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CN-122005852-A - Lian Sheng porous photocatalytic anticancer and antibacterial micro-nano material and preparation method thereof

CN122005852ACN 122005852 ACN122005852 ACN 122005852ACN-122005852-A

Abstract

The invention discloses a lotus seed porous photocatalytic anticancer and antibacterial micro-nano material and a preparation method thereof, and also relates to application of the lotus seed porous photocatalytic anticancer and antibacterial micro-nano material in synergistic antibacterial and tumor photocatalytic treatment under near infrared light driving. The preparation method comprises the steps of firstly, carrying out pretreatment operation of grinding, washing and suction filtration on Lotus pollen, secondly, reacting the pretreated Lotus pollen with titanium chloride solution, centrifugally washing and calcining to obtain a TiO 2 @Lotus micro-nano material, thirdly, preparing a dispersion liquid by using the TiO 2 @lotus micro-nano material, coating the dispersion liquid on a hydrophobic silicon wafer, carrying out platinum sputtering, stripping, washing and drying to obtain a Pt/TiO 2 @lotus micro-nano material, and fourthly, dispersing the Pt/TiO 2 @lotus micro-nano material in an doxorubicin water solution, and carrying out light-shielding adsorption and centrifugal washing to remove free doxorubicin to obtain the Lotus seed porous photocatalytic material. According to the invention, the Schottky heterojunction structure is constructed by the method, the prepared material can realize efficient generation of active oxygen and active depletion of intracellular glutathione under the irradiation of near infrared light, and meanwhile, the material has the pH/near infrared dual-response drug release characteristic, so that the synergistic effect of photodynamic, photothermal and chemotherapy is realized. The method has good biocompatibility, and provides a novel and efficient material for antibacterial and tumor photocatalytic treatment.

Inventors

  • SUN TIEDONG
  • FENG YANZHENG
  • CHEN CHUNXIA

Assignees

  • 东北林业大学

Dates

Publication Date
20260512
Application Date
20260303

Claims (10)

  1. 1. The preparation method of the lotus seed porous photocatalytic material is characterized by taking lotus flower pollen as a unique matrix, and comprises the following preparation steps: Step one, pretreatment of lotus pollen Grinding lotus pollen into fine powder, washing with absolute ethanol, ultrasonic cleaning with ultrapure water, washing with acetone, and vacuum filtering to obtain pretreated lotus pollen; Step two, synthesizing a TiO 2 @Lotus micro-nano material Dispersing pretreated Lotus pollen in absolute ethyl alcohol, dropwise adding TiCl 3 solution, stirring in a dark place for reaction, centrifugally washing, and calcining in the atmosphere of air in a muffle furnace to obtain a Ti 2 @Lotus micro-nano material; Step three, synthesis of Pt/TiO 2 @Lotus micro-nano material Dispersing the TiO 2 @Lotus micro-nano material in absolute ethyl alcohol to prepare a dispersion liquid, uniformly coating the dispersion liquid on a hydrophobic silicon wafer, carrying out Pt sputtering by an ion sputtering instrument, then stripping the sputtered micro-nano material from the silicon wafer, centrifugally washing and drying to obtain the Pt/TiO 2 @lotus micro-nano material; preparation of lotus seed porous photocatalytic material Dispersing the Pt/TiO 2 @Lotus micro-nano material into an aqueous solution of doxorubicin, stirring in a dark place to realize electrostatic adsorption of the doxorubicin, and centrifugally washing to remove unadsorbed free doxorubicin to obtain the Lotus seed porous photocatalytic material (Pt/TiO 2 -D@lotus).
  2. 2. The method for preparing the lotus seed porous photocatalytic material according to claim 1, wherein in the first step, the washing with absolute ethanol is a step of centrifuging 8000 r seed after vortexing 5min min -1 for 10 min and repeating 3 times, the ultrasonic ultra-pure water washing time is 15 min, and the washing with acetone and the suction filtration process are repeated 3 times.
  3. 3. The method for preparing the porous photocatalytic material for lotus seed according to claim 1, wherein in the second step, the drop volume of the TiCl 3 solution is 20mL, the reaction time of stirring in the dark is 15 h, the temperature rising rate of calcination is 10 ℃ and min -1 , the calcination temperature is 300 ℃, and the calcination time is 6 h.
  4. 4. The preparation method of the Lotus seed porous photocatalytic material according to claim 1, wherein in the third step, the dispersion liquid of the TiO 2 @Lotus micro-nano material is prepared by ultrasonic treatment of 10 min, the silicon wafer is subjected to hydrophobic pretreatment, the silicon wafer is placed at an angle of 9 degrees after the dispersion liquid is coated and is naturally evaporated to ethanol, the Pt sputtering is performed under an argon atmosphere, the sputtering time is 1 min, the peeling process is ultrasonic treatment of 10 min, and the drying condition is 60 ℃ and the vacuum drying is carried out overnight.
  5. 5. The preparation method of the Lotus seed porous photocatalytic material according to claim 1, wherein in the fourth step, the concentration of the doxorubicin aqueous solution is 1 mg percent, the feed liquid ratio of the -1 ,Pt/TiO 2 @lotus seed micro-nano material to the doxorubicin aqueous solution is 10 mg:5 mL, the temperature of the light-shielding stirring is room temperature, the time is 48 h, and the centrifugal washing adopts phosphate buffer solution with pH of 7.4 until the supernatant is colorless.
  6. 6. The Lotus seed porous photocatalytic material prepared by the preparation method according to any one of claims 1-5, wherein Lotus flower pollen is used as a unique matrix, tiO 2 nano particles are uniformly anchored on the surface and an inner pore canal of the Lotus flower pollen, a Pt layer is uniformly deposited on the surface of TiO 2 to form a Pt-TiO 2 Janus Schottky heterojunction, doxorubicin is loaded on the surface of a Pt/TiO 2 @lotus micro-nano material through electrostatic adsorption, the specific surface area of the material is 128 m 2 ・g -1 , the pore diameter is about 4.2 nm, and the photo-thermal conversion efficiency is 55.4%.
  7. 7. The application of the Lotus seed porous photocatalytic material according to claim 6, wherein the Pt/TiO 2 @ Lotus seed porous photocatalytic material or the Lotus seed porous photocatalytic material (Pt/TiO 2 -d@lotus) is dispersed in a buffer solution to prepare a treatment solution, and after the treatment solution is acted on bacteria, 808 nm near infrared light is used for irradiation, wherein the power density of the near infrared light is 1.5W cm < -2 >, the irradiation time is 5min, and the bacteria comprise staphylococcus aureus which is gram positive bacteria and escherichia coli which is gram negative bacteria.
  8. 8. The use of the porous photocatalytic material for the treatment of tumor according to claim 6, wherein the porous photocatalytic material for the treatment of tumor is applied to the tumor site by intratumoral injection (Pt/TiO 2 -d@lotus) at a concentration of 300 μg/mL -1 and an injection volume of 200 μl, followed by irradiation with 808 nm near infrared light having a power density of 1.5W cm -2 and an irradiation time of 5 min, and the tumor is S180 sarcoma.
  9. 9. The use according to claim 7 or 8, wherein the material is capable of efficiently generating active oxygen such as O 2 ⁻、・OH、¹O 2 under near infrared light irradiation and achieving dose dependent glutathione depletion of up to 70% at 500 μg of the seed mL -1 .
  10. 10. The use according to claim 8, wherein the material has a pH/near infrared dual response doxorubicin release profile, and the doxorubicin release rate of 75 h under near infrared light irradiation at pH 5.0+808 nm is up to 90%.

Description

Lian Sheng porous photocatalytic anticancer and antibacterial micro-nano material and preparation method thereof Technical Field The invention belongs to the technical field of biomedical materials and photocatalysis treatment, in particular relates to a lotus seed porous photocatalysis material, a preparation method of the material and application of the material in synergistic antibacterial and tumor photocatalysis treatment under near infrared light driving, and the material takes lotus pollen as a sole matrix raw material. Background Bacterial infections and neoplasms are serious diseases that seriously threaten human health, and existing therapeutic strategies for both have a number of prominent drawbacks, leading to limited therapeutic efficacy. The single mode treatment is difficult to thoroughly eradicate refractory bacteria or tumor cells, the chemotherapy has the problem of poor targeting, serious off-target toxicity is easy to cause, nonresponsive drug release cannot be matched with pathological microenvironment, the treatment accuracy is reduced, the photodynamic therapy (PDT) is insufficient in generation of Reactive Oxygen Species (ROS) due to rapid recombination of electrons and hole pairs in a photosensitizer, and meanwhile, intracellular ROS can be further cleared by pathogenic bacteria and over-expressed Glutathione (GSH) in tumor cells, so that the treatment effect is obviously weakened. In order to solve the problems, researchers try to adopt natural biomass derived nano carriers as a treatment platform, the natural biomass derived nano carriers have inherent biocompatibility, biodegradability and a porous structure, and can solve the problem of biocompatibility of the synthetic nano carriers, wherein lotus pollen becomes a core potential template due to the natural spherical porous structure and large specific surface area, and high-efficiency drug adsorption and mass transfer can be realized. However, the existing biomass-based platforms still lack an integrated solution, most of the existing biomass-based platforms fail to realize GSH depletion while promoting ROS production, heterojunction-mediated PDT, photothermal conversion and stimulus-responsive chemotherapy are rarely integrated into a single system, and meanwhile, the technology for constructing Schottky heterojunction on lotus pollen matrixes to promote charge separation is not fully developed, so that the synergistic potential of multi-mode treatment is limited. Therefore, a lotus seed porous photocatalytic material which takes lotus flower powder as a unique matrix, constructs a heterojunction structure with high-efficiency charge separation, simultaneously realizes high-efficiency generation of ROS, GSH exhaustion and stimulus response type drug release is developed, and realizes synergistic photodynamic, photothermal and chemotherapy under the drive of near infrared light, so that the lotus seed porous photocatalytic material has high-efficiency antibacterial effect and good biocompatibility, and becomes a technical problem to be solved urgently in the field. Disclosure of Invention The invention aims to overcome the defects of the prior art, and provides a Lotus seed porous photocatalytic material, a preparation method and an antibacterial anticancer application thereof, wherein Lotus flower pollen is used as a sole matrix, pt/TiO 2 @Lotus Janus Schottky heterojunction is constructed, doxorubicin (DOX) is loaded, ROS can be efficiently generated under near infrared light irradiation, intracellular GSH is actively exhausted, pH/near infrared dual-response medicine release characteristics are achieved, the synergistic effect of photodynamic therapy (PDT), photothermal therapy (PTT) and chemotherapy is achieved, the problems of insufficient ROS generation, GSH mediated ROS removal, poor targeting property, medicine nonresponsive release and the like in the traditional antibacterial and tumor treatment are solved, the material has excellent biocompatibility, the preparation process is simple, and high-efficiency in-vitro and in-vivo antibacterial and tumor treatment can be realized. In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: A method for preparing a lotus seed porous photocatalytic material, which comprises the following steps: Step one, pretreatment of lotus pollen Grinding lotus pollen into fine powder, washing with absolute ethanol, ultrasonic cleaning with ultrapure water, washing with acetone, and vacuum filtering to obtain pretreated lotus pollen. Step two, synthesizing a TiO 2 @Lotus micro-nano material Dispersing pretreated Lotus pollen in absolute ethyl alcohol, dropwise adding TiCl 3 solution, stirring in a dark place for reaction, centrifugally washing, and calcining in the atmosphere of air in a muffle furnace to obtain the Ti 2 @Lotus micro-nano material. Step three, synthesis of Pt/TiO 2 @Lotus micro-nano material Dispersing the TiO 2 @Lotus micro-nano ma