CN115531591B - Intelligent electrothermal dressing with temperature control and sectional drug delivery functions and preparation method thereof - Google Patents

Intelligent electrothermal dressing with temperature control and sectional drug delivery functions and preparation method thereof Download PDF

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CN115531591B
CN115531591B CN202211028002.2A CN202211028002A CN115531591B CN 115531591 B CN115531591 B CN 115531591B CN 202211028002 A CN202211028002 A CN 202211028002A CN 115531591 B CN115531591 B CN 115531591B
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temperature
drug
dressing
microgel
carrying
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CN115531591A (en
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侯恺
郭莹
闫婷
朱美芳
陈国印
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Donghua University
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Donghua University
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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
    • A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00—Bandages or dressings; Absorbent pads
    • A61F13/00051—Accessories for dressings
    • A61F13/00063—Accessories for dressings comprising medicaments or additives, e.g. odor control, PH control, debriding, antimicrobic
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00—Bandages or dressings; Absorbent pads
    • A61F13/02—Adhesive plasters or dressings
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00—Bandages or dressings; Absorbent pads
    • A61F13/02—Adhesive plasters or dressings
    • A61F13/0276—Apparatus or processes for manufacturing adhesive dressings or bandages
    • 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
    • A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
    • A61L15/28—Polysaccharides or their derivatives
    • 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
    • A61L15/42—Use of materials characterised by their function or physical properties
    • A61L15/44—Medicaments
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00—Bandages or dressings; Absorbent pads
    • A61F2013/00361—Plasters
    • A61F2013/00902—Plasters containing means
    • A61F2013/00906—Plasters containing means for transcutaneous or transdermal drugs application
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B30/00—Energy efficient heating, ventilation or air conditioning [HVAC]

Abstract

The intelligent electrothermal dressing comprises an electrically-heated conductive fabric, wherein the conductive fabric is provided with a plurality of independently-controlled heating coating areas, each coating area is provided with a medicine dressing layer, each medicine dressing layer comprises a gel matrix, temperature-sensitive medicine-carrying microgel coated in the gel matrix and medicine solutions loaded in the temperature-sensitive medicine-carrying microgel, and the types of the medicine solutions loaded by the temperature-sensitive medicine-carrying microgels in different coating areas are different. The invention can stimulate the temperature sensitive drug-carrying microgel in different areas to generate phase transition, so as to release different drugs according to the staged requirements of wound healing, and the drug administration type, the dosage and the release time are controllable, thereby shortening the wound healing period and improving the treatment effect; and the dressing is not required to be frequently replaced, so that secondary wound infection caused in the dressing replacement process is effectively avoided, great inconvenience is brought to a patient due to repeated dressing replacement, and the defect that pain of the patient can be increased due to each dressing replacement is overcome.

Description

Intelligent electrothermal dressing with temperature control and sectional drug delivery functions and preparation method thereof
Technical Field
The invention relates to the field of medical materials, in particular to an intelligent electrothermal dressing for temperature control sectional drug delivery and a preparation method thereof.
Background
Chronic wounds refer to wounds that fail to heal or have no healing tendency due to external or internal factors for more than 1 month, including, for example, pressure sores, diabetic foot ulcers, arteriovenous ulcers of the lower extremities, and the like. With the increasing proportion of chronic wound patients in recent years, how to improve the curative effect of chronic wound therapy has become a great problem in the medical field.
At present, the dressing is the most common means for nursing chronic wounds, can replace damaged skin in the healing period to play a role of barrier, prevent the wounds from being polluted by external environment, and provide excellent healing environment. The gel dressing is used as one of the wet dressing, is a high polymer material composed of a three-dimensional network structure, has high internal water content, good fit and excellent tissue compatibility, can avoid secondary injury caused in the replacement process, and can absorb a small amount of tissue fluid oozing from a wound.
However, healing of chronic wounds is a complex dynamic process involving the co-action of multiple drugs, growth factors, and the complex structure of the wound, with different areas of the wound being in different stages of healing. The gel dressing in the prior art is limited to passively releasing one to two active ingredients, but omits the staged and regional requirements of chronic wound healing, dressing materials of different medicine types need to be replaced frequently (such as 1 to 2 days) according to wound healing conditions, and repeated dressing replacement brings great inconvenience to patients, pain of patients can be increased when dressing replacement is performed each time, and in addition, the treatment cost, the treatment period and the poor effect are increased.
Disclosure of Invention
Based on the above, the invention provides the intelligent electrothermal dressing with temperature control and sectional drug delivery and the preparation method thereof, so as to solve the technical problems that the gel dressing in the prior art is limited to passively release one to two active ingredients, dressing materials with different drug types need to be frequently replaced according to wound healing conditions, and repeated drug replacement brings great inconvenience to patients and can increase pain of the patients.
In order to achieve the above purpose, the invention provides an intelligent electric heating dressing for temperature control sectional drug delivery, which comprises an electric heating conductive fabric, wherein the electric heating conductive fabric is provided with a plurality of coating areas capable of independently controlling heating, each coating area is provided with a drug dressing layer, each drug dressing layer comprises a gel matrix, temperature-sensitive drug-carrying microgel coated in the gel matrix, and drug solutions loaded in the temperature-sensitive drug-carrying microgel, and the types of the drug solutions loaded by the temperature-sensitive drug-carrying microgels in different coating areas are different.
As a further preferable technical scheme of the invention, the medicine dressing layer is provided with a plurality of gel units, the gel units are distributed in an array mode, the thickness of each gel unit is 0.2-2mm, the diameter is 2-5mm, and the interval is 2-5mm.
As a further preferable technical scheme of the invention, insulating separation areas with the width of 1-5mm are reserved between the drug dressing layers of different coating areas, and the insulating separation areas are coated with gel matrixes without thermosensitive drug-carrying microgels.
According to another aspect of the present invention, the present invention further provides a method for preparing an intelligent electrothermal dressing for temperature-controlled and sectional administration, the method comprising the steps of:
s1, soaking a fabric in a dispersion liquid of a carbon-containing material, taking out and passing through a roller to realize pad dyeing, and repeating pad dyeing for a plurality of times after drying to prepare a conductive fabric;
s2, adding two temperature-sensitive comonomers, sodium alginate, an initiator and an accelerator into an inorganic hectorite aqueous dispersion, polymerizing for 10-24 hours at room temperature, extruding the obtained polymer into a calcium chloride aqueous solution dropwise to form spherical microgel, and obtaining the spherical microgel with different response temperatures by adjusting the molar ratio of the two temperature-sensitive comonomers; washing the spherical microgel with deionized water, filtering, freeze-drying, and putting the freeze-dried spherical microgel with different response temperatures into different drug solutions respectively to swell for 12-24 hours to prepare a plurality of thermosensitive drug-carrying microgels loaded with different types of drug solutions;
s3, adding an acrylamide monomer, an initiator and an accelerator into the inorganic hectorite aqueous dispersion to form a prepolymer solution, adding the thermosensitive drug-carrying microgel, coating the prepolymer solution on the surface of the conductive fabric, and reacting the thermosensitive drug-carrying microgel loaded with different types of drug solutions at room temperature for 8-24 hours to enable the prepolymer solution to form a gel matrix coating the thermosensitive drug-carrying microgel through polymerization reaction, thus finally obtaining the intelligent electrothermal dressing with temperature control and sectional administration.
As a further preferable technical scheme of the invention, in the step S1, the fabric is knitted, woven or non-woven fabric formed by one or more fibers of cotton, nylon, polyphenylene sulfide or polypropylene; the carbon material is one or more of graphene oxide, carbon nanotubes, conductive carbon black or graphite; the mass fraction of the carbon material in the dispersion is 0.1-0.5 wt%, the solvent of the dispersion is a mixture of ethanol and water, and the volume ratio of the ethanol to the water is 1:10-1:1.
As a further preferable technical scheme of the invention, in the step S2, two temperature-sensitive comonomers are 2-methyl-2-acrylic acid-2- (2-methoxyethoxy) ethyl ester and oligopolyethylene glycol methyl ether methacrylate, and the response temperature of the spherical microgel is regulated and controlled by regulating the molar ratio of the two monomers, wherein the change range of the response temperature is 35-60 ℃.
As a further preferable technical scheme of the invention, in the step S2, the inorganic hectorite aqueous dispersion is obtained by uniformly dispersing inorganic hectorite in deionized water, the total content of the added two temperature-sensitive comonomers is 5-20wt.% of the mass of the deionized water, the inorganic hectorite and sodium alginate are 0.5-3wt.% of the mass of the deionized water, the concentration of the calcium chloride aqueous solution is 2%, and the concentration of the drug solution is 0.1-2 mg.mL -1 。
As a further preferable embodiment of the present invention, in the step S2, the particle size of the spherical microgel after lyophilization is 50-200. Mu.m.
In step S3, the inorganic hectorite aqueous dispersion is obtained by uniformly dispersing inorganic hectorite in water, wherein the inorganic hectorite content is 5-20wt.% of the water mass, the acrylamide monomer is 10-30wt.% of the water mass, and the temperature-sensitive drug-loaded microgel is 10-40wt.% of the acrylamide monomer.
As a further preferable technical scheme of the invention, in the steps S2 and S3, the initiator is one or more of potassium persulfate, ammonium persulfate or sodium persulfate, and the accelerator is one or more of N, N, N ', N' -tetramethyl ethylenediamine or N, N-dimethyl aniline, wherein: the amount of the initiator in the step S2 is 1-10wt.% of the content of the two temperature-sensitive comonomers, and the amount of the initiator in the step S3 is 1-10wt.% of the content of the acrylamide monomer; the using amount of the accelerator in the step S2 is 0.2-0.8% of the volume of the prepolymer, and the using amount of the accelerator in the step S3 is 0.2-0.8% of the volume of the prepolymer.
The intelligent electrothermal dressing with temperature control and sectional drug delivery and the preparation method thereof can achieve the following beneficial effects by adopting the technical scheme:
1) The advantages of the gel material are maintained, a moist environment can be provided for wound restoration, exudation tissue fluid can be absorbed, and the damage to new tissues is avoided while necrotic tissues and toxins are eliminated;
2) The fabric is used as the substrate, so that the mechanical strength of the coated gel can be improved to a certain extent, the defect of poor mechanical property of the traditional gel dressing is overcome, and the service life of the dressing is prolonged;
3) The heating circuit formed after the fabric tie-dyeing is connected with an external power supply, and the temperature of the drug dressing layer is changed along with the voltage adjustment, so that the temperature-sensitive drug-carrying microgel in different areas can be stimulated to be subjected to phase transition, different drugs are released according to the staged requirements of wound healing, the drug administration type, the dosage and the release time are controllable, the wound healing period is further shortened, and the treatment effect is improved;
4) The intelligent electrothermal dressing provided by the invention adopts temperature control sectional drug delivery, can be used for a long time, does not need frequent replacement, effectively avoids secondary wound infection caused in the dressing replacement process, and avoids the defects that a patient is inconvenient caused by repeated drug replacement and pain of the patient can be increased when the patient is changed for a plurality of times, namely, the treatment cost is reduced to a certain extent; in addition, the dressing does not need to be externally connected with complex equipment, and is convenient to carry;
5) The intelligent electrothermal dressing has relatively simple preparation process, no complicated chemical reaction, high temperature, high pressure, organic solvent and other conditions, and no toxic side effect on environment.
Drawings
The invention will be described in further detail with reference to the drawings and the detailed description.
FIG. 1 is a schematic illustration of a gel coating mode of an intelligent electrothermal dressing for temperature controlled and segmented drug delivery according to the present invention;
FIG. 2 is a flow chart diagram of a method for preparing the intelligent electrothermal dressing for temperature-controlled and sectional administration;
FIG. 3 is a graph showing the temperature versus time of the infrared images and the drug dressing layer before and after energizing in different coating modes.
The achievement of the objects, functional features and advantages of the present invention will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Detailed Description
The invention will be further described with reference to the drawings and detailed description. The terms such as "upper", "lower", "left", "right", "middle" and "a" in the preferred embodiments are merely descriptive, but are not intended to limit the scope of the invention, as the relative relationship changes or modifications may be otherwise deemed to be within the scope of the invention without substantial modification to the technical context.
The invention provides an intelligent electric heating dressing for temperature control sectional drug delivery, which comprises an electric heating conductive fabric, wherein the conductive fabric is provided with a plurality of coating areas capable of independently controlling heating, each coating area is provided with a drug dressing layer, each drug dressing layer comprises a gel matrix, thermosensitive drug-carrying microgels which are coated in the gel matrix and are granular (with the particle size of 50-200 mu m), and drug solutions loaded in the thermosensitive drug-carrying microgels, and the types of the drug solutions loaded by the thermosensitive drug-carrying microgels in different coating areas are different.
Preferably, for the convenience of use and portability of the user, the conductive fabric is further provided with an external power supply for providing electric energy required by heating the conductive fabric, and the power supply can adopt a conventional portable charging source with the specification of less than 10000mAh and 12V, and of course, a storage battery can also be adopted. In order to realize intelligent control, the power supply is also provided with a controller, and the controller is used for controlling and adjusting the voltage output by the power supply and selecting a coating area needing electric heating.
The intelligent electrothermal dressing and an external power supply are assembled into the intelligent electrothermal dressing with temperature control and sectional drug delivery, and the electrothermal fabric layer in a certain coating area is heated by applying voltage and is transferred to the drug dressing layer, so that the internal thermosensitive drug-carrying microgel is stimulated to undergo phase transition, and corresponding loaded drugs are released; after the power supply is cut off, the temperature is reduced, and the drug release is stopped; by changing the position (coating area) and the size of the applied voltage, another therapeutic drug can be released to the wound surface, and the effect of on-demand drug administration is achieved. In the heating process, the temperature rising range of the fabric layer is 50-75 ℃, and the temperature rising range of the medicine dressing layer is 40-65 ℃ and the temperature rising time is 60-300s because of certain heat loss in the transmission process.
The multiple coating areas capable of independently controlling heating can be arranged on the conductive fabric at will according to the requirement, such as left and right or up and down, or the multiple areas are arranged side by side, the multiple areas are arranged in concentric rings, the multiple areas are arranged around a certain point in sequence, etc., and fig. 1 shows the distribution of four coating areas (areas i-iv) on the conductive fabric in an example.
The coating structure of the drug dressing layer in the coating area can adopt the following several types of planar coating, vertical coating, parallel coating and array coating, wherein the planar coating refers to the drug dressing layer as a whole (a in fig. 3), the vertical coating refers to the drug dressing layer which is in a strip-shaped transverse parallel arrangement (b in fig. 3), the parallel coating refers to the drug dressing layer which is in a strip-shaped longitudinal parallel arrangement (c in fig. 3), and the array coating refers to the drug dressing which is in lattice distribution (d in fig. 3) by a plurality of gel units. The infrared images and gel layer temperature-time curves of the four coating structures before and after power-on are shown in fig. 3. In the coating process of the medicine dressing layer, because the fabric has a certain pore, the prepolymer liquid can permeate into the fabric, and a reinforcing network is formed after polymerization, so that the conductive path of the fabric is influenced to a certain extent, the electrothermal effect of the fabric is weakened, as can be seen from fig. 3, the surface temperature of the medicine dressing layer in plane coating is slowly increased, the temperature is lower, and the vertical and parallel coating modes are secondary, so that the array type coating effect is optimal. By comparing the changes in gel surface temperature in a planar, vertical, parallel or array coating mode, it is known that the array coating has relatively minimal impact on fabric resistance and can reach the internal microgel response temperature relatively quickly.
In a specific implementation, the drug dressing layer is provided with a plurality of gel units, the gel units are distributed in an array (dot matrix type coating structure), the thickness of each gel unit is 0.2-2mm, the diameter is 2-5mm, the distance is 2-5mm, the array distribution is shown in fig. 1, each circle in the figure is a coated gel matrix (gel unit) coated with the temperature-sensitive drug-carrying microgel, and different diagonal bars in the circle represent different types of drug solutions carried by the temperature-sensitive drug-carrying microgel.
Preferably, insulating separation areas with the width of 1-5mm are reserved between the drug dressing layers of different coating areas, and gel matrixes which do not contain the thermosensitive drug-carrying microgel are coated on the insulating separation areas, so that the release of the drugs in the different areas is facilitated, and the influence of the gel on the conductive paths and the electrothermal effect in the fabric can be reduced.
As shown in fig. 2, the invention also provides a preparation method of the intelligent electrothermal dressing with temperature control and sectional drug delivery, which comprises the following steps:
and S1, soaking the fabric in a dispersion liquid of a carbon-containing material, taking out and passing through a roller to realize pad dyeing, drying, and repeating the pad dyeing for a plurality of times, wherein the carbon-containing material is loaded in the fabric to form a heating circuit, so that the conductive fabric is prepared.
In the step S1, the fabric is knitted, woven or non-woven fabric formed by one or more fibers of cotton, nylon, polyphenylene sulfide or polypropylene; the carbon material is one or more of Graphene Oxide (GO), carbon Nanotubes (CNT), conductive carbon black or graphite; the mass fraction of the carbon material in the dispersion is 0.1-0.5 wt%, the solvent of the dispersion is a mixture of ethanol and water, and the volume ratio of the ethanol to the water is 1:10-1:1.
When the carbon material is graphene oxide, the reduction treatment is required after repeated pad dyeing, the reduction treatment takes a mixed solution of hydroiodic acid (HI) and glacial acetic acid (HAc) as a reducing agent, and the volume ratio HI is HAc=2:1, and the reduction treatment is carried out for 10 hours under the condition of 90 ℃.
Specifically, the conductive fabric has a plurality of coating areas which independently control heating, and insulation between different coating areas is also required, which can be achieved by the following operations: when the fabric is first soaked, the areas between adjacent coated areas are not impregnated with a dispersion of carbonaceous material, even though the fabric between adjacent coated areas is free of carbonaceous material; the different coating areas are respectively connected with an external power supply through wires, so that independent control of heating can be realized.
S2, adding two temperature-sensitive comonomers, sodium alginate (Alg), an initiator and an accelerator into inorganic hectorite (clay) water dispersion liquid, polymerizing for 10-24 hours at room temperature, extruding the obtained polymer into a calcium chloride water solution dropwise to form spherical microgel, and obtaining the spherical microgel with different response temperatures by adjusting the molar ratio of the two temperature-sensitive comonomers; washing the spherical microgel with deionized water, filtering, freeze-drying, and putting the freeze-dried spherical microgel with different response temperatures into different drug solutions respectively to swell for 12-24 hours to prepare various thermosensitive drug-carrying microgels loaded with different types of drug solutions.
In the step S2, the two temperature-sensitive comonomers are 2-methyl-2-acrylic acid-2- (2-methoxyethoxy) ethyl ester (MEO) 2 MA，M n ＝188g·mol -1 ) And oligo (ethylene glycol) methyl ether methacrylate (OEGMA, M) n ＝475g·mol -1 ) The response temperature of the spherical microgel is regulated and controlled by regulating the molar ratio of the two, and the change range of the response temperature is 35-60 ℃.
The inorganic hectorite aqueous dispersion is obtained by uniformly dispersing inorganic hectorite in deionized water, wherein the total content of the added two temperature-sensitive comonomers is 5-20wt.% of the mass of the deionized water, the mass of the inorganic hectorite and the mass of the sodium alginate are 0.5-3wt.% of the mass of the deionized water, and the concentration of the calcium chloride aqueous solution is 2%.
The initiator is one or more of potassium persulfate (KPS), ammonium Persulfate (APS) or sodium persulfate (NaPS), the accelerator is one or more of N, N, N ', N' -tetramethyl ethylenediamine (TEMED) or N, N-dimethyl aniline, the initiator is 1-10wt.% of the content of the two temperature-sensitive comonomers, and the accelerator is 0.2-0.8% of the volume of the prepolymer.
The drug solution can be any one or more of the followingHealing promoting substance solution with hemostatic, antibacterial or antiinflammatory effects with concentration of 0.1-2 mg/mL -1 。
The polymer formed by the two temperature-sensitive comonomers is extruded into calcium chloride aqueous solution drop by drop through an injection needle to form spherical microgel, the size of the spherical microgel can be changed by changing the model of the injection needle, and the particle size of the microgel after freeze-drying is 50-200 mu m. The drug loading capacity of the spherical microgel is limited by the size, and the spherical microgels with different sizes have different drug loading energies, so that the dispersion capacity in the prepolymer liquid is different, and in practical application, the size of the spherical microgel can be reasonably selected according to the requirement of the actual drug loading amount per unit area so as to meet the use requirement.
In the step, the water in the microgel is removed by adopting a freeze-drying operation method, so that the subsequent storage and drug loading are facilitated.
S3, adding an acrylamide monomer (AAm), an initiator and an accelerator into inorganic hectorite (clay) aqueous dispersion to form a prepolymer solution, adding a thermosensitive drug-carrying microgel, coating the prepolymer solution on the surface of a conductive fabric after microcoagulation, and reacting the thermosensitive drug-carrying microgel loaded with different types of drug solutions at room temperature for 8-24 hours to enable the prepolymer solution to form a gel matrix coating the thermosensitive drug-carrying microgel through polymerization reaction, thus finally obtaining the intelligent electrothermal dressing with temperature control and sectional drug administration.
In the step S3, the inorganic hectorite aqueous dispersion is obtained by uniformly dispersing inorganic hectorite in water, wherein the content of the inorganic hectorite is 5-20wt.% of the mass of the water, the content of the acrylamide monomer is 10-30wt.% of the mass of the water, and the content of the thermosensitive drug-carrying microgel is 10-40wt.% of the mass of the acrylamide monomer.
The initiator is one or more of potassium persulfate, ammonium persulfate and sodium persulfate, the accelerator is one or more of N, N, N ', N' -tetramethyl ethylenediamine or N, N-dimethyl aniline, the initiator is 1-10wt.% of the acrylamide monomer content, and the accelerator is 0.2-0.8% of the volume of the prepolymer.
In order to enable the person skilled in the art to further understand the technical scheme of the present invention, the technical scheme of the preparation method of the present invention is further described in detail through specific examples.
Example 1
(1) Preparing a conductive fabric: adding 1g of Carbon Nano Tube (CNT) powder into a mixed solvent of 900g of water and 100g of ethanol (EtOH), and carrying out pre-stirring for 0.5h and ultrasonic treatment for 1h to obtain a dispersion liquid with the weight percent of 0.1; soaking the cut all-cotton knitted fabric in the dispersion liquid, taking out, passing through a roller to enable the liquid to penetrate into the fabric and remove residual liquid; after drying and repeated pad dyeing for 30 times, a CNT-coated all-cotton knitted fabric (conductive fabric) with good conductivity is prepared for standby, and the conductive fabric is provided with four coating areas (areas i-iv) which independently control heating.
(2) Preparation of drug-loaded microgel: dispersing 0.05g inorganic hectorite (clay) in 10g deionized water, sequentially adding 0.119g oligo (ethylene glycol) methyl ether methacrylate (OEGMA) and 0.3831 g 2-methyl-2-acrylic acid-2- (2-methoxyethoxy) ethyl ester (MEO) 2 MA), sodium alginate (Alg) 0.1g, potassium persulfate (KPS) 0.02g and 20 μ L N, N, N ', N' -tetramethyl ethylenediamine (TEMED) at room temperature for 10h, and then extruding it drop by drop to CaCl 2 Obtaining a spherical microgel having a response temperature of about 35 ℃ in an aqueous solution; then adjusting the mole ratio of the two comonomers to obtain spherical microgel with response temperature of about 37 ℃, 40 ℃ and 42 ℃ in sequence; washing the spherical microgel with deionized water for a plurality of times to remove unreacted monomers, cross-linking agents and the like; filtering, lyophilizing, and respectively adding the obtained four spherical microgels into 1mg.mL -1 Cefazolin, curcumin, insulin and 0.1 mg.ml -1 Swelling for 24h in vascular endothelial growth factor solution to obtain four thermosensitive drug-carrying microgels loaded with four different drug solutions respectively.
(3) Preparation of dressing: adding 0.5g of clay into 10g of deionized water, and uniformly stirring to obtain a dispersion with the mass fraction of 5 wt.%; then adding 1g acrylamide monomer (AAm), 0.04g KPS and 30 mu L TEMED to prepare a prepolymer, dividing the prepolymer into four parts, adding 0.1g of the four temperature-sensitive drug-loaded microgels to prepare coating solutions, and coating the coating solutions coated with the 4 temperature-sensitive drug-loaded microgels in the areas I-IV of the conductive fabric (shown in figure 1)) Reacting for 8 hours at room temperature to obtain a final product; wherein the areas of the areas are uniform and are 20 multiplied by 20mm 2 Coating liquid is distributed in a dot-like array mode, the diameter of each single coating point is 3mm, and the adjacent distance is 3mm; the interval between the adjacent coating areas is 1mm, and the thickness of the prepolymer liquid coated with the temperature-sensitive drug-carrying microgel is 0.5mm.
And (3) effect verification: the prepared intelligent electrothermal dressing and an external power supply are assembled into the intelligent electrothermal dressing with temperature control and sectional drug delivery, when the output voltage is 8V, the temperature of a fabric layer is measured to be about 46 ℃, the temperature of a drug dressing layer is increased to 35 ℃ after 80 seconds, and the temperature-sensitive drug-carrying microgel in the area I immediately undergoes phase transition and releases the loaded drug; after the preset time, applying 9V voltage to the area II, stabilizing the temperature of the drug dressing layer to about 38 ℃, enabling the temperature-sensitive drug-carrying microgel of the area II to reach the critical phase transition temperature, and responding to the stimulus to release another drug; by analogy, targeted quantitative and timed drug administration can be realized.
Example 2
(1) Preparing a conductive fabric: 250g of GO dispersion with a concentration of 1wt.% are taken together with 500g H 2 Mixing O and 250g EtOH, pre-stirring for 0.5h and carrying out ultrasonic treatment for 1h to obtain 0.25wt.% of dispersion; soaking the cut PPS woven fabric in the dispersion liquid, then passing through a roller to enable the liquid to penetrate into the fabric and remove residual liquid; after repeated pad dyeing for 35 times by drying, preparing a reducing agent according to the volume ratio of HI to HAc=2:1, completely immersing the fabric, and reacting for 10 hours in a 90 ℃ environment to prepare the rGO coated PPS woven fabric (conductive fabric) with good conductivity for standby, wherein the conductive fabric is provided with four coating areas (areas I-IV) for independently controlling heating.
(2) Preparation of drug-loaded microgel: 0.1g of clay is evenly dispersed in 10g of deionized water, and 0.274g of OEGMA and 0.726g of MEO are added in sequence 2 MA, 0.2g Alg, 0.04g KPS and 30. Mu.L TEMED, polymerized for 12h at RT, and extruded drop wise to CaCl 2 Obtaining a spherical microgel having a response temperature of about 37 ℃ in an aqueous solution; then adjusting the mole ratio of the two comonomers to obtain spherical microgel with response temperature of 40 ℃, 42 ℃ and 45 ℃ in sequence; washing the spherical microgel with deionized water for several times to remove unreacted monomersA bulk, a crosslinking agent, etc.; filtering, lyophilizing, and respectively adding the obtained four spherical microgels into 1.2 mg.mL -1 Cefazolin, vancomycin, insulin and 0.2 mg.ml -1 Swelling for 24h in vascular endothelial growth factor solution to obtain four thermosensitive drug-carrying microgels loaded with four different drug solutions respectively.
(3) Preparation of dressing: adding 1g of clay into 10g of deionized water, and uniformly stirring to obtain a dispersion with the mass fraction of 10wt.%; then adding 2g of monomer AAm, 0.08g of KPS and 30 mu L of TEMED to prepare a prepolymer, dividing the prepolymer into four parts, respectively adding 0.4g of the prepared four temperature-sensitive drug-loaded microgels to prepare coating solutions, respectively coating and coating the coating solutions (shown in figure 1) for coating the 4 temperature-sensitive drug-loaded microgels in the areas I-IV of the conductive fabric, and reacting for 10 hours at room temperature to obtain a final product; wherein the areas of the areas are uniform and are 20 multiplied by 20mm 2 Coating liquid is distributed in a dot-like array mode, the diameter of each single coating point is 2mm, and the adjacent spacing is 2mm; the interval between the adjacent coating areas is 2mm, and the thickness of the prepolymer liquid coated with the temperature-sensitive drug-carrying microgel is 0.8mm.
And (3) effect verification: the prepared dressing and an external power supply are assembled into an intelligent electric heating dressing for temperature control sectional drug delivery, when the output voltage is 8V, the temperature of a fabric layer is measured to be about 48 ℃, the temperature of a drug dressing layer is increased to 37 ℃ after 90 seconds, and temperature-sensitive drug-carrying microgel in a region I is subjected to phase transition immediately and releases a drug carried; after the preset time, applying 9V voltage to the area II, stabilizing the temperature of the drug dressing layer to about 40 ℃, enabling the temperature-sensitive drug-carrying microgel of the area II to reach the critical phase transition temperature, and responding to the stimulus to release another drug; by analogy, targeted quantitative and timed drug administration can be realized.
Example 3
(1) Preparing a conductive fabric: adding 4g of conductive carbon black powder into 800g H 2 In a mixed solvent of O and 200g of EtOH, pre-stirring for 0.5h and carrying out ultrasonic treatment for 1h to obtain 0.4wt.% of dispersion; soaking the cut nylon Long Zhen fabric in the dispersion liquid, then passing through a roller to enable the liquid to penetrate into the fabric and remove residual liquid; after drying and repeated pad dyeing for 40 times, the carbon black coated nylon knitted fabric (guide) with good conductivity is preparedElectrical fabric) is ready for use and the conductive fabric has four coated areas (areas i-iv) that independently control heat generation.
(2) Preparation of drug-loaded microgel: 0.2g of clay is evenly dispersed in 10g of deionized water, and 0.535g of OEGMA and 0.965g of MEO are added in sequence 2 MA, 0.2g Alg, 0.09g APS and 50. Mu.L dimethylaniline, after 14h polymerization at room temperature, were extruded drop wise to CaCl 2 Obtaining a spherical microgel having a response temperature of about 40 ℃ in an aqueous solution; subsequently, the molar ratio of the two comonomers is regulated, and microgels with response temperatures of about 42 ℃, 45 ℃ and 48 ℃ are obtained in sequence; washing with deionized water for several times to remove unreacted monomers, crosslinking agent and the like; filtering, freeze-drying, and respectively placing 4 kinds of microgels into 1.5 mg.mL -1 Vancomycin, curcumin, insulin or 0.3 mg.ml -1 Swelling for 24h in vascular endothelial growth factor solution to obtain four thermosensitive drug-carrying microgels loaded with four different drug solutions respectively.
(3) Preparation of dressing: adding 1.5g of clay into 10g of deionized water, and uniformly stirring to obtain a dispersion with the mass fraction of 15 wt.%; then adding 3g of monomer AAm, 0.18g of APS and 50 mu L of dimethylaniline to prepare a prepolymer, dividing the prepolymer into four parts, respectively adding 0.9g of the four temperature-sensitive drug-carrying microgels prepared by the above method, respectively coating solutions (shown in figure 1) for coating the 4 temperature-sensitive drug-carrying microgels on the areas I-IV of the conductive fabric, and reacting for 12 hours at room temperature to obtain a final product; wherein the areas of the areas are uniform and are 30 multiplied by 30mm 2 Coating liquid is distributed in a dot-like array mode, the diameter of each single coating point is 4mm, and the adjacent distance is 4mm; the interval between the adjacent coating areas is 3mm, and the thickness of the prepolymer liquid coated with the temperature-sensitive drug-carrying microgel is 1mm.
And (3) effect verification: the prepared dressing and an external power supply are assembled into an intelligent electric heating dressing for temperature control sectional drug delivery, when the output voltage is 7V, the temperature of a fabric layer is measured to be about 50 ℃, the temperature of a drug dressing layer is increased to 40 ℃ after 100 seconds, and temperature-sensitive drug-carrying microgel in a region I is subjected to phase transition immediately and releases a drug carried; after the preset time, 9V voltage is applied to the area II, the temperature of the drug dressing layer is stabilized to about 42 ℃, the temperature-sensitive drug-carrying microgel of the area II reaches the critical phase transition temperature, and another drug is released in response to the stimulus; by analogy, targeted quantitative drug delivery can be realized.
Example 4
(1) Preparing a conductive fabric: adding 5g graphite powder into 500g H 2 In a mixed solvent of O and 500g of EtOH, pre-stirring for 0.5h and carrying out ultrasonic treatment for 1h to obtain 0.5wt.% of dispersion; soaking the cut PP non-woven fabric in the dispersion liquid, then passing through a roller to enable the liquid to penetrate into the fabric and remove residual liquid; and (3) drying and repeated pad dyeing for 45 times, preparing the graphite coating PP non-woven fabric (conductive fabric) with good conductivity for standby application, wherein the conductive fabric is provided with four coating areas (areas I-IV) for independently controlling heating.
(2) Preparation of drug-loaded microgel: 0.3g of clay is evenly dispersed in 10g of deionized water, and 0.804g of OEGMA and 1.196g of MEO are added in sequence 2 MA, 0.3g Alg, 0.2g NaPS and 60. Mu.L dimethylaniline, after polymerization for 24h at room temperature, were extruded drop wise to CaCl 2 Obtaining a spherical microgel having a response temperature of about 42 ℃ in an aqueous solution; subsequently, the molar ratio of the two comonomers is regulated, and microgels with response temperatures of about 45 ℃, 48 ℃ and 50 ℃ are obtained in sequence; washing with deionized water for several times to remove unreacted monomers, crosslinking agent and the like; filtering, freeze-drying, and respectively placing 4 kinds of microgels into 2 mg.mL -1 Cefazolin, curcumin, insulin or 0.1 mg.ml -1 Swelling for 24h in the epidermal cell growth factor solution to obtain four thermosensitive drug-carrying microgels loaded with four different drug solutions respectively.
(3) Preparation of dressing: adding 2g of clay into 10g of deionized water, and uniformly stirring to obtain a solution with the mass fraction of 20 wt.%; then adding 3g of monomer AAm, 0.3g of NaPS and 60 mu L of dimethylaniline to prepare a prepolymer, dividing the prepolymer into four parts, respectively adding 1.0g of the four prepared temperature-sensitive drug-carrying microgels, respectively coating the coating liquid (shown in figure 1) for coating the 4 temperature-sensitive drug-carrying microgels on the areas I-IV of the conductive fabric, and reacting for 24 hours at room temperature to obtain a final product; wherein the areas of the areas are uniform and are 40X 40mm 2 Coating liquid is distributed in a dot-like array mode, the diameter of each single coating point is 5mm, and the adjacent distance is 5mm;the interval between the adjacent coating areas is 4mm, and the thickness of the prepolymer liquid coated with the temperature-sensitive drug-carrying microgel is 1.5mm.
And (3) effect verification: the prepared dressing and an external power supply are assembled into an intelligent electric heating dressing for temperature control sectional drug delivery, when the output voltage is 6V, the temperature of a fabric layer is measured to be about 54 ℃, the temperature of a drug dressing layer is increased to 43 ℃ after 80 seconds, and the sensitive drug-carrying microgel in the area I is subjected to phase transition immediately and releases the drug-carrying; after the preset time, 8V voltage is applied to the area II, the temperature of the drug dressing layer is stabilized to about 45 ℃, the sensitive drug-carrying microgel of the area II reaches the critical phase transition temperature, and another drug is released in response to the stimulus; by analogy, targeted quantitative and timed drug administration can be realized.
The conductive fabric provided by the invention is provided with a plurality of coating areas capable of independently controlling heating, the phase transition temperatures of the thermosensitive drug-carrying microgels in different coating areas are different, and the types of the loaded drug solutions are different, when the temperature-controlled sectional drug delivery is carried out in practical application, the temperature is controlled sequentially according to the increasing condition of the phase transition temperature of each thermosensitive drug-carrying microgel, wherein the thermosensitive drug-carrying microgel with lower temperature releases the drug firstly, and the thermosensitive drug-carrying microgel with higher temperature releases the drug after being heated.
While particular embodiments of the present invention have been described above, it will be appreciated by those skilled in the art that these are merely illustrative, and that many variations or modifications may be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined only by the appended claims.

Claims (9)

1. The intelligent electric heating dressing is characterized by comprising an electric heating conductive fabric, wherein the electric heating conductive fabric is provided with a plurality of coating areas capable of independently controlling heating, each coating area is provided with a medicine dressing layer, each medicine dressing layer comprises a gel matrix, thermosensitive medicine-carrying microgels coated in the gel matrix and medicine solutions loaded in the thermosensitive medicine-carrying microgels, and the types of the medicine solutions loaded by the thermosensitive medicine-carrying microgels in different coating areas are different; the medicine dressing layer is provided with a plurality of gel units, the gel units are distributed in an array, the thickness of each gel unit is 0.2-2mm, the diameter is 2-5mm, and the interval is 2-5mm;
the temperature-sensitive drug-loaded microgel is prepared by the following method:
adding two temperature-sensitive comonomers, sodium alginate, an initiator and an accelerator into an inorganic hectorite aqueous dispersion liquid, polymerizing for 10-24 hours at room temperature, extruding the obtained polymer into a calcium chloride aqueous solution dropwise to form spherical microgel, and obtaining the spherical microgel with different response temperatures by adjusting the molar ratio of the two temperature-sensitive comonomers; washing the spherical microgel with deionized water, filtering, freeze-drying, and putting the freeze-dried spherical microgel with different response temperatures into different drug solutions respectively to swell for 12-24 hours to prepare various thermosensitive drug-carrying microgels loaded with different types of drug solutions.
2. The intelligent electrothermal dressing for temperature-controlled segmented administration according to claim 1, wherein insulating separation areas with the width of 1-5mm are reserved between the drug dressing layers of different coating areas, and the insulating separation areas are coated with gel matrixes without thermosensitive drug-carrying microgels.
3. The method for preparing the intelligent electrothermal dressing for temperature-controlled segmented administration according to claim 1 or 2, comprising the following steps:
s1, soaking a fabric in a dispersion liquid of a carbon-containing material, taking out and passing through a roller to realize pad dyeing, and repeating pad dyeing for a plurality of times after drying to prepare a conductive fabric;
s2, adding two temperature-sensitive comonomers, sodium alginate, an initiator and an accelerator into an inorganic hectorite aqueous dispersion, polymerizing for 10-24 hours at room temperature, extruding the obtained polymer into a calcium chloride aqueous solution dropwise to form spherical microgel, and obtaining the spherical microgel with different response temperatures by adjusting the molar ratio of the two temperature-sensitive comonomers; washing the spherical microgel with deionized water, filtering, freeze-drying, and putting the freeze-dried spherical microgel with different response temperatures into different drug solutions respectively to swell for 12-24 hours to prepare a plurality of thermosensitive drug-carrying microgels loaded with different types of drug solutions;
s3, adding an acrylamide monomer, an initiator and an accelerator into the inorganic hectorite aqueous dispersion to form a prepolymer solution, adding the thermosensitive drug-carrying microgel, coating the prepolymer solution on the surface of the conductive fabric, and reacting the thermosensitive drug-carrying microgel loaded with different types of drug solutions at room temperature for 8-24 hours to enable the prepolymer solution to form a gel matrix coating the thermosensitive drug-carrying microgel through polymerization reaction, thus finally obtaining the intelligent electrothermal dressing with temperature control and sectional administration.
4. The method for preparing the intelligent electrothermal dressing for temperature-controlled segmented administration according to claim 3, wherein in the step S1, the fabric is knitted, woven or non-woven fabric formed by one or more fibers of cotton, nylon, polyphenylene sulfide or polypropylene; the carbon material is one or more of graphene oxide, carbon nanotubes, conductive carbon black or graphite; the mass fraction of the carbon material in the dispersion is 0.1-0.5 wt%, the solvent of the dispersion is a mixture of ethanol and water, and the volume ratio of the ethanol to the water is 1:10-1:1.
5. The method for preparing the intelligent electrothermal dressing for temperature-controlled segmented administration according to claim 3, wherein in the step S2, two temperature-sensitive comonomers are 2-methyl-2-acrylic acid-2- (2-methoxyethoxy) ethyl ester and oligopolyethylene glycol methyl ether methacrylate, and the response temperature of the spherical microgel is regulated and controlled by adjusting the molar ratio of the two monomers, and the change range of the response temperature is 35-60 ℃.
6. The method for preparing the intelligent electrothermal dressing with temperature-controlled and sectional dosing according to claim 3, wherein in the step S2, the inorganic hectorite aqueous dispersion is obtained by uniformly dispersing inorganic hectorite in deionized water, the total content of the added two temperature-sensitive comonomers is 5-20wt.% of the mass of the deionized water, and the inorganic hectorite and the sodium alginate are deionized0.5-3wt.% of water, 2% of calcium chloride aqueous solution, and 0.1-2 mg.mL of medicinal solution -1 。
7. The method for preparing a temperature-controlled sectional-drug-delivery intelligent electrothermal dressing according to claim 3, wherein in the step S2, the particle size of the spherical microgel after lyophilization is 50-200 μm.
8. The method for preparing the temperature-controlled sectional-dosing intelligent electrothermal dressing according to claim 3, wherein in the step S3, the inorganic hectorite aqueous dispersion is obtained by uniformly dispersing inorganic hectorite in water, the content of the inorganic hectorite is 5-20wt.% of the water mass, the acrylamide monomer is 10-30wt.% of the water mass, and the temperature-sensitive drug-loaded microgel is 10-40wt.% of the acrylamide monomer.
9. The method for preparing the intelligent electrothermal dressing for temperature-controlled segmented administration according to any one of claims 4 to 8, wherein in steps S2 and S3, the initiator is one or more of potassium persulfate, ammonium persulfate and sodium persulfate, and the accelerator is N, N ’ ,N ’ One or more of tetramethyl ethylenediamine or N, N-dimethylaniline,
wherein: the amount of the initiator in the step S2 is 1-10wt.% of the content of the two temperature-sensitive comonomers, and the amount of the initiator in the step S3 is 1-10wt.% of the content of the acrylamide monomer; the using amount of the accelerator in the step S3 is 0.2-0.8% of the volume of the prepolymer.
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