CN112472806B - Sph-Ru-MMT @ PZ nano antibacterial agent and preparation method and application thereof - Google Patents
Sph-Ru-MMT @ PZ nano antibacterial agent and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to an Sph-Ru-MMT @ PZ nano antibacterial agent, wherein Sph-Ru-MMT @ PZ nano particles are obtained by sequentially loading montmorillonite MMT and a photosensitizer zinc phthalocyanine PZ onto nano ruthenium complex particles Sph-Ru, and the diameter of the nano particles Sph-Ru-MMT @ PZ is 85-155 nm; the invention also provides an application of the Sph-Ru-MMT @ PZ nano antibacterial agent in the field of escherichia coli resistance. The MMT is loaded on the Sph-Ru nano-particles and then anchored on the outer surface of an escherichia coli membrane, the membrane anchoring functional photosensitizer zinc phthalocyanine photosensitizer PZ is irradiated by 670nm near infrared NIR light, the structure of bacteria can be damaged by generating reactive oxygen ROS, so that escherichia coli is cracked, and the Sph-Ru-MMT @ PZ nano antibacterial agent has the capability of targeting cell membranes and effectively improves antibacterial activity.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a Sph-Ru-MMT @ PZ nano antibacterial agent, and a preparation method and application thereof.
Background
Bacterial diseases are threatening to the health and life of millions of patients each year, and antibiotics to treat infectious pathogen diseases are currently the most common methods. Traditional antibiotics selectively inhibit or kill microbial cells by preventing cellular processes such as cell replication, repair, protein synthesis, and cell wall renewal. Pathogenic bacteria have developed resistance to almost all types of traditional antibiotics through mutation or acquisition of resistance genes from other organisms for many years. However, due to the lack of intuitive results, the therapeutic effect of antibiotics cannot be fed back in time, which easily leads to overdosing of the drug.
Photodynamic antibacterial therapy is an effective alternative to traditional antibiotics. Under the irradiation of proper wavelength, the excited photosensitizer is in triplet state and reacts with ground molecular oxygen to generate excited singlet oxygen, so that the biological organic molecule can be oxidized. The photodynamic antibacterial therapy is not easy to cause drug resistance, but lacks targeting. How to transport the photosensitizer to the bacterial cell membrane in a short distance and enable the photosensitizer to effectively generate ROS is the most critical problem for improving the antibacterial activity.
Based on the content, the Sph-Ru-MMT @ PZ nano antibacterial agent and the preparation method and the application thereof are provided.
Disclosure of Invention
The invention aims to provide a Sph-Ru-MMT @ PZ nano antibacterial agent, and a preparation method and application thereof, so as to solve the problems in the background technology.
The invention realizes the purpose through the following technical scheme:
the invention provides an Sph-Ru-MMT @ PZ nano antibacterial agent which comprises nano particles Sph-Ru-MMT @ PZ, wherein the nano particles Sph-Ru-MMT @ PZ are obtained by sequentially loading montmorillonite MMT and a photosensitizer zinc phthalocyanine PZ onto nano ruthenium complex particles Sph-Ru, and the diameters of the nano particles Sph-Ru-MMT @ PZ are 85-155 nm.
The invention also provides application of the Sph-Ru-MMT @ PZ nano antibacterial agent in the field of preparation of anti-Escherichia coli medicaments.
As a further optimization scheme of the invention, the Sph-Ru-MMT @ PZ nano antibacterial agent is irradiated by infrared light under the condition of resisting escherichia coli.
The invention also provides a preparation method of the nano-particles Sph-Ru-MMT, which comprises the following steps:
(1) will [ Ru (bpy)2Cl2]And dppz are dissolved in an ethanol solution, a polystyrene suspension is added into the solution dropwise, the mixture is obtained by vigorous mixing, and the mixture is heated, refluxed, cooled, precipitated, centrifugally washed and dried to obtain nano ruthenium complex particles Sph-Ru;
(2) mixing montmorillonite MMT with an ethanol solution, adding cetyl trimethyl ammonium bromide CTAB into the solution to obtain a mixture, stirring, condensing, refluxing, centrifuging and washing to obtain a precipitate, and dissolving the precipitate in water to obtain a first stock solution;
(3) mixing the stock solution I in the step (2) with a silane coupling agent KH-550, adding ethanol to form a mixture, adjusting the pH of the mixture to acidity, heating, cooling, centrifugally washing, and suspending the obtained substance in deionized water to obtain a suspension II;
(4) dissolving the nano ruthenium complex particles Sph-Ru in deionized water, mixing the solution with the suspension II in the step (3), stirring, filtering, collecting filtrate, centrifuging, washing and drying the filtrate to obtain nano particles Sph-Ru-MMT;
(5) dissolving a photosensitizer zinc phthalocyanine PZ in a hydrofluoric acid solution, adding a nanoparticle Sph-Ru-MMT solution dissolved in deionized water into the solution to obtain a mixture, adjusting the PH of the mixture to be alkaline, filtering the mixture, collecting filtrate, and centrifugally washing and drying the filtrate to obtain the nanoparticles Sph-Ru-MMT @ PZ.
As a further optimization scheme of the invention, the diameter of the nano ruthenium complex particle Sph-Ru in the step (1) is 5-25 nm.
As a further optimization scheme of the invention, HCl is adopted in the step (3) to adjust the pH value of the mixture to 3-4.
As a further optimization scheme of the invention, the diameter of the nanoparticles Sph-Ru-MMT in the step (4) is 75-135 nm.
As a further optimization scheme of the above invention, the step before the filtration of the mixture in the step (5) is specifically: completely dissolving photosensitizer zinc phthalocyanine PZ and hydrofluoric acid by using an ultrasonic bath, dissolving Sph-Ru-MMT in deionized water by using the ultrasonic bath for 20-30 min, stirring for 2-3 h in the dark at room temperature, adding the solution into a mixed solution of the photosensitizer zinc phthalocyanine PZ and hydrofluoric acid, and adjusting the pH of the mixture to 7-8 by using NaOH.
As a further optimization scheme of the invention, the filtration in the step (4) and the filtration in the step (5) are both carried out by adopting a membrane filter with the diameter of 0.45 μm.
As a further optimization scheme of the invention, the number of times of centrifugal washing in the steps (1) to (5) is at least three, the centrifugal rotation speed is 3000-5000 rpm, and the centrifugal time is 3-5 min.
The invention has the beneficial effects that: MMT is loaded on Sph-Ru nano-particles and anchored on the outer surface of an escherichia coli membrane, and the membrane anchoring functional photosensitizer zinc phthalocyanine PZ is irradiated by 670nm near infrared NIR light and can damage the structure of bacteria by generating reactive oxygen ROS, so that escherichia coli is cracked; after bacteria are cracked, Sph-Ru-MMT @ PZ is combined with biomolecules of damaged bacteria, Sph-Ru emits strong red fluorescence, and more importantly, Sph-Ru-MMT @ PZ has no response to live Escherichia coli with complete cell membranes, but selectively stains and displays fluorescence in early cell membrane damage and late cell nucleus exposure periods, red fluorescence can be observed when bacteria die, and excessive use of drugs is effectively avoided.
Drawings
FIG. 1 is a TEM of Sph-Ru prepared in comparative example 1;
FIG. 2 is a TEM of Sph-Ru-MMT obtained by comparative example 2;
FIG. 3 is a TEM of the Sph-Ru-MMT @ PZ nano antibacterial agent prepared in example 1;
FIG. 4 is an infrared spectrum of Sph-Ru prepared in comparative example 1, Sph-Ru-MMT prepared in comparative example 2, and Sph-Ru-MMT @ PZ prepared in example 1;
FIG. 5 is a Zeta potential diagram of Sph-Ru prepared in comparative example 1, Sph-Ru-MMT prepared in comparative example 2, and Sph-Ru-MMT @ PZ prepared in example 1.
FIG. 6 is a MIC chart for minimum inhibitory concentration determination of Sph-Ru-MMT @ PZ prepared in example 1.
FIG. 7 is a graph showing the fluorescence effect of Sph-Ru-MMT @ PZ and E.coli.
Detailed Description
The present application will now be described in further detail with reference to the drawings, it should be noted that the following detailed description is given for illustrative purposes only and is not to be construed as limiting the scope of the present application, as those skilled in the art will be able to make numerous insubstantial modifications and adaptations to the present application based on the above disclosure.
The invention relates to a preparation method of a Sph-Ru-MMT @ PZ nano antibacterial agent, which comprises the following steps:
(1) will [ Ru (bpy)2Cl2]0.27 g-2.7 g and dppz0.15g-1.5 g are dissolved in 8.0-20 mL of ethanol solution, and the volume ratio of ethanol to water in the ethanol solution is 3: 1, putting the mixture into a three-neck flask, dropwise adding 500-1500 muL of polystyrene suspension, violently mixing to obtain a mixture, heating the mixture to reflux for 10-12 h at 100-110 ℃ under argon, cooling the reaction mixture to room temperature to obtain a yellow solution, removing the solvent by using a rotary evaporator, and adding NH4PF6Precipitating the complex by using an aqueous solution, suspending the solid in ethanol for 3min by using an 80KHz ultrasonic bath, centrifugally washing with tetrahydrofuran to remove polystyrene, finally centrifugally washing with deionized water, removing the solvent, and drying to obtain the nano ruthenium complex particles Sph-Ru with the diameter of 5-25 nm.
(2) Mixing 1.0-5.0 g of montmorillonite MMT with 2.0-6.0 mL of water and 2.0-6.0 mL of ethanol in a conical flask, then adding 2.0-5.0 g of cetyl trimethyl ammonium bromide CTAB to obtain a mixture, stirring for reaction, then heating to 60-70 ℃ by using a reflux condenser, keeping for 1-2 h, centrifuging the reaction mixture, centrifugally washing by using deionized water, centrifugally washing by using ethanol, dissolving the obtained precipitate in the deionized water, and taking the precipitate as a first stock solution.
(3) Mixing the stock solution I and 5.0-10 mL of silane coupling agent KH-550 in a conical flask, adding 5.0-10 mL of ethanol to form a mixture, adjusting the pH of the mixture to 3-4 by using HCl, heating the mixture to 55-65 ℃, keeping the temperature for 3-4 h, cooling, centrifugally washing the reaction mixture by using deionized water, and suspending the reaction mixture in the deionized water to obtain a suspension II.
(4) Ultrasonically dissolving 5.0-10 mg of nano ruthenium complex particles Sph-Ru in 5-10 mL of deionized water for 30min, then mixing with 2.0-4.0 mL of suspension II, stirring at room temperature for 3-4 h in a beaker, filtering turbid solution through a 0.45-micrometer membrane filter, collecting filtrate, centrifugally washing with deionized water, removing solvent, and drying to obtain 75-135 nm-diameter nano particles Sph-Ru-MMT.
(5) Completely dissolving 2.0-4.0 mg of photosensitizer zinc phthalocyanine PZ and 3.0-6.0 mL of hydrofluoric acid in a beaker by using an ultrasonic bath, dissolving 5.0-10 mg of Sph-Ru-MMT in 5.0-10 mL of deionized water in the ultrasonic bath for 20-30 min, stirring for 2-3 h in the dark at room temperature, adding the mixture into the beaker to obtain a mixture, adjusting the pH of the obtained mixture to 7-8 by using NaOH, filtering the obtained mixture by using a 0.45-micrometer membrane filter, centrifuging and washing the filtrate by using deionized water, removing the solvent and drying to obtain 85-155 nm-diameter nanoparticle Sph-Ru-MMT @ PZ.
In the steps, centrifugal washing is carried out for at least three times, the centrifugal rotating speed is 3000-5000 rpm, and the centrifugal time is 3-5 min.
Example 1
(1) 0.27g of [ Ru (bpy)2Cl2]And 0.15g dppz in 8.0mL ethanol solution into a three-necked flask, 500 μ L of polystyrene suspension was added dropwise, vigorous mixing was performed to obtain a mixture, the mixture was heated to reflux at 100 ℃ under argon for 10h, the reaction mixture was cooled to room temperature to obtain a yellow solution, and the solvent was removed using a rotary evaporator by adding NH4PF6Precipitating the complex with water solution, suspending the solid in ethanol for 3min with 80KHz ultrasonic bath, centrifuging with tetrahydrofuran to remove polystyrene, centrifuging with deionized water, removing solvent, and oven drying to obtain nanometer powderRuthenium complex particles Sph-Ru.
(2) In an erlenmeyer flask, 1.0g montmorillonite MMT and 6.0mL water and 6.0mL ethanol mixture, then, adding 3.0g cetyl trimethyl ammonium bromide CTAB to obtain a mixture, stirring reaction, then using the reflux condenser to heat to 70 degrees C for 2 hours, the reaction mixture centrifugal, using deionized water centrifugal washing, and then ethanol centrifugal washing, the obtained precipitate dissolved in deionized water, and used as a stock solution one.
(3) Mixing the first stock solution with 5.0mL of KH-550 in a conical flask, adding 5.0mL of ethanol to form a mixture, adjusting the pH of the mixture to 4 with 3mol/L HCl, heating the mixture to 65 ℃ for 4h, cooling, washing the reaction mixture with deionized water by centrifugation, and suspending the reaction mixture in deionized water to obtain a second suspension.
(4) And ultrasonically dissolving 5.0mg of nano ruthenium complex particles Sph-Ru in 5mL of deionized water for 30min, then mixing with 2.0mL of the suspension II, stirring for 4h at room temperature in a beaker, filtering the turbid solution through a 0.45-micrometer membrane filter, collecting filtrate, centrifugally washing with deionized water, removing the solvent, and drying to obtain the nano particles Sph-Ru-MMT.
(5) Completely dissolving 2.0mg of photosensitizer zinc phthalocyanine PZ and 3.0mL of hydrofluoric acid in a beaker by using an ultrasonic bath, dissolving 5.0mg of Sph-Ru-MMT in 5.0mL of deionized water in the ultrasonic bath for 30min, stirring for 3h in the dark at room temperature, adding the solution into the beaker to obtain a mixture, adjusting the pH of the obtained mixture to 7 by using a substance with the quantity concentration of 0.1mol/LNaOH, filtering the obtained mixture by using a 0.45 mu m membrane filter, centrifugally washing the filtrate by using deionized water, removing the solvent and drying to obtain the nano-particle Sph-Ru-MMT @ PZ.
The Sph-Ru-MMT @ PZ prepared in example 1 is shown in FIG. 3, and the average diameter is 85-155 nm.
Comparative example 1
0.27g of [ Ru (bpy)2Cl2]And 0.15g dppz in 8.0mL of ethanol solution were placed in a three-necked flask, 500 μ L of polystyrene suspension was added dropwise, vigorous mixing was performed to obtain a mixture, and the mixture was heated to reflux at 100 ℃ under argonAfter 10h, the reaction mixture was cooled to room temperature to give a yellow solution, and the solvent was removed using a rotary evaporator by addition of NH4PF6Precipitating the complex by using an aqueous solution, suspending the solid in ethanol for 3min by using an 80KHz ultrasonic bath, centrifugally washing by using tetrahydrofuran to remove polystyrene, finally centrifugally washing by using deionized water, removing the solvent and drying to obtain the nano ruthenium complex particles Sph-Ru.
Sph-Ru prepared in comparative example 1 is shown in figure 1, and the average diameter of the Sph-Ru is 15-20 nm.
Comparative example 2
(1) 0.27g of [ Ru (bpy)2Cl2]And 0.15g dppz in 8.0mL ethanol solution into a three-necked flask, 500 μ L of polystyrene suspension was added dropwise, vigorous mixing was performed to obtain a mixture, the mixture was heated to reflux at 100 ℃ under argon for 10h, the reaction mixture was cooled to room temperature to obtain a yellow solution, and the solvent was removed using a rotary evaporator by adding NH4PF6Precipitating the complex by using an aqueous solution, suspending the solid in ethanol for 3min by using an 80KHz ultrasonic bath, centrifugally washing by using tetrahydrofuran to remove polystyrene, finally centrifugally washing by using deionized water, removing the solvent and drying to obtain the nano ruthenium complex particles Sph-Ru.
(2) In an erlenmeyer flask, 1.0g montmorillonite MMT and 6.0mL water and 6.0mL ethanol mixture, then, adding 3.0g cetyl trimethyl ammonium bromide CTAB to obtain a mixture, stirring reaction, then using the reflux condenser to heat to 70 degrees C for 2 hours, the reaction mixture centrifugal, using deionized water centrifugal washing, and then ethanol centrifugal washing, the obtained precipitate dissolved in deionized water, and used as a stock solution one.
(3) Mixing the first stock solution with 5.0mL of KH-550 in a conical flask, adding 5.0mL of ethanol to form a mixture, adjusting the pH of the mixture to 4 with 3mol/L HCl, heating the mixture to 65 ℃ for 4h, cooling, washing the reaction mixture with deionized water by centrifugation, and suspending the reaction mixture in deionized water to obtain a second suspension.
(4) And ultrasonically dissolving 5.0mg of nano ruthenium complex particles Sph-Ru in 5mL of deionized water for 30min, then mixing with 2.0mL of the suspension II, stirring for 4h at room temperature in a beaker, filtering the turbid solution through a 0.45-micrometer membrane filter, collecting filtrate, centrifugally washing with deionized water, removing the solvent, and drying to obtain the nano particles Sph-Ru-MMT.
The Sph-Ru-MMT prepared in the comparative example 2 is shown in figure 2, and the average diameter is 75-135 nm.
FIG. 4 is an infrared spectrum of Sph-Ru prepared in comparative example 1, Sph-Ru-MMT prepared in comparative example 2, and Sph-Ru-MMT @ PZ prepared in example 1, as shown by infrared spectroscopy: all RuNP samples were 1653cm-1Shows a pyridine ring peak at 709cm-1The Sph-Ru peak is subjected to blue shift, which indicates that the compound drug loading system is more stable.
FIG. 5 is a Zeta potential plot of the Sph-Ru prepared in comparative example 1, the Sph-Ru-MMT prepared in comparative example 2, and the Sph-Ru-MMT @ PZ prepared in example 1, showing that the Zeta potential of Sph-Ru dissolved in deionized water is 8.0 + -0.2 mV, the surface of the Sph-Ru-MMT is negatively charged when the negatively charged MMT is wrapped around the Sph-Ru, and the Zeta potential drops to-12.2 + -0.5 mV, and as the positively charged PZ is further adsorbed, the potential rises to-6.1 + -0.2 mV, and these changes in Zeta potential are observed at each step, indicating successful encapsulation of the MMT and complete modification of the PZ.
FIG. 6 is a MIC chart of Minimum Inhibitory Concentration (MIC) assay of Sph-Ru-MMT @ PZ prepared in example 1, and the results show that: the MIC of the Sph-Ru-MMT @ PZ subjected to infrared irradiation is obviously reduced, the bacteriostatic ability is obviously enhanced, and the minimum bacteriostatic concentration of the Sph-Ru-MMT @ PZ nano antibacterial agent on Escherichia coli E.coli is 3.3 +/-0.21 mug/mL.
FIG. 7 shows the fluorescence effect of Sph-Ru-MMT @ PZ and Escherichia coli, wherein after three RuNPs are incubated in Escherichia coli, no fluorescence is observed, lysozyme LZM is added dropwise and then the incubation is carried out for 30 minutes, and if the fluorescence effect is observed under ultraviolet light, red fluorescence is generated; in the Sph-Ru-MMT @ PZ + IR group, after 12 hours incubation with E.coli, strong red fluorescence was observed under UV light. This result indicates that the Sph-Ru-MMT @ PZ + IR treatment acts on e.coli as the lysozyme treatment, both will disrupt the cell wall, leading to cell lysis, the DNA in the lysate then binds to Sph-Ru and fluorescence quenched by Sph-Ru is recovered.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (10)
1. The nano antibacterial agent is characterized by comprising nano particles Sph-Ru-MMT @ PZ, wherein the nano particles Sph-Ru-MMT @ PZ are obtained by sequentially loading montmorillonite MMT and a photosensitizer zinc phthalocyanine PZ onto nano ruthenium complex particles Sph-Ru, and the diameters of the nano particles Sph-Ru-MMT @ PZ are 85-155 nm.
2. The use of the Sph-Ru-MMT @ PZ nanoantimicrobial of claim 1 in the preparation of an anti-escherichia coli medicament.
3. The application of the Sph-Ru-MMT @ PZ nano antibacterial agent in preparation of an anti-Escherichia coli drug according to claim 2, wherein the Sph-Ru-MMT @ PZ nano antibacterial agent is subjected to infrared light IR irradiation.
4. A method of making Sph-Ru-MMT @ PZ nanoparticles as claimed in claim 1, comprising the steps of:
(1) will [ Ru (bpy)2Cl2]And dppz are dissolved in an ethanol solution, a polystyrene suspension is added into the solution dropwise, the mixture is obtained by vigorous mixing, and the mixture is heated, refluxed, cooled, precipitated, centrifugally washed and dried to obtain nano ruthenium complex particles Sph-Ru;
(2) mixing montmorillonite MMT with an ethanol solution, adding cetyl trimethyl ammonium bromide CTAB into the solution to obtain a mixture, stirring, condensing, refluxing, centrifuging and washing to obtain a precipitate, and dissolving the precipitate in water to obtain a first stock solution;
(3) mixing the stock solution I in the step (2) with a silane coupling agent KH-550, adding ethanol to form a mixture, adjusting the pH of the mixture to acidity, heating, cooling, centrifugally washing, and suspending the obtained substance in deionized water to obtain a suspension II;
(4) dissolving the nano ruthenium complex particles Sph-Ru in deionized water, mixing the solution with the suspension II in the step (3), stirring, filtering, collecting filtrate, centrifuging, washing and drying the filtrate to obtain nano particles Sph-Ru-MMT;
(5) dissolving a photosensitizer zinc phthalocyanine PZ in a hydrofluoric acid solution, adding a nanoparticle Sph-Ru-MMT solution dissolved in deionized water into the solution to obtain a mixture, adjusting the PH of the mixture to be alkaline, filtering the mixture, collecting filtrate, and centrifugally washing and drying the filtrate to obtain the nanoparticles Sph-Ru-MMT @ PZ.
5. The preparation method of the nano ruthenium complex particle Sph-Ru according to claim 4, wherein the diameter of the nano ruthenium complex particle Sph-Ru in the step (1) is 5-25 nm.
6. The preparation method of the nano ruthenium complex particle Sph-Ru as claimed in claim 4, wherein HCl is used in the step (3) to adjust the pH of the mixture to 3-4.
7. The preparation method of the Sph-Ru-MMT @ PZ nano antibacterial agent according to claim 4, wherein the diameter of the nano particles Sph-Ru-MMT in the step (4) is 75-135 nm.
8. The method for preparing a nano antibacterial agent Sph-Ru-MMT @ PZ as claimed in claim 4, wherein the step (5) of filtering the mixture is specifically as follows: completely dissolving photosensitizer zinc phthalocyanine PZ and hydrofluoric acid by using an ultrasonic bath, dissolving Sph-Ru-MMT in deionized water by using the ultrasonic bath for 20-30 min, stirring for 2-3 h in the dark at room temperature, adding the solution into a mixed solution of the photosensitizer zinc phthalocyanine PZ and hydrofluoric acid, and adjusting the pH of the mixture to 7-8 by using NaOH.
9. The method for preparing a nano antibacterial agent Sph-Ru-MMT @ PZ as claimed in claim 4, wherein the filtration in step (4) and the filtration in step (5) are performed by using a 0.45 μm membrane filter.
10. The preparation method of the Sph-Ru-MMT @ PZ nano antibacterial agent according to claim 4, wherein the number of times of centrifugal washing in the steps (1) to (5) is at least three, the centrifugal rotation speed is 3000-5000 rpm, and the centrifugal time is 3-5 min.
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