CN115475242A - Non-invasive composite photothermal dressing, preparation method thereof and application thereof in tumor targeted therapy - Google Patents
Non-invasive composite photothermal dressing, preparation method thereof and application thereof in tumor targeted therapy Download PDFInfo
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Abstract
The invention relates to a non-invasive composite photothermal dressing, a preparation method thereof and application thereof in tumor targeted therapy. The invention innovatively provides a novel non-invasive nano photothermal film for treating skin or near-epidermal tumors, and aims to solve the problems that the current blood or intratumoral injection type photothermal tumor treatment medicine has low photothermal conversion efficiency, and has potential cell biotoxicity particularly after being delivered into blood or tumors.
Description
Technical Field
The invention belongs to the technical field of nano composite materials, relates to a composite photothermal dressing, a preparation method thereof and application thereof in tumor targeted therapy, and particularly relates to a non-invasive composite photothermal dressing, a preparation method thereof and application thereof in tumor targeted therapy.
Background
Cancer is the first enemy of human, no effective treatment method is available at present, and surgical resection, radiotherapy and chemotherapy are the main ways to treat cancer, but the methods have great limitations in clinical practice. For example, side effects of chemotherapy and radiotherapy may damage adjacent or distant healthy tissues or organs, while surgical resection and post-operative wound healing may induce distant metastasis of cancer cells. Therefore, the development of non-invasive, targeted therapeutic strategies that can assist conventional therapeutic approaches has become an important research topic.
In recent years, photo-thermal therapy (PTT) based on Near-infrared has attracted more and more attention, which uses photo-thermal drugs to absorb Near-infrared (NIR) light to generate local overheating (hyperthermia) at 42-45 ℃, ablate tumor cells with poor vascularization microenvironment in a target area, and irreversibly damage diseased protein cells in the target area by changing gene expression, thereby finally achieving a therapeutic effect. Meanwhile, the lower overheating temperature can prevent unnecessary damage to the non-target area, so that compared with the traditional treatment method, the method has the characteristics of no wound, remarkable low toxicity, good biological safety and the like. In contrast, some conventional thermal treatments, including radiofrequency and microwave ablation, typically require high temperatures of 60-100 ℃ to ablate the tumor, which can affect the tumor microenvironment and compromise healthy cells, causing side effects even at the sub-cellular level. In addition, the generation and application of the near infrared rays are relatively safe and simple, special transmission and protection devices are not needed, and the near infrared rays are used as external and remote stimulation, so that the local temperature can be accurately controlled in time and space, and the adverse side effect is reduced to the minimum.
Photothermal materials are central to photothermal therapy. In clinical medicine application, the used photothermal medicine is required to have high photothermal conversion efficiency, and the scattering and absorption of near infrared light by normal tissues are also required to be reduced to the minimum, so that the self-heating phenomenon is reduced. In recent years, research into novel light absorbing materials having photothermal conversion efficiency and high light section, mainly including bio-dyes, inorganic Quantum Dots (QDs), magnetic nanoparticles, metal nanoparticles, semiconductor nanoparticles, and nanocarbon materials, has been actively conducted. Among them, a two-dimensional (2D) material, as a novel nanomaterial having an ultra-thin layer structure and excellent physicochemical properties, has received much attention in the field of nanomedicine such as bio-imaging, biosensors, implantable repair materials, drug delivery, and cancer treatment. Particularly, the wide spectral response characteristics, high photothermal conversion efficiency, high extinction coefficient and the like of the compound in a first biological infrared window (NIR-I, 650-950 nm) and a second biological infrared window (NIR-II, 1000-1700 nm) enable the compound to be widely researched for the photothermal treatment of tumors and show good treatment effect. Such as graphene and its derivatives, black Phosphorus (BP), pd nanosheets, sn, transition Metal Sulfides (TMDs), and two-dimensional metal carbonitrides (MXene), and the like.
Although these two-dimensional photothermal nanomedicine studies further expand and increase the range of options for photothermal therapy materials, from the published patents and literature, photonanomedicine is currently delivered to tumor-targeted sites by in vivo injection, which inevitably involves the above-mentioned problems regarding photothermal biotoxicity and metabolism. The potential biological toxicity, biodegradability or whether the biological toxicity can be completely eliminated from the body after clinical application are not clear, and the like, and the long-term biological toxicity of normal organs in the body can be increased. Although some small-molecule organic dyes have good biocompatibility and biodegradability, the photo-thermal conversion efficiency is low, and the photo-bleaching is serious, so that the practical application of the small-molecule organic dyes in PTT is limited.
The patent CN112121164A discloses a preparation method of an intelligent photo-nano-drug for cancer treatment, which is characterized in that MXene, adriamycin (Doxorubicin) and deferasirox (Exjade) drugs are compounded to prepare a Dox-Exjade double-drug loaded intelligent photo-nano-drug MXene @ Dox-Exjade, and the Dox-Exjade double-drug loaded intelligent photo-nano-drug MXene @ Dox-Exjade is further dispersed into a PBS solution and delivered into a tumor-bearing mouse body in an intravenous injection mode to perform photo-thermal treatment on tumors. Although MXene @ Dox-Exjade has a remarkable effect of inhibiting tumor growth, the problems of biocompatibility and metabolism of MXene are not negligible, and the biological safety is not yet proved.
Patent CN112107547A discloses a hydrogel photonic crystal microsphere with photo-thermal responsiveness and a preparation method thereof, and the hydrogel photonic crystal microsphere is used for photo-thermal treatment of tumors. The hydrogel microspheres prepared by the method have near infrared light response and thermal responsiveness, can load drugs and controllably release the drugs at tumor treatment sites, and realize the removal of tumor cells in a multifunctional and synergetic manner. However, the photo-thermal responsive material is also prepared by mixing one or more than two materials of MXene, graphene quantum dots and black phosphorus quantum dots according to a certain proportion, and the problems of low photo-thermal conversion efficiency, biotoxicity and the like still exist when the materials are injected into a body for treatment.
The local targeting treatment of tumors is very attractive, and can be particularly used for treating some superficial tumors, such as melanoma, squamous cell carcinoma and the like. Compared with intravenous injection, the local treatment of tumor has direct targeting property, thereby reducing the side effect of the medicine.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a composite photothermal dressing, a preparation method thereof and application thereof in tumor targeted therapy, and particularly provides a non-invasive composite photothermal dressing, a preparation method thereof and application thereof in tumor targeted therapy.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a non-invasive composite photothermal dressing comprising an MXene film layer and a transparent medical dressing layer in a layered arrangement.
The invention innovatively provides a novel non-invasive nano photothermal film for treating skin or near-epidermal tumors, and aims to solve the problems that the current blood or intratumoral injection type photothermal tumor treatment medicine has low photothermal conversion efficiency, and has potential cell biotoxicity particularly after being delivered into blood or tumors. The MXene film is selected as a photo-thermal response material, and the photo-thermal response material has nearly 100% photo-thermal conversion efficiency on near-infrared laser of a biological window with 808nm, so that the composite photo-thermal dressing has excellent photo-thermal performance; meanwhile, by controlling the thickness of the MXene film and different types of medical transparent dressings, composite photothermal dressings with different sizes, shapes and photothermal response characteristics and suitable for different parts can be obtained, and the applicability is wide; the composite film can be easily adhered to different skin parts, is used for non-invasive treatment of epidermal or near-epidermal early-stage tumor cells, is simple and convenient to use, and has good treatment effect and application prospect.
Preferably, the mass fraction of the MXene film layer in the non-invasive composite photothermal dressing is 0.05-2.5%, such as 0.05%, 0.1%, 0.2%, 0.4%, 0.5%, 0.8%, 1.0%, 1.2%, 1.5%, 1.8%, 2.0%, 2.2%, 2.5%, etc., and other specific points in the numerical range can be selected, which is not described in detail herein.
The mass fraction of the MXene film layer in the non-invasive composite photothermal dressing is specifically selected to be 0.05-2.5%, because if the mass fraction of the MXene film layer is further increased, the visible light transmittance of the composite photothermal dressing is influenced, the in-situ observation effect on the tumor treatment effect is further influenced, and if the mass fraction of the MXene film layer is further reduced, the photothermal efficiency is low, and the temperature required by photothermal treatment cannot be reached.
Preferably, the MXene is selected from Ti 3 C 2 T x 、Ti 2 CT x Or Nb 2 CT x Any one or a combination of at least two of; wherein T is a functional group OH, F or O.
Preferably, the transparent medical dressing layer is selected from a PU adhesive transparent dressing or a PE adhesive transparent dressing.
The transparent medical dressing layer is a transparent waterproof breathable dressing with certain adhesiveness on one side, and is not limited to common brands such as 3M Tegaderm film, schlerhui IV3000, nitto31B and other common clinical PU transparent tapes and medical PE transparent tapes.
In a second aspect, the present invention provides a method of preparing a non-invasive composite photothermal dressing as described in the first aspect, the method comprising:
and (2) carrying out suction filtration on the MXene colloid dispersion liquid on the microporous filter paper by using a vacuum suction filtration method, drying to obtain an MXene film layer loaded on the microporous filter paper, and then transferring the MXene film layer to a transparent medical dressing layer to obtain the non-invasive composite photothermal dressing.
The preparation method of the non-invasive composite photothermal dressing is simple and easy to operate, is very suitable for industrial production, and has remarkable practicability.
Preferably, the concentration of the MXene colloidal dispersion is 0.01-1mg/mL, such as 0.01mg/mL, 0.05mg/mL, 0.1mg/mL, 0.2mg/mL, 0.4mg/mL, 0.5mg/mL, 0.6mg/mL, 0.7mg/mL, 0.8mg/mL, 0.9mg/mL, 1mg/mL, etc., and other specific values in the numerical range can be selected, which is not repeated herein.
Preferably, the pressure of the vacuum filtration is 0.01-0.1MPa, such as 0.01MPa, 0.02MPa, 0.04MPa, 0.05MPa, 0.06MPa, 0.08MPa, 0.09MPa, 0.1MPa, etc., and other specific values in the numerical range can be selected, which is not described in detail herein.
The specific selection of the pressure of the vacuum filtration is 0.01-0.1MPa because the filter membrane is cracked if the pressure of the vacuum filtration is further increased; if the suction filtration pressure is further reduced, MXene cannot be formed into a film.
Preferably, the pore size of the microporous filter paper is 0.22-0.45 μm.
Preferably, the microporous filter paper is a mixture film of cellulose acetate and cellulose nitrate.
Preferably, the drying means includes forced air drying at 50-90 deg.C, such as 50 deg.C, 60 deg.C, 70 deg.C, 80 deg.C, 90 deg.C, etc.; the drying time is 10-60min, such as 10min, 20min, 30min, 40min, 50min, 60min, etc., and other specific values within the numerical range can be selected, which is not described in detail herein.
Preferably, the mode of transfer is a bond-mechanical peel process.
Preferably, the preparation method of the MXene colloidal dispersion comprises the following steps:
(1) Carrying out chemical etching by taking MAX ceramic powder as a raw material, and then centrifuging and washing by using deionized water to prepare MXene aqueous phase dispersion liquid;
(2) Centrifuging the MXene aqueous phase dispersion liquid again, and taking the upper layer liquid to obtain the MXene colloidal dispersion liquid.
Preferably, the MAX ceramic powder is selected from Ti 3 AlC 2 、Ti 2 AlC or Nb 2 Any one or a combination of at least two of the alcs. Due to Ti 3 AlC 2 Ti obtained after etching 3 C 2 T x Higher chemical stability, more preferably Ti 3 AlC 2 。
Preferably, the mesh number of the MAX ceramic powder is 200-400 mesh, such as 200 mesh, 250 mesh, 300 mesh, 350 mesh, 400 mesh, and the like, and other specific values within the numerical range can be selected, which is not described herein again.
Preferably, the etching solution used in the chemical etching is a mixed solution of 7 to 12M (e.g., 7M, 8M, 9M, 10M, 11M, 12M, etc.) of HCl and 5 to 15wt% (5 wt%, 8wt%, 10wt%, 12wt%, 15wt%, etc.) of LiF, and other specific values in the above numerical range can be selected, which is not described in detail herein.
Preferably, the chemical etching is performed for 6 to 24 hours (6 hours, 10 hours, 15 hours, 20 hours, 24 hours, etc.) at 25 to 60 ℃ (e.g., 25 ℃,30 ℃,40 ℃, 50 ℃, 60 ℃, etc.), and other specific values within the above numerical range can be selected, which is not described in detail herein.
Preferably, the chemical etching is performed while stirring.
Preferably, the deionized water washing is performed at a rotation speed of 2000-5000rpm (e.g., 2000rpm, 3000rpm, 4000rpm, 5000rpm, etc.), and other specific values within the numerical range can be selected, which is not described in detail herein.
Preferably, the deionized water is washed to a pH value greater than 6, such as pH =6.5, pH =7.0, pH =7.5, pH =8.0, pH =8.5, pH =9.0, pH =9.5, and the like, and other specific values within the range of values are selectable, and are not described in detail herein.
Preferably, the rotation speed of the centrifugation in the step (1) is 3500-7500rpm, such as 3500rpm, 4000rpm, 4500rpm, 5000rpm, 5500rpm, 6000rpm, 6500rpm, 7000rpm, 7500rpm and the like; the time is 5-30min, such as 5min, 10min, 15min, 20min, 25min, 30min, etc., and other specific values within the above numerical range can be selected, which is not described in detail herein.
Preferably, the concentration of the MXene aqueous phase dispersion liquid is 0.5-3mg/mL, such as 0.5mg/mL, 1mg/mL, 1.5mg/mL, 2mg/mL, 2.5mg/mL, 3mg/mL, and the like, and other specific values in the numerical range can be selected, which is not described in detail herein.
Preferably, the rotation speed of the centrifugation in the step (2) is 2500-4500rpm, such as 2500rpm, 3000rpm, 3500rpm, 4000rpm, 4500rpm and the like; the time is 10-60min, such as 10min, 20min, 30min, 40min, 50min, 60min, etc., and other specific values within the above numerical range can be selected, which are not described in detail herein.
Preferably, the MXene colloid has a flake diameter of 1-10 μm, such as 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, and other specific values within the value range can be selected, which is not described herein again.
In a third aspect, the invention provides a use of the non-invasive composite photothermal dressing according to the first aspect in preparation of a drug or a medical material for tumor targeted therapy.
Compared with the prior art, the invention has the following beneficial effects:
the invention innovatively provides a novel non-invasive nano photothermal film for treating skin or near-epidermal tumors, and aims to solve the problems that the current blood or intratumoral injection type photothermal tumor treatment medicine has low photothermal conversion efficiency, and has potential cell biotoxicity particularly after being delivered into blood or tumors. The MXene film is selected as a photo-thermal response material, and the photo-thermal response material has nearly 100% photo-thermal conversion efficiency on near-infrared laser of a biological window with 808nm, so that the composite photo-thermal dressing has excellent photo-thermal performance; meanwhile, by controlling the thickness of the MXene film and different types of medical transparent dressings, composite photothermal dressings with different sizes, shapes and photothermal response characteristics and suitable for different parts can be obtained, and the applicability is wide; the composite film can be easily adhered to different skin parts, is used for non-invasive treatment of epidermal or near-epidermal early-stage tumor cells, is simple and convenient to use, and has good treatment effect and application prospect.
Drawings
FIG. 1 is a pictorial view of a non-invasive composite photothermal dressing in accordance with the present invention;
FIG. 2 is a schematic diagram of the use of the non-invasive composite photothermal dressing for treating a tumor mouse model according to the present invention;
FIG. 3 is a graph showing the temperature change of the heating-cooling cycle under laser irradiation of the non-invasive composite photothermal dressings prepared in examples 1, 4 and 5;
FIG. 4 is a graph showing the use of 0.38W/cm in a tumor-bearing mouse after placing the composite photothermal dressing prepared in example 1 2 808nm near-infrared laser irradiation for 0s, 3s, 7s and 10s, and then carrying out infrared thermal imaging on the tumor part;
FIG. 5 is a tumor site observation image on day 0, day 3, day 7, day 14, and day 21 of the blank group of mice and the non-invasive complex photothermal dressing +808nm near-infrared light irradiated group of mice in example 1;
FIG. 6 is a tumor tissue anatomical map of the blank group, 808 nm-only near-infrared irradiation group, and the non-invasive composite photothermal dressing and 808 nm-near-infrared irradiation group of example 1 at 21 days;
fig. 7 is H & E staining patterns of tumor tissues on day 0, 7, 14 and 21 of the blank group, the example 1 non-invasive composite photothermal dressing and 808nm near-infrared irradiation group.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
0.22 μm microporous filter paper and 0.45 μm microporous filter paper referred to below were purchased from Merck chemical technology (Shanghai) Inc.; the melanoma cell is from Shanghai cell bank of Chinese academy of sciences; the BLAB/c Nude mice were from the laboratory animal technology, inc. of Wei Tongli, beijing.
The animal experiments related to the following contents are approved by the animal ethics committee of the research institute of physical and chemical technology of the Chinese academy of sciences, and meet the standard requirements for animal welfare.
Example 1
The embodiment provides a non-invasive composite photothermal dressing which is composed of an MXene film layer (mass fraction of 0.5%) and a transparent medical dressing layer (mass fraction of 99.5%) which are arranged in a stacking mode. The preparation method comprises the following steps:
(1) 0.5g of Ti with the particle size of 400 meshes is weighed 3 AlC 2 Slowly adding the powder into a mixed solution of 0.8g LiF and 10mL 9M HCl, and stirring and reacting for 24 hours at the temperature of 25 ℃, wherein the stirring speed is 300rpm;
(2) Centrifuging at 3500rpm for 5min after the reaction is finished, pouring out the supernatant, and then repeatedly shaking and washing with deionized water until the pH value of the dispersion is 6.5;
(3) Centrifuging the dispersion at 3500rpm for 60min to obtain Ti with concentration of 2mg/mL 3 C 2 T x (T is a functional group OH, F or O) colloidal dispersion;
(4) Diluting the colloidal dispersion liquid to 0.1mg/mL by using deionized water, carrying out suction filtration on 50mL of the diluted dispersion liquid to a microporous filter paper with the aperture of 0.22 mu m by using a vacuum filtration method, wherein the vacuum pressure of the suction filtration is 0.1MPa, and carrying out forced air drying at 60 ℃ for 1h after the suction filtration is finished to obtain an MXene thin film layer loaded by the microporous filter paper;
(5) Adhering the 3M Tegaderm film 1626W medical transparent dressing to one side of the MXene film layer, and applying pressure to ensure that the adhesion is tight and uniform;
(6) The microporous filter membrane is then mechanically peeled off to obtain the non-invasive composite photothermal dressing, and the physical diagram of the non-invasive composite photothermal dressing is shown in figure 1. The non-invasive composite photothermal dressing is used for treating a tumor mouse model in a way shown in figure 2.
Example 2
The embodiment provides a non-invasive composite photothermal dressing which is composed of an MXene film layer and a transparent medical dressing layer which are arranged in a stacked mode. The preparation method comprises the following steps:
(1) 0.5g of Ti with the particle size of 300 meshes is weighed 3 AlC 2 Powder, slowAdding the mixture into a mixed solution of 0.8g LiF and 10mL12M HCl, and stirring and reacting for 12 hours at the temperature of 40 ℃, wherein the stirring speed is 300rpm;
(2) Centrifuging at 3500rpm for 5min after the reaction is finished, pouring out the supernatant, and then repeatedly shaking and washing with deionized water until the pH value of the dispersion is 7;
(3) Centrifuging the dispersion at 4500rpm for 10min to obtain Ti with concentration of 2mg/mL 3 C 2 T x (T is a functional group OH, F or O) colloidal dispersion;
(4) Diluting the colloidal dispersion liquid to 0.05mg/mL by using deionized water, performing suction filtration on 100mL of the diluted dispersion liquid to obtain microporous filter paper with the aperture of 0.45 mu m by using a vacuum filtration method, performing suction filtration under the vacuum pressure of 0.05MPa, and performing forced air drying at 80 ℃ for 15min after the suction filtration is finished to obtain an MXene film layer loaded on the microporous filter paper;
(5) Adhering the Schlenhui IV3000 medical transparent dressing to one side of the MXene film layer, and applying pressure to ensure tight and uniform adhesion;
(6) And then mechanically peeling off the microporous filter membrane to obtain the non-invasive composite photothermal dressing.
Example 3
The embodiment provides a non-invasive composite photothermal dressing which consists of an MXene film layer and a transparent medical dressing layer which are arranged in a laminated mode. The preparation method comprises the following steps:
(1) 0.5g of Ti with the particle size of 200 meshes is weighed 3 AlC 2 Slowly adding the powder into a mixed solution of 0.8g LiF and 10mL7M HCl, and stirring and reacting for 6 hours at the temperature of 25 ℃, wherein the stirring speed is 300rpm;
(2) Centrifuging at 3500rpm for 5min after the reaction is finished, pouring out the supernatant, and then repeatedly shaking and washing with deionized water until the pH value of the dispersion is 8;
(3) Centrifuging the dispersion at 2500rpm for 60min to obtain Ti with concentration of 2mg/mL 3 C 2 T x (T is a functional group OH, F or O) colloidal dispersion;
(4) Diluting the colloidal dispersion liquid to 0.01mg/mL by using deionized water, performing suction filtration on 100mL of the diluted dispersion liquid to obtain microporous filter paper with the aperture of 0.22 mu m by using a vacuum filtration method, performing suction filtration under the vacuum pressure of 0.02MPa, and performing forced air drying at 50 ℃ for 60min after the suction filtration is finished to obtain an MXene film layer loaded on the microporous filter paper;
(5) Adhering NITTO31B medical transparent dressing to one side of the MXene film layer, and applying pressure to ensure tight and uniform adhesion;
(6) And then mechanically peeling off the microporous filter membrane to obtain the non-invasive composite photothermal dressing.
Example 4
The embodiment provides a non-invasive composite photothermal dressing which is composed of an MXene film layer (mass fraction of 0.1%) and a transparent medical dressing layer (mass fraction of 99.9%) which are arranged in a stacking mode. The preparation method differs from example 1 only in that the suction filtration amount of the diluted dispersion in step (4) is different, resulting in a difference in the mass ratio of the MXene thin film layer in the final product.
Example 5
This example provides a non-invasive composite photothermal dressing, which is composed of a Mxene film layer (mass fraction of 2.5%) and a transparent medical dressing layer (mass fraction of 97.5%) in a stacked arrangement. The preparation method differs from example 1 only in the amount of suction filtration of the diluted dispersion in step (4), resulting in a different mass ratio of the MXene film layer in the final product.
Example 6
The embodiment provides a non-invasive composite photothermal dressing which consists of an MXene film layer and a transparent medical dressing layer which are arranged in a laminated mode. The preparation method differs from example 1 only in that Ti in step (1) 3 AlC 2 Powder is replaced by equal amount of Ti 2 The AlC powder and other conditions are kept unchanged.
Example 7
The embodiment provides a non-invasive composite photothermal dressing which is composed of an MXene film layer and a transparent medical dressing layer which are arranged in a stacked mode. The preparation method differs from example 1 only in that Ti in step (1) is added 3 AlC 2 Powder is replaced by equal amount of Nb 2 The AlC powder and other conditions are kept unchanged.
Evaluation test 1
Evaluation of photothermal response characteristics of the non-invasive composite photothermal dressings prepared in examples 1, 4 and 5:
(1) Healthy female BLAB/c Nude mice (5-6 weeks old, 16-20 g) were used to establish a subcutaneous mouse melanoma model: subcutaneous injection of 5X 10 5 Melanoma cells (type B16) to the right of the mouse gluteus maximus site when the tumor volume reached 100mm 3 When the modeling is successful, the modeling is successful;
(2) The non-invasive composite photothermal dressing prepared in examples 1, 4 and 5 was cut into 2 cm-sized pieces and adhered to the tumor-bearing mouse target site, the near-infrared laser was perpendicular to the photothermal dressing surface by 15cm, and then the distance was 0.38W/cm 2 The laser was turned on and off for 10s each cycle with 3 photo-thermal cycles (heating-cooling cycles) under 808nm illumination, and the temperature profile is shown in fig. 3. As can be seen from fig. 3: the composite photothermal dressings have rapid photothermal response rate, and the maximum stable temperature of the target position is increased along with the increase of the MXene mass fraction. When the laser is turned off, the surface temperature of the photothermal dressing is rapidly reduced to the surface temperature of the mouse body, which shows that the photothermal dressing has excellent thermal conductivity, and is beneficial to the heat generated by photothermal to be diffused to the tumor position, so that the tumor cells at the target position are killed by local overheating.
FIG. 4 is a graph showing the tumor-bearing mice used 0.38W/cm after being adhered with the non-invasive composite photothermal dressing prepared in example 1 2 And 808nm near-infrared laser irradiation for 0s, 3s, 7s and 10 s. As can be seen from fig. 4: the photothermal dressing has good photothermal response efficiency, reaches stable heat balance temperature after irradiating for 10s, has even temperature distribution, and can effectively kill tumor cells at a target position.
Evaluation test 2
The therapeutic effect of the non-invasive composite photothermal dressing on mouse melanoma is as follows:
(1) Healthy female BLAB/c Nude mice (5-6 weeks old, 16-20 g) were used to establish a subcutaneous mouse melanoma model: subcutaneous injection of 5X 10 5 Melanoma cells (type B16) to the gluteus maximus region of miceRight side, when tumor volume reaches 100mm 3 When the modeling is successful, the modeling is successful;
(2) All mice were randomly divided into 7 groups (n = 6/group) (2.1) blank group (without any treatment) (2.2) 808nm only near-infrared light irradiation group (2.3) example 1 non-invasive composite photothermal dressing +808nm near-infrared light irradiation group (2.4) example 2 non-invasive composite photothermal dressing +808nm near-infrared light irradiation group (2.5) example 3 non-invasive composite photothermal dressing +808nm near-infrared light irradiation group (2.6) example 6 non-invasive composite photothermal dressing +808nm near-infrared light irradiation group (2.7) example 7 non-invasive composite photothermal dressing +808nm near-infrared light irradiation group. After 24h, near infrared laser irradiation is carried out for in vivo photothermal therapy (808nm, 0.38W/cm) 2 30 min), the treatment was carried out for 7 days, and the same treatment was carried out every day.
(3) The tumor sites were photographed on day 0, day 3, day 7, day 14, and day 21 for the blank group of mice and the non-invasive complex photothermal dressing +808nm near-infrared light irradiated group of mice in example 1, as shown in fig. 5. As can be seen from fig. 5: the tumor cell growth of the mouse subjected to the photothermal dressing targeted therapy is obviously inhibited and killed, and the tumor protrusion part is sunken, so that the tumor cells are greatly killed. However, the tumor cells of the mice without any intervention showed a tendency to grow continuously, and a phenomenon of explosive growth occurred on days 7 to 21, and the tumor volume increased significantly. And the change rule of the tumor volume of each group with time is measured according to the following formula: tumor volume = [ (tumor length) × (tumor width) 2 ][ 2 ] As shown in Table 1, it can be seen from Table 1 that: the growth of tumor cells of a mouse subjected to photothermal dressing targeted therapy is obviously inhibited and killed, the volume of the tumor cells is obviously reduced, and the growth rate is obviously reduced, so that the composite photothermal dressing has the effect of obviously inhibiting and killing the near-epidermal melanoma cells.
(4) The mice were dissected on day 21, and the sizes of tumor tissues in the blank group, the 808 nm-only near-infrared light irradiation group, and the non-invasive composite photothermal dressing +808 nm-near-infrared light irradiation group of example 1 are shown in fig. 6, and it can be seen from fig. 6 that: after 21 days of treatment, the tumor cell volumes of the mice in the blank group and the 808nm near-infrared laser irradiation treatment group are obviously larger than those of the photothermal dressing targeted treatment group, and further, the photothermal dressing has an excellent targeted photothermal treatment effect on the near-epidermal tumor cells.
TABLE 1 tumor volume size in different groups of mice as a function of time (mm) 3 )
| Group of | |
3 |
7 days | 14 days | 21 days |
| (2.1) | 121±5 | 143±4 | 169±5 | 207±6 | 347±2 |
| (2.2) | 128±2 | 151±3 | 176±5 | 237±2 | 354±4 |
| (2.3) | 132±6 | 101±3 | 94±3 | 86±4 | 71±6 |
| (2.4) | 123±4 | 100±2 | 97±2 | 93±3 | 82±6 |
| (2.5) | 136±3 | 115±5 | 103±2 | 98±4 | 87±3 |
| (2.6) | 129±2 | 122±5 | 115±2 | 101±3 | 90±1 |
| (2.7) | 137±5 | 122±2 | 117±6 | 103±3 | 88±2 |
(5) Tumor fixation, paraffin embedding, 8mm sectioning, H & E staining, digital microscopic observation, H & E staining of tumor cells and pathological analysis were performed on the blank group of mice and the non-invasive complex photothermal dressing +808nm near-infrared light irradiation group of mice of example 1 with 4% neutral paraformaldehyde on days 0, 7, 14, and 21, respectively, as shown in fig. 7 (scale in the figure is 50 μm). The results show that the number of cancer cells is rapidly reduced after the photothermal dressing treatment compared with the blank group, and the normal tissue morphology is mainly shown after 21 days; the cancer cell density of the blank mouse always presents a high-density distribution state, and is typical pathological morphology of tumor cell tissues. The above results again demonstrate that the composite photothermal dressing of the present invention has excellent photothermal targeting tumor treatment effect.
The applicant states that the invention is described by the above examples to illustrate a non-invasive composite photothermal dressing of the invention, its preparation method and its application in tumor-targeted therapy, but the invention is not limited to the above examples, i.e. it does not mean that the invention must be implemented by the above examples. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of the raw materials of the product of the present invention, and the addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that, in the above embodiments, the various features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, the present invention does not separately describe various possible combinations.
Claims (10)
1. The non-invasive composite photothermal dressing is characterized by comprising an MXene film layer and a transparent medical dressing layer which are arranged in a stacking mode.
2. The non-invasive composite photothermal dressing according to claim 1, wherein the weight fraction of the MXene film layer in the non-invasive composite photothermal dressing is 0.05-2.5%.
3. The non-invasive composite photothermal dressing according to claim 1 or 2, wherein MXene is selected from Ti 3 C 2 T x 、Ti 2 CT x Or Nb 2 CT x Any one or a combination of at least two of; wherein T is a functional group OH, F or O.
4. The non-invasive composite photothermal dressing according to any one of claims 1 to3, wherein said transparent medical dressing layer is selected from the group consisting of PU adhesive transparent dressing or PE adhesive transparent dressing.
5. The method of making a non-invasive composite photothermal dressing according to any of claims 1-4, wherein the method of making comprises:
and (2) carrying out suction filtration on the MXene colloid dispersion liquid on the microporous filter paper by using a vacuum suction filtration method, drying to obtain an MXene film layer loaded on the microporous filter paper, and then transferring the MXene film layer to a transparent medical dressing layer to obtain the non-invasive composite photothermal dressing.
6. The method for preparing the non-invasive composite photothermal dressing according to claim 5, wherein the concentration of the MXene colloidal dispersion is 0.01-1mg/mL;
preferably, the pressure of the vacuum filtration is 0.01-0.1MPa;
preferably, the pore diameter of the microporous filter paper is 0.22-0.45 μm;
preferably, the microporous filter paper is a mixture film of cellulose acetate and cellulose nitrate.
7. The method for preparing the non-invasive composite photothermal dressing according to claim 5 or 6, wherein the drying manner comprises forced air drying, wherein the drying temperature is 50-90 ℃, and the drying time is 10-60min;
preferably, the mode of transfer is a bond-mechanical peel process.
8. The method for preparing the non-invasive composite photothermal dressing according to any one of claims 5 to 7, wherein the MXene colloidal dispersion is prepared by the method comprising:
(1) Carrying out chemical etching by taking MAX ceramic powder as a raw material, centrifuging, and washing with deionized water to prepare MXene aqueous phase dispersion liquid;
(2) Centrifuging the MXene aqueous phase dispersion liquid again, and taking the upper layer liquid to obtain the MXene colloidal dispersion liquid.
9. The method of preparing the non-invasive composite photothermal dressing of claim 8, wherein the MAX ceramic powder is selected from Ti 3 AlC 2 、Ti 2 AlC or Nb 2 Any one or a combination of at least two of AlC;
preferably, the mesh number of the MAX ceramic powder is 200-400 meshes;
preferably, the etching solution used for the chemical etching is a mixed solution of 7-12M HCl and 5-15wt% LiF;
preferably, the chemical etching is carried out at 25-60 ℃ for 6-24h;
preferably, the chemical etching is performed while stirring;
preferably, the deionized water washing is carried out at a rotation speed of 2000-5000 rpm;
preferably, the deionized water is washed to a pH value of more than 6;
preferably, the rotation speed of the centrifugation in the step (1) is 3500-7500rpm, and the time is 5-30min;
preferably, the concentration of the MXene aqueous phase dispersion liquid is 0.5-3mg/mL;
preferably, the rotation speed of the centrifugation in the step (2) is 2500-4500rpm, and the time is 10-60min;
preferably, the MXene colloid has a flake diameter of 1-10 μm.
10. Use of the non-invasive composite photothermal dressing according to any one of claims 1-4 in the preparation of a drug or medical material for tumor targeted therapy.
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