CN116440289A - PVP modified FeTA nano particle and preparation method and application thereof - Google Patents

PVP modified FeTA nano particle and preparation method and application thereof Download PDF

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CN116440289A
CN116440289A CN202310216933.3A CN202310216933A CN116440289A CN 116440289 A CN116440289 A CN 116440289A CN 202310216933 A CN202310216933 A CN 202310216933A CN 116440289 A CN116440289 A CN 116440289A
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tannic acid
feta
iron
pvp
solution
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李翔
万士齐
傅译可
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Zhejiang University ZJU
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Abstract

The invention discloses PVP modified FeTA nano particles, a preparation method and application thereof, wherein the preparation method of the FeTA nano particles comprises the following steps: adding polyvinylpyrrolidone into deionized water, and fully stirring and dissolving to obtain 0.075-0.75wt% polyvinylpyrrolidone solution; adding an aqueous solution of ferric chloride into the polyvinylpyrrolidone solution to obtain a mixed solution; adding tannic acid water solution into the mixed solution, and dialyzing to obtain tannin after the reaction is completedAn aqueous solution of iron acid nanoparticles; wherein the polyvinylpyrrolidone: tannic acid: the mass ratio of the ferric chloride is (4.4-44): 5:10. the FeTA nano-particles in the invention have simple synthesis method and uniform size. TA reduces Fe in acidic tumor microenvironment 3+ Generates Fe 2+ Greatly improves the catalysis H 2 O 2 Efficiency of hydroxyl radical production (. OH) while Fe 2+ Will be again H 2 O 2 Oxidation to Fe 3+ Local iron circulation is formed, and efficient in-situ chemical power treatment of tumors is realized.

Description

PVP modified FeTA nano particle and preparation method and application thereof
Technical Field
The invention belongs to the technical fields of biological nano materials and nano medicine, and particularly relates to PVP modified FeTA nano particles, and a preparation method and application thereof.
Background
In recent years, the incidence and mortality of cancer have been rising year by year and have been rising, and cancer has become one of the diseases that pose the greatest threat to human health. The incidence rate of domestic cancers is increased by 3.9% each year, the death rate of the cancers is increased by 2.5% each year, and the method brings great burden to the development of the economic society of China while bringing difficulty and harm to patients and families. Common tumor treatment means are surgical excision, chemotherapy (chemotherapy), radiotherapy (radiotherapy) and the like, but the surgical excision is large in wound and slow in recovery, and the radiotherapy and the chemotherapy are easy to produce larger toxic and side effects on normal cells. Therefore, diagnosis and treatment of cancer have been a hot spot of research in the fields of nano-medical technology and biological nano-materials.
One of the important components of nano-medical technology is the use of nanoparticles as drug carriers. Nanoparticles are widely used in research of some cancer treatment means, such as photodynamic therapy (PDT), photothermal therapy (PTT), sonodynamic therapy (SDT), hunger therapy, and chemodynamic therapy (CDT), etc., due to their low toxicity, easy metabolism, targeting, and controllable release. Currently, most nanoparticles used in chemodynamic therapy are iron-based Fenton reagent, and ferrous ions can catalyze H under acidic conditions 2 O 2 The disadvantages of the iron-based Fenton reagent are that it generates highly toxic hydroxyl radicals (.OH): ferric iron has low catalytic activity and ferrous ion is unstable. Therefore, it is important to study new iron-based nanoparticles for use in chemo-kinetic therapy that are stable and have high catalytic activity.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art, and provides PVP modified FeTA nano particles, a preparation method and application thereof, so as to solve the technical problem that the iron-based Fenton reactant in the related art is difficult to have high catalytic activity and stability.
The aim of the invention is realized by the following technical scheme: a method for preparing PVP-modified FeTA nanoparticles, comprising the steps of:
adding polyvinylpyrrolidone into deionized water, and fully stirring and dissolving to obtain polyvinylpyrrolidone solution with the concentration of 1-10 mg/mL;
adding ferric chloride into the polyvinylpyrrolidone solution to obtain a mixed solution;
adding tannic acid into the mixed solution, and dialyzing to obtain PVP modified iron tannic acid nanoparticle aqueous solution after the tannic acid is reacted completely; centrifuging the PVP modified iron tannic acid nanoparticle aqueous solution to obtain PVP modified iron tannic acid nanoparticles;
wherein the polyvinylpyrrolidone: tannic acid: the mass ratio of the ferric chloride is (4.4-44): 5:10.
further, the solute mass volume concentration of the polyvinylpyrrolidone solution is 7.5mg/mL.
Further, the dialysis is specifically: dialyzing for 12-36 hours, and changing clear water every 4 hours.
Further, the iron tannic acid nanoparticles have an average particle diameter of 70nm.
Further, the iron tannic acid nanoparticles have an average hydrated particle diameter of 220 nm.
The iron tannic acid nano particles prepared according to the preparation method are prepared.
The use of the above iron tannic acid nanoparticle as a pH-responsive Fenton reagent.
The application of the iron tannic acid nano-particle is that the iron tannic acid nano-particle is used as a multifunctional anticancer nano-particle.
The beneficial effects of the invention are as follows: using Fe 3+ The ion is used as metal ion, tannic acid is used as organic ligand to coordinate, PVP is used as surfactant, and a stable FeTA nano particle is synthesized. Overcomes the defect that FeTA particles are prepared by the conventional methodThe problems of oversized size, unstable complexation and the like occur.
Due to Fe 3+ The ions have reversible redox properties, and tannic acid can reduce Fe in acidic environment 3+ Ion to obtain Fe 2+ Ion, fe 2+ The ions are again covered by H 2 O 2 Oxidation to Fe 3+ Ions. Thus forming a redox reaction cycle of Fe in the in situ chemo-dynamic treatment of tumors. Fe (Fe) 2+ Ions can catalyze H efficiently 2 O 2 Generates toxic hydroxyl radicals (OH). Thus, in the present invention, tannic acid and Fe in an acidic environment are utilized 3+ Overcomes the existence of iron-based Fenton reactants: fe (Fe) 2 + Ion instability, fe 3+ Low catalytic activity. Has very excellent tumor killing effect.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort to a person skilled in the art.
FIG. 1 is a schematic illustration of FeTA nanoparticle synthesis procedure in example 1;
FIG. 2 is a scanning electron micrograph of FeTA nanoparticles of example 1;
FIG. 3 is a transmission electron micrograph of FeTA nanoparticles of example 1;
FIG. 4 is a particle size distribution diagram of FeTA nanoparticles in example 1;
FIG. 5 is an ESR spectrum of FeTA nanoparticles of example 1 after Fenton reaction at different pH conditions;
FIG. 6 is a graph of the ultraviolet visible spectrum of the TMB color reaction of FeTA particles in example 1;
FIG. 7 is a graph showing the absorbance versus time at 652nm of TMB color development reactions for FeTA particles at different pH conditions in example 1;
FIG. 8 is a real viewFeTA particles at different H in example 1 2 O 2 Graph of absorbance versus time for TMB color reaction at 652nm at concentration conditions;
FIG. 9 shows FeTA particles at different H in example 1 2 O 2 A graph is fitted by a Mie equation of TMB color reaction under the concentration condition;
FIG. 10 shows FeTA particles at different H in example 1 2 O 2 A graph of the double reciprocal plot of the TMB color reaction at concentration conditions.
Detailed Description
Reference will now be made in detail to exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, the same numbers in different drawings refer to the same or similar elements, unless otherwise indicated. The implementations described in the following exemplary examples do not represent all implementations consistent with the invention. Rather, they are merely examples of apparatus and methods consistent with aspects of the invention as detailed in the accompanying claims.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any or all possible combinations of one or more of the associated listed items.
It should be understood that although the terms first, second, third, etc. may be used herein to describe various information, these information should not be limited by these terms. These terms are only used to distinguish one type of information from another. For example, first information may also be referred to as second information, and similarly, second information may also be referred to as first information, without departing from the scope of the invention. The word "if" as used herein may be interpreted as "at … …" or "at … …" or "responsive to a determination", depending on the context.
The present invention will be described in detail with reference to the accompanying drawings. The features of the examples and embodiments described below may be combined with each other without conflict.
Chemical: ferric (iii) trichloride hexahydrate (FeCl) 3 ·6H 2 O), tannic acid (TA, C) 76 H 52 O 46 ) Polyvinylpyrrolidone (PVP) was purchased from alaa Ding Shiji (Shanghai) limited. All drugs used, unless specified, did not require additional purification.
Example 1:
as shown in fig. 1, the preparation of iron tannic acid (FeTA) nanoparticles comprises the following steps:
66mg of PVP was dissolved in 8.8mL of deionized water at room temperature and stirred for 1 hour to give an aqueous PVP solution. Then, an aqueous solution of ferric chloride (0.2 mL,100 mg/mL) was added to the PVP aqueous solution, and the mixture was stirred for 1 hour. An aqueous tannic acid solution (1 mL,10 mg/mL) was added to the above mixed solution, and stirred for 12 hours. Finally, dialyzing with pure water for 12-36 hours, and changing water every 4 hours to obtain PVP modified FeTA nano particle aqueous solution; and centrifuging the PVP modified iron tannic acid nanoparticle aqueous solution to obtain PVP modified iron tannic acid nanoparticle.
Characterization of materials:
the microstructure and morphology of the FeTA nanoparticles were observed by field emission scanning electron microscopy (FESEM, apreo 2S,Thermo Scientific,USA) and transmission electron microscopy (TEM, talos F200X, thermo Scientific). The diameter size distribution of the FeTA nanoparticles was measured and analyzed using a nanoparticle size potentiometer measurement (Zetasizer nano ZS, malvern).
Structural analysis:
according to fig. 2 and 3, the prepared FeTA nanoparticles have a uniform size distribution, and a particle diameter of about 70nm. The hydrodynamic diameter of the FeTA nanoparticles prepared according to DLS measurement was about 220nm, as shown in FIG. 4.
The FeTA nanoparticle of the invention can be used as a pH responsive Fenton reagent and as a multifunctional anticancer nanoparticle.
Fenton performance characterization:
the ability of FeTA particles to catalyze the production of OH was investigated using Electron Spin Resonance (ESR) spectroscopy. The OH was captured using 5, 5-dimethyl-1-pyrroline-N-oxide (DMPO). The results are shown in FIG. 5, in the presence of H 2 O 2 The formation of OH was observed in the (1 mM) mixed solution, which was manifested by the appearance of feature 1 in the ESR spectrum: 2:2:1, the signal exhibiting an increasing trend as the pH decreases.
The Fenton performance of the material was indirectly characterized using the 3,3', 5' -Tetramethylbenzidine (TMB) chromogenic method, and all ultraviolet-visible absorption spectra (UV-vis) were measured using an ultraviolet-visible spectrophotometer (UV-2600, shimadzu, japan). As shown in fig. 6, feTA nanoparticles and H 2 O 2 After mixing, the TMB solution was allowed to have a distinct absorption peak at 652 nm. The absorbance profile of the mixed solution at 652nm was then examined over time at different pH conditions, and it was found that the material had substantially no fenton performance at neutral conditions (ph=7.4) and significantly enhanced fenton performance at acidic conditions (ph=6.5, ph=4.7), as shown in fig. 7. When the reaction substrate H 2 O 2 Measuring the absorbance time-dependent curve of the mixed solution at 652nm when the concentrations are different, as shown in fig. 8; and according to the data, performing double reciprocal mapping and Michaelis equation fitting, and calculating to obtain Michaelis constant K m And the reaction rate V at which the enzyme is saturated with the substrate max The two methods fit the calculated K m And V max 53.49mM and 2.16X10, respectively - 8 M·s -1 55.19mM and 2.19X10) -8 M·s -1 The material was shown to have strong Fenton performance as shown in FIGS. 9 and 10.
Conclusion:
based on the strategy of improving the existing iron-based Fenton reagent, PVP modified FeTA nano particles are designed and prepared, and the PVP modified FeTA nano particles are uniform in size and have the performance of strongly catalyzing Fenton reaction; the nanoparticle material can realize in-situ chemical power treatment of tumor, and solve Fe common to iron-based Fenton reactant 2+ Ion instability, fe 3+ Low catalytic activity. The FeTA nanoparticle material in the invention has simple synthesis method and can be used for preparing acidic tumor microringsIn the environment, can catalyze H 2 O 2 Generates a large amount of hydroxyl free radicals (OH), realizes the high-efficiency targeted killing of tumors, and has broad spectrum of application.
Example 2:
preparation of iron tannic acid (FeTA) nanoparticles:
88mg of PVP was dissolved in 8.8mL of deionized water at room temperature and stirred for 1 hour. Then, an aqueous solution of ferric chloride (0.2 mL,100 mg/mL) was added to the PVP aqueous solution, and the mixture was stirred for 1 hour. An aqueous tannic acid solution (1 mL,10 mg/mL) was added to the above mixed solution, and stirred for 12 hours. Finally, dialyzing with pure water for 24 hours, and changing water every 4 hours to obtain PVP modified FeTA nano particle aqueous solution; and centrifuging the PVP modified iron tannic acid nanoparticle aqueous solution to obtain PVP modified iron tannic acid nanoparticle.
The FeTA nanoparticles also exhibit catalytic H in weak acid environments 2 O 2 The ability to catalyze Fenton's reaction to generate large amounts of hydroxyl radicals (& OH); can be used as a multifunctional anticancer nano particle.
Example 3:
preparation of iron tannic acid (FeTA) nanoparticles:
8.8mg PVP was dissolved in 8.8mL deionized water at room temperature and stirred for 1 hour. Then, an aqueous solution of ferric chloride (0.2 mL,100 mg/mL) was added to the PVP aqueous solution, and the mixture was stirred for 1 hour. An aqueous tannic acid solution (1 mL,10 mg/mL) was added to the above mixed solution, and stirred for 12 hours. Finally, dialyzing with pure water for 24 hours, and changing water every 4 hours to obtain PVP modified FeTA nano particle aqueous solution.
The FeTA nanoparticles also exhibit catalytic H in weak acid environments 2 O 2 The ability to catalyze Fenton's reaction to generate large amounts of hydroxyl radicals (& OH); can be used as a multifunctional anticancer nano particle.
Example 4:
preparation of iron tannic acid (FeTA) nanoparticles:
44mg of PVP was dissolved in 8.8mL of deionized water at room temperature and stirred for 1 hour. Then, an aqueous solution of ferric chloride (0.2 mL,100 mg/mL) was added to the PVP aqueous solution, and the mixture was stirred for 1 hour. An aqueous tannic acid solution (1 mL,10 mg/mL) was added to the above mixed solution, and stirred for 12 hours. Finally, dialyzing with pure water for 24 hours, and changing water every 4 hours to obtain PVP modified FeTA nano particle aqueous solution; and centrifuging the PVP modified iron tannic acid nanoparticle aqueous solution to obtain PVP modified iron tannic acid nanoparticle.
The FeTA nanoparticles also exhibit catalytic H in weak acid environments 2 O 2 The ability to catalyze Fenton's reaction to generate large amounts of hydroxyl radicals (& OH); can be used as a multifunctional anticancer nano particle.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather to enable any modification, equivalent replacement, improvement or the like to be made within the spirit and principles of the invention.
The above embodiments are merely for illustrating the design concept and features of the present invention, and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, the scope of the present invention is not limited to the above embodiments. Therefore, all equivalent changes or modifications according to the principles and design ideas of the present invention are within the scope of the present invention.
Other embodiments of the present application will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure herein. This application is intended to cover any variations, uses, or adaptations of the application following, in general, the principles of the application and including such departures from the present disclosure as come within known or customary practice within the art to which the application pertains. The specification and examples are to be regarded in an illustrative manner only.
It is to be understood that the present application is not limited to the precise arrangements and instrumentalities shown in the drawings, which have been described above, and that various modifications and changes may be effected without departing from the scope thereof.

Claims (8)

1. The preparation method of PVP modified FeTA nano particles is characterized by comprising the following steps:
adding polyvinylpyrrolidone into deionized water, and fully stirring and dissolving to obtain polyvinylpyrrolidone solution with the concentration of 1-10 mg/mL;
adding ferric chloride into the polyvinylpyrrolidone solution to obtain a mixed solution;
adding tannic acid into the mixed solution, and dialyzing to obtain PVP modified iron tannic acid nanoparticle aqueous solution after the tannic acid is reacted completely; centrifuging the PVP modified iron tannic acid nanoparticle aqueous solution to obtain PVP modified iron tannic acid nanoparticles;
wherein the polyvinylpyrrolidone: tannic acid: the mass ratio of the ferric chloride is (4.4-44): 5:10.
2. the method for preparing PVP modified FeTA nanoparticles according to claim 1, wherein the solute mass volume concentration of the polyvinylpyrrolidone solution is 7.5mg/mL.
3. The method for preparing PVP-modified FeTA nanoparticles according to claim 1, wherein the dialysis is specifically: dialyzing for 12-36 hours, and changing clear water every 4 hours.
4. The method for preparing PVP modified FeTA nanoparticles according to claim 1, wherein the average particle size of the iron tannic acid nanoparticles is 70nm.
5. The method of preparing PVP-modified FeTA nanoparticles according to claim 1, wherein the iron tannic acid nanoparticles have an average hydrated particle size of 220 nm.
6. Iron tannic acid nanoparticles prepared by the preparation method according to any one of claims 1 to 5.
7. Use of iron tannic acid nanoparticles according to claim 6 as a pH-responsive Fenton reagent.
8. Use of iron tannic acid nanoparticles according to claim 7 as a multifunctional anticancer nanoparticle.
CN202310216933.3A 2023-03-08 2023-03-08 PVP modified FeTA nano particle and preparation method and application thereof Pending CN116440289A (en)

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