, after anesthesia with 3% pentobarbital, were fixed on surgical cork boards, then shaved and sterilized with iodine, and then four full thickness incisions (about 2cm long) were created in the backs of the rats, and the molybdenum disulfide nanofiber membrane dressing prepared in example 1 was applied to the wounds and irradiated with near infrared rays to leave no treatment as a blank group. The cut area was monitored and photographed on day 14.
The test results are shown in fig. 4: compared with a blank group, the area of the wound corresponding to the embodiment 1 is obviously reduced a lot, and the molybdenum disulfide nanofiber membrane dressing prepared by the invention has better wound healing promoting capability.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.

Claims (4)

1. A preparation method of a molybdenum disulfide nanofiber membrane dressing is characterized by comprising the following steps of: the method comprises the following steps:
s1, adding molybdenum disulfide into deionized water, magnetically stirring until the molybdenum disulfide is uniformly dispersed, adding sodium carboxymethylcellulose aqueous solution, stirring for 25-35 minutes, adding ascorbic acid aqueous solution, stirring for 5-10 minutes, adding palladium chloride aqueous solution, stirring for 1-3 hours to obtain a mixture, washing the mixture with deionized water for 3 times, and then placing the mixture into a vacuum drying oven for vacuum drying for 24 hours to obtain MoS 2 A @ Pd nanomaterial;
s2, performing MoS obtained in the step S1 2 Adding the@Pd nano material into hexafluoroisopropanol, stirring for 8 hours until the mixture is uniformly dispersed, adding PLGA, and continuously stirring for 22-26 hours to obtain PLGA/MoS 2 A @ Pd solution;
s3, PLGA/MoS obtained in the step S2 is processed 2 Filling the@Pd solution into a syringe, preparing a nanofiber membrane through electrostatic spinning, and placing the nanofiber membrane into a vacuum drying oven for vacuum drying for 24 hours to obtain the molybdenum disulfide nanofiber membrane dressing.
2. The method for preparing the molybdenum disulfide nanofiber membrane dressing according to claim 1, which is characterized in that: in the step S1, the mass concentration of the sodium carboxymethyl cellulose aqueous solution is 1-3%, the concentration of the ascorbic acid aqueous solution is 50-100 mg/mL, the concentration of the palladium chloride aqueous solution is 10-20 mg/mL, and the proportion of the molybdenum disulfide, the deionized water, the sodium carboxymethyl cellulose aqueous solution, the ascorbic acid aqueous solution and the palladium chloride aqueous solution is (0.5-2) g (200-500) mL (2-10) mL (30-50) mL (1-2) mL.
3. The method for preparing the molybdenum disulfide nanofiber membrane dressing according to claim 1, which is characterized in that: the steps are as follows
S2, moS 2 The ratio of the @ Pd nano material, the hexafluoroisopropanol and the PLGA is (0.1-0.5) g (5-10) mL 1g.
4. The method for preparing the molybdenum disulfide nanofiber membrane dressing according to claim 1, which is characterized in that: in the step S3, the distance between the injector and the receiver is 15cm, the receiving speed is 50-100 rpm, the positive voltage is 15-18 kv, and the negative voltage is-3 to-5 kv during electrostatic spinning.
CN202211607708.4A 2022-12-14 2022-12-14 Preparation method of molybdenum disulfide nanofiber membrane dressing Pending CN116212095A (en)

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