Hollow Cu7S4Nano cubic structure and preparation method and application thereof
阅读说明：本技术 一种空心Cu7S4纳米立方结构及其制备方法和应用 (Hollow Cu7S4Nano cubic structure and preparation method and application thereof ) 是由 蔡称心 孙宇杰 胡耀娟 乔玲 吴萍 于 2021-03-12 设计创作，主要内容包括：本发明公开了一种空心Cu-7S-4纳米立方结构及其制备方法和应用,该空心Cu-7S-4纳米立方结构的边长约为70～80nm,形貌为空心纳米立方结构；其制备方法为：将聚乙烯吡咯烷酮溶于水中,然后加入乙酸铜、氢氧化钠、抗坏血酸搅拌,随后油浴加热,加入硫化钠持续反应,待反应完全后将产物离心洗涤分散。本发明制备的空心Cu-7S-4纳米立方结构,具有良好的稳定性和生物相容性,在近红外光区900～1100nm处具有较大的吸收,且光热转换效率高,为肿瘤细胞的光热治疗提供了条件,并且其制备方法简单,条件温和,环境友好,同时本发明材料由于表面存在的大的空穴,可以更加高效地应用在制备治疗癌症的光热治疗试剂中。(The invention discloses a hollow Cu 7 S 4 Nano cubic structure, preparation method and application thereof, and hollow Cu 7 S 4 The side length of the nano cubic structure is about 70-80 nm, and the shape is hollow nanoA cubic structure of rice; the preparation method comprises the following steps: dissolving polyvinylpyrrolidone in water, adding copper acetate, sodium hydroxide and ascorbic acid, stirring, heating in an oil bath, adding sodium sulfide for continuous reaction, and centrifuging, washing and dispersing the product after the reaction is completed. Hollow Cu prepared by the invention 7 S 4 The nano cubic structure has good stability and biocompatibility, has larger absorption at the near infrared region of 900-1100 nm, has high photo-thermal conversion efficiency, provides conditions for photo-thermal treatment of tumor cells, has simple preparation method, mild conditions and environmental friendliness, and can be more efficiently applied to preparation of photo-thermal treatment reagents for treating cancers due to large cavities on the surface of the material.)
1. Hollow Cu7S4A nano-cubic structure characterized in that said Cu7S4Is of a hollow nano-cubic structure and mainly consists of a precursor Cu2Partial oxidation of O to CuO, with S2-After anion exchange.
2. Hollow Cu according to claim 17S4A nano-cubic structure characterized in that said hollow Cu7S4The side length of the nano cubic structure is 70-80 nm.
3. The hollow Cu of claim 17S4The preparation method of the nano cubic structure is characterized by comprising the following steps of: dissolving polyvinylpyrrolidone in deionized water, sequentially adding copper acetate, sodium hydroxide and ascorbic acid AA, stirring, heating in an oil bath, adding sodium sulfide under stirring for reaction, centrifuging the product, taking the lower layer precipitate for washing after the reaction is completed, and dispersing the product in deionized water to obtain the hollow Cu7S4A nano-cubic structure.
4. Hollow Cu according to claim 37S4The preparation method of the nano cubic structure is characterized in that the polyvinylpyrrolidone is preferably dissolved in 500mL of deionized water of 400-5 g in proportion.
5. Hollow Cu according to claim 37S4The preparation method of the nano cubic structure is characterized in that the sodium hydroxide is a sodium hydroxide aqueous solution with the concentration of 1-2mol/L, and the solution is adjustedThe pH value of the solution is 11.0-12.0, the copper acetate is a copper acetate aqueous solution with the concentration of 0.1-0.2mol/L, the ascorbic acid is an ascorbic acid aqueous solution with the concentration of 0.1-0.2mol/L, the sodium hydroxide aqueous solution, the copper acetate aqueous solution and the ascorbic acid aqueous solution are in a volume ratio of 3-5: 3-4: 6-8.
6. Hollow Cu according to claim 37S4The preparation method of the nano cubic structure is characterized in that the stirring is magnetic stirring, and the stirring time is 30-40 min.
7. Hollow Cu according to claim 37S4The preparation method of the nano cubic structure is characterized in that the oil bath heating temperature is 80-100 ℃.
8. Hollow Cu according to claim 37S4The preparation method of the nano cubic structure is characterized in that after a sodium sulfide aqueous solution with the concentration of 0.1-0.2mol/L is added, the reaction time is 1.5-2 h, and the volume ratio of the sodium sulfide aqueous solution to the copper acetate aqueous solution is 1.5-2.5: 3-4.
9. The hollow Cu of claim 17S4Use of a nanocube structure for the preparation of a photothermal therapeutic agent for the treatment of cancer.
10. Use according to claim 9, wherein the hollow Cu7S4The nano cubic structure is loaded with cancer treatment drugs to carry out photo-thermal-drug synergistic treatment.
Technical Field
The invention belongs to a nano inorganic material, and particularly relates to hollow Cu7S4A nano cubic structure, a preparation method and application thereof.
Background
Copper chalcogenide (Cu)2-xS) is an important semiconductor with unique electronic, optical and chemical properties, is a promising material, and has potential application values in many fields such as sensors, solar radiation absorbers, catalysts, nanoscale switches and the like. At present, several methods such as solvothermal microwave method, solvothermal, hydrothermal, chemical conversion and ultrasonic treatment methods are available for synthesizing Cu2-xAnd (3) S nanoparticles. Cu2-xS nanoparticles (Cu)2-xS NPs), an emerging nano-platform with dual diagnostic and therapeutic applications, is being extensively studied in this "cancer war" era due to its versatility and adaptability. Cu2- xThe multifunctional properties of S NPs semiconductors have been extensively studied. Their emergence as promising therapeutic agents for cancer. Because of their different diagnostic and therapeutic potential, such nanoparticles have attracted the greatest interest among various inorganic materials due to biocompatibility, low toxicity and low cost. But the ability of the material to be bio-metabolised remains to be enhanced.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems of toxicity, low stability, poor targeting property and the like of the existing photo-thermal nano material, the invention provides a hollow Cu7S4Nano-cubic structure of the hollow Cu7S4The nano cubic structure has excellent photo-thermal conversion performance, good targeting property, low biotoxicity and low cost; effectively solves the problems of low cytotoxicity and low photo-thermal conversion efficiency and the like.
The invention also provides hollow Cu7S4A preparation method and application of a nano cubic structure.
The technical scheme is as follows: in order to achieve the purpose, the invention provides hollow Cu7S4Nano cubic structure of said Cu7S4Is a hollow nano cubic structure, wherein the molar ratio of copper to sulfur is 7: 4 is made of a precursor Cu2O is partially oxidized to CuO and finally reacts with S2-After anion exchange, the final product Cu is obtained7S4。
Wherein the hollow Cu7S4The side length of the nano cubic structure is 70-80 nm.
Wherein the hollow Cu7S4The ultraviolet spectrum of the nano cubic structure has a characteristic absorption broad peak at 900-1100 nm.
The hollow Cu of the invention7S4The preparation method of the nano cubic structure comprises the following steps: dissolving polyvinylpyrrolidone in deionized water, sequentially adding copper acetate, sodium hydroxide solution and ascorbic acid AA, stirring, heating in an oil bath, adding sodium sulfide under stirring for reaction, centrifuging the product, washing the lower layer precipitate after the reaction is completed, and dispersing the product in deionized water to obtain the hollow Cu7S4A nano-cubic structure.
Wherein the polyvinylpyrrolidone is dissolved in 500mL of 400-500mL deionized water according to the proportion of 2.5-5 g and has the molecular weight of 10000 or 24000.
Wherein the sodium hydroxide is a sodium hydroxide aqueous solution with the concentration of 1-2mol/L, the pH value of the adjusting solution is 11.0-12.0, the copper acetate is a copper acetate aqueous solution with the concentration of 0.1-0.2mol/L, the ascorbic acid is an ascorbic acid aqueous solution with the concentration of 0.1mol/L, and the volume ratio of the sodium hydroxide aqueous solution to the copper acetate aqueous solution to the ascorbic acid aqueous solution is 3-5: 3-4: 6-8.
Preferably, the sodium hydroxide is added into a 1-2mol/L sodium hydroxide aqueous solution with the volume of 3-5 mL, the pH value of the solution is adjusted to be 11.0-12.0, the copper acetate is a 0.1-0.2mol/L copper acetate aqueous solution with the volume of 3-4mL, and the ascorbic acid is a 0.1-0.2mol/L ascorbic acid aqueous solution with the volume of 6-8 mL.
Wherein the stirring is magnetic stirring, and the stirring time is 30-40 min.
Wherein the heating temperature of the oil bath is 80-100 ℃.
Wherein, after adding sodium sulfide aqueous solution with the concentration of 0.1-0.2mol/L, the reaction time is 1.5-2 h, and the volume ratio of the sodium sulfide aqueous solution to the copper acetate aqueous solution is 1.5-2.5: 3-4.
Preferably, the reaction time after adding 1.5-2.5mL of 0.1-0.2mol/L sodium sulfide aqueous solution is 1.5-2 h.
Further, the concentration of the weighed copper acetate solution is 0.1mol/L, the concentration of the weighed sodium sulfide solution is 0.1mol/L, the two are equimolar, and the proportion is controlled by volume.
The hollow Cu of the invention7S4Use of a nanocube structure for the preparation of a photothermal therapeutic agent for the treatment of cancer.
Wherein the hollow Cu7S4The nano cubic structure loaded cancer treatment drug is used for photo-thermal-drug cooperative treatment, and can be applied to preparation of a cancer drug photo-thermal-drug cooperative treatment reagent or a drug.
Wherein, the Cu7S4The dispersion liquid of the photothermal material in preparing the photothermal reagent for treating tumor cells is deionized water, phosphoric acid buffer solution or cell culture solution. The photothermal reagent has good dispersibility in the dispersion liquid, and has no obvious precipitation phenomenon after being placed for one week.
Wherein, the Cu7S4The concentration of the photothermal material dispersed into the dispersion liquid is 50-200 mug/mL when the photothermal reagent for treating tumor cells is prepared.
Preferably, the prepared Cu with a hollow cubic structure7S4Preparation of photothermal materialWhen applied to a reagent for photothermal therapy of tumor cells, the concentration of the dispersion in the dispersion is 100. mu.g/mL.
Wherein, the Cu7S4Incubating the photothermal material and tumor cells MCF-7 at 37 deg.C for 12h, and irradiating with 980nm laser at 0.7W/cm at room temperature2Is irradiated for 10 min.
Cu of the invention7S4The photo-thermal material can promote the released photo-thermal effect to influence tumor cells and enable the cells to die under the irradiation of near-infrared laser.
When Cu of the present invention is mentioned7S4When the concentration of the photo-thermal material dispersion liquid is less than 200 mu g/mL, the cell survival rate is higher than 75% (without irradiation); when the concentration of the photo-thermal reagent dispersion liquid is 50-200 mug/mL, the photo-thermal property can be shown when the temperature can be increased from room temperature to 40-65 ℃ under the irradiation of near-infrared laser with the wavelength of 980nm for 5min, and photo-thermal conversion can be effectively carried out; the Cu is added7S4The photo-thermal material is dispersed in the cell culture solution, when the concentration is 50 mu g/mL-200 mu g/mL, the tumor inhibition rate is up to 86% after 980nm laser irradiation for 10 min.
The Cu with the hollow cubic structure7S4The photothermal material has good biocompatibility, and the photothermal material (0-100 mu g/mL dispersion liquid) and the tumor cell MCF-7 are incubated for 12 hours at 37 ℃, and the result shows that the activity of the cell can still reach more than 90%. Adding the Cu7S4Nano cubic structure (100. mu.g/mL dispersion) and MCF-7 cells (1X 10)6One) were incubated for 12h at room temperature with a 980nm laser at 0.7W/cm2After 10min of irradiation with power density, the cells were evaluated for apoptosis and the results indicated that 95% of MCF-7 cells died.
The photothermal-drug synergistic therapeutic composition comprises the Cu7S4Photothermal material and loaded with medicine such as antitumor drug doxorubicin DOX. The Cu with the hollow cubic structure prepared by the invention7S4The photothermal material has a unique hollow cubic structure, so that the specific surface area is large, and the photothermal conversion efficiency after irradiation is high. It has a large broad-peak absorption in the near infrared region, and thus can be used for preparing a fluorescent materialThe photo-thermal conversion efficiency is higher when 980nm laser is used for treatment.
The mechanism is as follows: the hollow Cu of the invention7S4The nano cubic structure has higher photo-thermal conversion efficiency, and the hollow Cu7S4The nano cubic structure has strong wide absorption in a near infrared region, can convert light energy into heat energy, has low cytotoxicity, and is a high-efficiency photothermal reagent for treating tumor cells. Also, the hollow Cu of the present invention7S4The nano cubic structure has large cavities, so that the nano cubic structure not only has larger surface area, but also can load tumor treatment medicines such as DOX and the like more efficiently, and can be effectively applied to the preparation of photo-thermal treatment reagents for treating cancers.
The preparation method is simple one-pot method, firstly, copper acetate reacts with PVP, AA and NaOH to generate Cu2O precursor, and oxidizing in air to obtain Cu as final product7S4. The method is characterized in that the feeding ratio is designed (the copper-sulfur ratio is close to 7: 4), and finally, the morphological structure is a special hollow cubic structure. The side length is about 70-80 nm, the shape is cubic, and the element distribution Cu: and S is 7: 4.
in addition, the pH value has great influence on the formation of the final appearance in the preparation process, and the pH value of the solution is adjusted to 11.0-12.0 by adding sodium hydroxide solution in the preparation process, so that a hollow cubic structure can be obtained, and only solid Cu can be obtained without adjusting the pH value7S4A nano-cubic structure.
In addition, the invention selects a 980nm laser irradiation material for photo-thermal treatment. The use of 980nm laser can produce higher absorption relative to 808nm laser, higher photo-thermal efficiency and deeper penetration depth into biological tissue compared to gold nano-material at the same laser power.
Has the advantages that: compared with the prior art, the invention has the following advantages:
1. cu prepared by the invention7S4The nano-cube has a unique hollow cube structure, so the specific surface area is large, and the photo-thermal conversion effect after irradiationThe rate is high and there are large cavities available for loading of DOX for photothermal-drug co-therapy. The nano-particle has great broad-peak absorption in a near-infrared region (900-1100 nm), so that 980nm laser can be used for treatment, and the photo-thermal conversion efficiency is higher.
2. Hollow Cu prepared by the invention7S4The nano cubic structure has low cytotoxicity and good biocompatibility, and is suitable for cell treatment.
3. Hollow Cu prepared by the invention7S4The preparation method of the hollow nano cubic structure is simple, mild in condition, environment-friendly, easy to popularize and produce in a large scale, high in photothermal conversion efficiency, good in stability and biocompatibility, good in condition for photothermal treatment of tumor cells, and capable of being applied to preparation of photothermal reagents for treating cancers.
Drawings
FIG. 1 is a schematic view of a hollow Cu of the present invention7S4Transmission electron microscopy images of nano-cubic structures;
FIG. 2 is a view showing a hollow Cu of the present invention7S4A spectrum of ultraviolet-visible absorption of the nano-cubic structure;
FIG. 3 is a view of the hollow Cu of the present invention7S4Transmission electron microscopy of the nanoshell structure;
FIG. 4 is a view showing a hollow Cu of the present invention7S4XRD pattern of nano-cubic structure;
FIG. 5 is a view showing a hollow Cu of the present invention7S4XPS plot of Cu in nano-cubic structure;
FIG. 6 is a hollow Cu of the present invention7S4XPS plot of S of the nano-cubic structure;
FIG. 7 is a view of the hollow Cu of the present invention7S4Nano cubic structure (100 mug/mL) at 0.7W/cm2A photo-thermal conversion effect diagram under 980nm laser irradiation under power density;
FIG. 8 shows Cu7S4In the range of 0 to 200. mu.g mL-1A map of cell activity of co-incubated MCF-7 cells at ranges;
FIG. 9 shows the photothermal treatment of MCF-7 cells before and afterActivity evaluation chart of (1); the photothermal agent used for the treatment is the Cu with the hollow cubic structure7S4The photo-thermal material (100 mu g/mL) has the excitation wavelength of 980nm and the power density of 0.7W/cm2The illumination time is 10 min.
Detailed Description
The present invention is further illustrated by the following examples.
The experimental methods described in the examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
Weighing 4g of polyvinylpyrrolidone (PVP) with the molecular weight of 10000 at the room temperature of 25 ℃, dissolving in 400mL of deionized water, stirring, magnetically stirring for 10min, adding 3.5mL of 0.1mol/L copper acetate solution, continuously stirring, adding 3.6mL of 1mol/L sodium hydroxide solution after 5min, adjusting the pH of the solution to be about 11.0, quickly adding 6mL of 0.1mol/L ascorbic acid solution after 30s, and continuously stirring for 30 min. Heating to 92 ℃ in an oil bath, adding 2mL of 0.1mol/L sodium sulfide solution under stirring for reaction for 2h, centrifuging the product for 15min after complete reaction, taking the lower layer precipitate for washing, repeating the steps for 3 times, and dispersing into deionized water (100 mu g/mL) to obtain the hollow Cu7S4The nano cubic structure has the side length of a cube of about 70-80 nm, as shown in figure 1. FIG. 2 shows the resulting hollow Cu7S4UV-Vis diagram of Nano-cubic Structure, as can be seen from FIG. 2, the hollow Cu7S4The nano cubic structure has a characteristic absorption broad peak at 900-1100 nm. As can be seen from the comparison of the XRD spectra of FIG. 4, the substance is exactly the same as Cu7S4Corresponding to the standard card JCPDS NO.23-0958, and has several distinct characteristic peaks such as 46.839, 31.204 and 34.061 degree. As can be seen from FIGS. 5 and 6, the substance has 4 and 2 XPS peaks (Cu) corresponding to Cu and S elements, respectively2+2p3/2:934.9eV，Cu2+2p1/2:934.9eV，Cu+2p3/2:934.9eV，Cu+2p3/2934.9eV) and (S2 p)3/2:934.9eV，S2p1/2:934.9eV)。
Example 2
Weighing 5g of polyvinylpyrrolidone (PVP) with the molecular weight of 10000 at the room temperature of 25 ℃, dissolving in 400mL of deionized water, stirring, magnetically stirring for 10min, adding 3.5mL0.1mol/L of copper acetate solution, continuously stirring, adding 4.5mL of 1mol/L of sodium hydroxide solution after 6min, adjusting the pH of the solution to be about 11.0, quickly adding 6mL0.1mol/L of ascorbic acid solution after 30s, and continuously stirring for 40 min. Heating to 95 ℃ in an oil bath, adding 2mL0.1mol/L sodium sulfide solution under stirring for reaction for 2h, centrifuging the product for 15min after complete reaction, taking the lower layer precipitate for washing, repeating the steps for 3 times, and dispersing into deionized water (100 mu g/mL) to obtain the hollow Cu7S4A nano-cubic structure.
Example 3
Weighing 5g of polyvinylpyrrolidone (PVP) with the molecular weight of 24000 at the room temperature of 25 ℃, dissolving in 400mL of deionized water, stirring, magnetically stirring for 10min, adding 3.5mL0.1mol/L of copper acetate solution, continuously stirring, adding 3.6mL of 1mol/L of sodium hydroxide solution after 5min, adjusting the pH of the solution to be about 11.0, quickly adding 6mL0.1mol/L of ascorbic acid solution after 30s, and continuously stirring for 40 min. Heating to 90 deg.C in oil bath, adding 2mL of 0.1mol/L sodium sulfide solution under stirring, reacting for 1.5h, centrifuging the product for 15min, washing the lower layer precipitate, repeating the above steps for 3 times, and dispersing in deionized water (100 μ g/mL) to obtain hollow Cu7S4A nano-cubic structure.
Example 4
Weighing 2.5g of polyvinylpyrrolidone (PVP) with the molecular weight of 24000 at the room temperature of 25 ℃, dissolving in 400mL of deionized water, stirring, magnetically stirring for 8min, adding 1.75mL of 0.1mol/L copper acetate solution, continuously stirring, adding 3mL of 1mol/L sodium hydroxide solution after 5min, adjusting the pH of the solution to be about 11.0, quickly adding 6mL of 0.1mol/L ascorbic acid solution after 30s, and continuously stirring for 30 min. Heating to 88 deg.C in oil bath, adding 1mL of 0.1mol/L sodium sulfide solution under stirring, reacting for 1.5h, centrifuging the product for 15min, washing the lower layer precipitate, repeating the above steps for 3 times, and dispersing in deionized water (100 μ g/mL) to obtain hollow Cu7S4A nano-cubic structure.
Comparative example 1
Weighing 4g of polyvinylpyrrolidone (PVP) with the molecular weight of 10000 at the room temperature of 25 ℃, dissolving in 400mL of deionized water, stirring, magnetically stirring for 10min, adding 3.5mL0.1mol/L of copper acetate solution, continuously stirring, adding 3.6mL of 1mol/L of sodium hydroxide solution after 5min, adding 6mL0.1mol/L of ascorbic acid solution after 30s, and standing for 30 min. Heating to 92 ℃ in an oil bath, adding 2mL0.1mol/L sodium sulfide solution under stirring for reaction for 2h, centrifuging the product for 15min after complete reaction, taking the lower layer precipitate for washing, repeating the steps for 3 times, and dispersing in deionized water to obtain hollow Cu7S4Nanosphere structure (100. mu.g/mL), indicating that this comparative example does not yield hollow Cu7S4Nano cubic structure, only hollow Cu can be obtained7S4The nano spherical shell structure has a significantly smaller specific surface area under the same size, as shown in fig. 3.
Comparative example 2
Weighing 4g of polyvinylpyrrolidone (PVP) with the molecular weight of 10000 at the room temperature of 25 ℃, dissolving in 400mL of deionized water, stirring, magnetically stirring for 10min, adding 3.5mL0.1mol/L of copper acetate solution, continuously stirring, after 5min, adding 6mL0.1mol/L of ascorbic acid solution after 30s, and stirring for 30min without adding sodium hydroxide solution, wherein the pH value is 5.8. Heating to 92 ℃ in an oil bath, adding 2mL0.1mol/L sodium sulfide solution under stirring for reaction for 2h, centrifuging the product for 15min after the reaction is completed, taking the lower layer precipitate for washing, repeating the steps for 3 times, and dispersing into deionized water (100 mu g/mL) to obtain solid Cu7S4Nano-cubic structure, indicating that this comparative example does not yield hollow Cu7S4Nano cubic structure, only solid Cu can be obtained7S4The nano cubic structure is adopted, the solid structure is small in specific surface area, and a cavity-free structure is used for loading drugs or has extremely low drug loading rate.
Comparative example 3
Weighing 4g of polyvinylpyrrolidone (PVP) with the molecular weight of 10000 at the room temperature of 25 ℃, dissolving in 400mL of deionized water, stirring, magnetically stirring for 10min, adding 0.5mL0.1mol/L of copper acetate solution, continuously stirring, adding 3.6mL of 1mol/L of sodium hydroxide solution after 5min, adding 6mL0.1mol/L of ascorbic acid solution after 30s of reaction, and stirring for 30 min. And heating the mixture to 92 ℃ in an oil bath, adding 2mL of 0.1mol/L sodium sulfide solution under a stirring state, reacting for 2h, centrifuging the product for 15min after the reaction is completed, taking the lower layer precipitate, washing, repeating the step for 3 times, and dispersing into deionized water (100 mu g/mL), wherein the nano particles (with the size of about 10-20 nm) are obtained in the comparative example, the maximum absorption wavelength of the nano particles is less than 900nm, and the photo-thermal conversion can not be better carried out by using 980nm laser.
Test example 1
The hollow Cu obtained in example 1 was mixed at room temperature at 25 deg.C7S4Aqueous dispersions of nanocube structures (100. mu.g/mL) were prepared at room temperature with a 980nm laser at 0.7W/cm2After the power density is irradiated for 15min, the light source is closed, the light source is naturally cooled to the room temperature, and the temperature change from continuous laser irradiation for 15min to natural cooling is recorded, which shows that the hollow Cu is prepared by the invention7S4The photo-thermal effect of the nano cubic structure is good. (shown in FIG. 7), the description will be given of the hollow Cu7S4The nano cubic structure can effectively convert light energy into heat energy, and has potential application value in tumor cell photothermal therapy.
Test example 2
The hollow cubic structured Cu obtained in example 1 was mixed at room temperature of 25 deg.C7S4Dispersion of photothermal material and tumor cell MCF-7 (-1X 10)6Respectively) incubating at 37 ℃ for 12h (the concentration of the material in the culture solution is 0-200 mu g/mL), and testing when Cu is contained7S4In the range of 0 to 200. mu.g mL-1Within the range, the cell activity of the co-incubated MCF-7 cells is shown in FIG. 8, which indicates that the cell activity can still be as high as 80% or more.
Test example 3
The hollow cubic structured Cu obtained in example 1 was mixed at room temperature of 25 deg.C7S4Dispersion of photothermal material and MCF-7 cells (1X 10)6One) was incubated at 37 ℃ for 12 hours (concentration of material in culture medium 100. mu.g/mL) at room temperature with a 980nm laser at 0.7W/cm2After the power density of the light is irradiated for 10min, the apoptosis condition of the cells is evaluated. FIG. 9 shows MCF-7 activity evaluation graphs before and after cell photothermal treatment, lines a and b are cell activity statistics conditions after 10min of non-illumination (a) and illumination (b), respectively, the results show that after 10min of illumination, the apoptosis rate reaches 95%, and the non-illumination has no effect, which shows that the Cu with the hollow cubic structure7S4The photothermal material has a remarkable ability of killing tumor cells.
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