CN108200907B - Hexadecyl trimethyl ammonium bromide supported amino modified magnetic mesoporous nano particle and preparation method and application thereof - Google Patents

Hexadecyl trimethyl ammonium bromide supported amino modified magnetic mesoporous nano particle and preparation method and application thereof Download PDF

Info

Publication number
CN108200907B
CN108200907B CN201611183848.8A CN201611183848A CN108200907B CN 108200907 B CN108200907 B CN 108200907B CN 201611183848 A CN201611183848 A CN 201611183848A CN 108200907 B CN108200907 B CN 108200907B
Authority
CN
China
Prior art keywords
magnetic
nanoparticles
amino
trimethyl ammonium
ammonium bromide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201611183848.8A
Other languages
Chinese (zh)
Other versions
CN108200907A (en
Inventor
常智敏
董文飞
王政
张翼
李力
葛明锋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Suzhou Institute of Biomedical Engineering and Technology of CAS
Original Assignee
Suzhou Institute of Biomedical Engineering and Technology of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Suzhou Institute of Biomedical Engineering and Technology of CAS filed Critical Suzhou Institute of Biomedical Engineering and Technology of CAS
Priority to CN201611183848.8A priority Critical patent/CN108200907B/en
Publication of CN108200907A publication Critical patent/CN108200907A/en
Application granted granted Critical
Publication of CN108200907B publication Critical patent/CN108200907B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
    • A01N33/02—Amines; Quaternary ammonium compounds
    • A01N33/12—Quaternary ammonium compounds
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y25/00—Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Landscapes

  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Environmental Sciences (AREA)
  • Zoology (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Pest Control & Pesticides (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Toxicology (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention belongs to the field of nano materials, and particularly relates to amino-modified magnetic mesoporous nanoparticles supported by hexadecyl trimethyl ammonium bromide, and a preparation method and application thereof. The hexadecyl trimethyl ammonium bromide supported amino modified magnetic mesoporous nano particle comprises: (a) the mesoporous silica rod is embedded with the magnetic nanoparticles at one end of the silica rod; (b) cetyltrimethylammonium bromide supported on the silica rods; (c) functionalized amino groups on the surfaces of the magnetic nanoparticles; the length of the silicon dioxide rod is 70-200 nm, the particle size of the magnetic nanoparticles is 50-150 nm, and the pore diameter of the mesopores is 1-3 nm. The amino-modified magnetic mesoporous nanoparticles supported by the hexadecyl trimethyl ammonium bromide not only can realize the capture and separation of bacteria, but also has strong inhibition effect on the growth of the bacteria, and can be used for preparing bacteria capture and separation materials and antibacterial materials.

Description

Hexadecyl trimethyl ammonium bromide supported amino modified magnetic mesoporous nano particle and preparation method and application thereof
Technical Field
The invention belongs to the field of nano materials, and particularly relates to amino-modified magnetic mesoporous nanoparticles supported by hexadecyl trimethyl ammonium bromide, and a preparation method and application thereof.
Background
In the fields of health care, cosmetics and foods, the problems of bacterial infection and bacterial contamination are becoming more and more serious. Although sterilization techniques have advanced significantly with the continued development of detection techniques, accurate measurement and effective removal of pathogenic bacteria remains a significant challenge to today's scientists. To overcome these obstacles, the scientific community has made continuous efforts to design and improve multifunctional platforms for rapid bacterial capture efficiency and simultaneous bacterial detection and elimination, which may greatly facilitate the development of the fields of clinical diagnosis, environmental detection and food safety.
Among these many attempts, magnetic nanoparticles are widely used for detecting and killing bacteria by virtue of their excellent properties (excellent properties can be used for rapid bacteria capture and separation, easy surface functionalization for targeted bacteria capture and separation, excellent biocompatibility, etc.). However, the bare magnetic nanoparticles have limited their further applications due to the limitations of the loading capacity of bactericidal drugs and low bacterial capture efficiency. Therefore, the development of magnetic-based nano-platforms with outstanding bacteria capturing, separating and removing performance is the most urgent problem to be solved.
At present, no report that the magnetic mesoporous nano particles are used for preparing bacteria capture and separation materials or bacteriostatic materials exists.
Disclosure of Invention
Therefore, the invention provides an amino-modified magnetic mesoporous nanoparticle supported by hexadecyl trimethyl ammonium bromide and a preparation method and application thereof.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention provides a hexadecyl trimethyl ammonium bromide supported amino modified magnetic mesoporous nano particle, which comprises the following components in part by weight:
(a) the mesoporous silica rod is embedded with the magnetic nanoparticles at one end of the silica rod;
(b) cetyltrimethylammonium bromide supported on the silica rods;
(c) functionalized amino groups on the surfaces of the magnetic nanoparticles;
the length of the silicon dioxide rod is 70-200 nm, the particle size of the magnetic nanoparticles is 50-150 nm, and the pore diameter of the mesopores is 1-3 nm.
Preferably, the surface area of the magnetic mesoporous nanoparticles modified by amino carried by cetyl trimethyl ammonium bromide is 500-800 m2G, cumulative pore volume of not less than 0.3cm3(ii)/g; the magnetic response capacity of the magnetic nanoparticles is not less than 50 emu/g.
The invention also provides a preparation method of the hexadecyl trimethyl ammonium bromide supported amino modified magnetic mesoporous nanoparticles, which comprises the following steps:
and (2) ultrasonically dispersing 0.5-2 mL of magnetic nanoparticle aqueous solution with the concentration of 8-10 mg/mL, adding the aqueous solution into 8-12 mL of hexadecyl trimethyl ammonium bromide aqueous solution with the concentration of 4-6 mg/mL, fully dispersing, adding 0.1-1 mL of ammonia water, slowly adding 20-40 mu L of ethyl orthosilicate and 4-6 mu L of 3-aminopropyl trimethoxy silane, and continuously stirring for 20-40 minutes to obtain the amino modified magnetic mesoporous nanoparticles supported by the hexadecyl trimethyl ammonium bromide.
Preferably, the preparation method of the hexadecyl trimethyl ammonium bromide supported amino modified magnetic mesoporous nanoparticles comprises the following steps:
and (2) ultrasonically dispersing 1mL of the magnetic nanoparticle aqueous solution with the concentration of 8.6mg/mL, adding the magnetic nanoparticle aqueous solution into 10mL of hexadecyl trimethyl ammonium bromide aqueous solution with the concentration of 5mg/mL, fully dispersing, adding 0.5mL of ammonia water, slowly adding 30 mu L of ethyl orthosilicate and 5 mu L of 3-aminopropyl trimethoxy silane, and continuously stirring for 30 minutes to obtain the amino-modified magnetic mesoporous nanoparticles supported by the hexadecyl trimethyl ammonium bromide.
More preferably, the method for preparing the amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide according to the present invention,
the magnetic nanoparticles are prepared by the following method: stirring a mixture of a magnetic precursor, polyacrylic acid and diethylene glycol at 100-1000 rpm for 20-40 minutes under the conditions of nitrogen protection and room temperature, heating to 220-270 ℃, and continuing stirring at 100-1000 rpm for 20-40 minutes to prepare a first reaction solution; and injecting 60-80 ℃ diethylene glycol solution of sodium hydroxide into the first reaction solution, and continuously stirring at 100-1000 rpm for 0.5-2 hours to react to obtain the magnetic nanoparticles.
More preferably, the method for preparing the amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide according to the present invention,
also comprises the following steps: and separating, washing and drying the magnetic nanoparticles.
More preferably, the method for preparing the amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide according to the present invention,
the molar ratio of the polyacrylic acid to the magnetic precursor is 8-12: 1; the ratio of the volume of the diethylene glycol to the mole of the magnetic precursor is 30-40 mL/mmol.
The invention also provides the hexadecyl trimethyl ammonium bromide supported amino modified magnetic mesoporous nano particle prepared by the preparation method.
The invention also provides application of the amino modified magnetic mesoporous nano particle loaded with the hexadecyl trimethyl ammonium bromide in preparation of a bacteria capturing and separating material.
Preferably, in the above application of the present invention, the bacteria-capturing and separating material is a bacteria-capturing and separating material of staphylococcus aureus or escherichia coli.
The invention also provides application of the amino-modified magnetic mesoporous nanoparticles loaded with the hexadecyl trimethyl ammonium bromide in preparation of antibacterial materials.
Preferably, in the above application of the present invention, the bacteriostatic material is a bacteriostatic material of staphylococcus aureus or escherichia coli.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) on one hand, the size of the amino modified magnetic mesoporous nano particle loaded with the hexadecyl trimethyl ammonium bromide is 1 order of magnitude smaller than that of bacteria, and the magnetic mesoporous nano particle has a surface effect, so that the capacity of combining the bacteria is greatly improved; on the other hand, the magnetic mesoporous nano particle has positive charges on the surface, so the magnetic mesoporous nano particle can be combined with bacteria with negative charges on the surface through electrostatic interaction; in addition, the magnetic material also has magnetism, so that the capture and separation of bacteria (such as escherichia coli, staphylococcus aureus and the like) can be realized, and the magnetic material can be used for preparing a bacteria capture and separation material;
(2) the amino-modified magnetic mesoporous nanoparticles loaded with the hexadecyl trimethyl ammonium bromide have a strong inhibition effect on the growth of bacteria (such as escherichia coli, staphylococcus aureus and the like), and can be used for preparing antibacterial materials;
(3) the amino-modified magnetic mesoporous nanoparticles supported by the hexadecyl trimethyl ammonium bromide can be prepared by a one-pot method through the magnetic nanoparticles, so that the experimental steps are simplified, the preparation method is simple and convenient, and the industrial production and application of the magnetic mesoporous nanoparticles are facilitated.
Drawings
In order that the present disclosure may be more readily and clearly understood, reference is now made to the following detailed description of the present disclosure taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a diagram showing the procedure of capturing and separating bacteria in experimental examples 1 and 3, wherein 1 is amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide, 2 is bacteria, 3 is amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide and electrostatically adsorbed to the bacteria, and 4 is an additional magnet;
FIG. 2 is a graph showing the efficiency of bacterial trapping in Escherichia coli in the experimental group and the control group in Experimental example 1;
FIG. 3 is a graph showing bacterial capturing efficiency of Staphylococcus aureus in the experimental group and the control group in Experimental example 3;
FIG. 4(a) is a graph showing the inhibitory effect on Escherichia coli in the experimental group of Experimental example 2;
FIG. 4(b) is a graph showing the inhibitory effect on Staphylococcus aureus in Experimental example 4.
Detailed Description
Example 1
The preparation method of the amino-modified magnetic mesoporous nanoparticle supported by hexadecyl trimethyl ammonium bromide in the embodiment comprises the following steps:
stirring a mixture of a magnetic precursor, polyacrylic acid and diethylene glycol at 500rpm for 30 minutes under the conditions of nitrogen protection and room temperature, heating to 250 ℃, and continuing stirring at 500rpm for 30 minutes to prepare a first reaction solution; injecting a diethylene glycol solution of sodium hydroxide at 70 ℃ into the first reaction solution, and continuously stirring at 500rpm for 1 hour to react to obtain the magnetic nanoparticles; the molar ratio of the polyacrylic acid to the magnetic precursor is 10: 1; the ratio of the volume of the diethylene glycol to the mole of the magnetic precursor is 35 mL/mmol;
separating, washing and drying the magnetic nanoparticles;
and (2) ultrasonically dispersing 1mL of the magnetic nanoparticle aqueous solution with the concentration of 8.6mg/mL, adding the magnetic nanoparticle aqueous solution into 10mL of hexadecyl trimethyl ammonium bromide aqueous solution with the concentration of 5mg/mL, fully dispersing, adding 0.5mL of ammonia water, slowly adding 30 mu L of tetraethoxysilane and 5 mu L of 3-aminopropyl trimethoxy silane, continuously stirring for 30 minutes, and cleaning for 3 times by using ethanol after the reaction is finished to obtain the amino modified magnetic mesoporous nanoparticles supported by the hexadecyl trimethyl ammonium bromide.
The magnetic mesoporous nanoparticles modified by amino carried by cetyl trimethyl ammonium bromide in the embodiment include: (a) the mesoporous silica rod is embedded with the magnetic nanoparticles at one end of the silica rod; (b) cetyltrimethylammonium bromide supported on the silica rods; (c) functionalized amino groups on the surface of the magnetic nanoparticles. Through detection, the length of the silicon dioxide rod is 120nm, the particle size of the magnetic nanoparticles is 100nm, and the aperture of the mesopores is 2 nm; the specific surface area of the magnetic nanoparticles is 650m2G, cumulative pore volume of not less than 0.3cm3(ii)/g; the magnetic response capacity of the magnetic nanoparticles is not less than 50 emu/g.
Example 2
The preparation method of the amino-modified magnetic mesoporous nanoparticle supported by hexadecyl trimethyl ammonium bromide in the embodiment comprises the following steps:
stirring a mixture of a magnetic precursor, polyacrylic acid and diethylene glycol at 100rpm for 40 minutes under the conditions of nitrogen protection and room temperature, heating to 220 ℃, and continuing stirring at 100rpm for 40 minutes to prepare a first reaction solution; injecting a 60 ℃ diethylene glycol solution of sodium hydroxide into the first reaction solution, and continuously stirring at 100rpm for 2 hours to react to obtain the magnetic nanoparticles; the molar ratio of the polyacrylic acid to the magnetic precursor is 12: 1; the ratio of the volume of the diethylene glycol to the mole of the magnetic precursor is 30 mL/mmol;
separating, washing and drying the magnetic nanoparticles;
and (2) ultrasonically dispersing 0.5mL of magnetic nanoparticle aqueous solution with the concentration of 10mg/mL, adding the magnetic nanoparticle aqueous solution into 8mL of hexadecyl trimethyl ammonium bromide aqueous solution with the concentration of 6mg/mL, fully dispersing, adding 0.1mL of ammonia water, slowly adding 40 mu L of tetraethoxysilane and 4 mu L of 3-aminopropyl trimethoxy silane, continuously stirring for 40 minutes, and cleaning for 3 times by using ethanol after the reaction is finished to obtain the amino modified magnetic mesoporous nanoparticles carried by the hexadecyl trimethyl ammonium bromide.
The magnetic mesoporous nanoparticles modified by amino carried by cetyl trimethyl ammonium bromide in the embodiment include: (a) the mesoporous silica rod is embedded with the magnetic nanoparticles at one end of the silica rod; (b) cetyltrimethylammonium bromide supported on the silica rods; (c) functionalized amino groups on the surfaces of the magnetic nanoparticles; the length of the silicon dioxide rod is 70nm, the particle size of the magnetic nanoparticles is 150nm, and the aperture of the mesopores is 1 nm; the specific surface area of the magnetic nano-particles is 800m2G, cumulative pore volume of not less than 0.3cm3(ii)/g; the magnetic response capacity of the magnetic nanoparticles is not less than 50 emu/g.
Example 3
The preparation method of the amino-modified magnetic mesoporous nanoparticle supported by hexadecyl trimethyl ammonium bromide in the embodiment comprises the following steps:
stirring a mixture of the magnetic precursor, polyacrylic acid and diethylene glycol at 1000rpm for 20 minutes under the conditions of nitrogen protection and room temperature, heating to 270 ℃, and continuing stirring at 1000rpm for 20 minutes to prepare a first reaction solution; injecting a diethylene glycol solution of sodium hydroxide at the temperature of 80 ℃ into the first reaction solution, and continuously stirring at 1000rpm for 0.5 hour to react to obtain the magnetic nanoparticles; the molar ratio of the polyacrylic acid to the magnetic precursor is 8: 1; the ratio of the volume of the diethylene glycol to the mole of the magnetic precursor is 40 mL/mmol;
separating, washing and drying the magnetic nanoparticles;
ultrasonically dispersing 2mL of magnetic nanoparticle aqueous solution with the concentration of 8mg/mL, adding the magnetic nanoparticle aqueous solution into 12mL of hexadecyl trimethyl ammonium bromide aqueous solution with the concentration of 4mg/mL, fully dispersing, adding 1mL of ammonia water, slowly adding 20 mu L of ethyl orthosilicate and 6 mu L of 3-aminopropyl trimethoxy silane, continuously stirring for 20 minutes, and cleaning for 3 times by using ethanol after the reaction is finished to obtain the amino modified magnetic mesoporous nanoparticles supported by the hexadecyl trimethyl ammonium bromide.
The magnetic mesoporous nanoparticles modified by amino carried by cetyl trimethyl ammonium bromide in the embodiment include: (a) the mesoporous silica rod is embedded with the magnetic nanoparticles at one end of the silica rod; (b) cetyltrimethylammonium bromide supported on the silica rods; (c) functionalized amino groups on the surfaces of the magnetic nanoparticles; the length of the silicon dioxide rod is 200nm, the particle size of the magnetic nanoparticles is 50nm, and the aperture of the mesopores is 3 nm; the specific surface area of the magnetic nano-particles is 500m2G, cumulative pore volume of not less than 0.3cm3(ii)/g; the magnetic response capacity of the magnetic nanoparticles is not less than 50 emu/g.
Examples of the experiments
The following experimental examples demonstrate the technical effects of the present invention.
Experimental example 1Coli trapping and separating experiment
1. Experimental methods
Escherichia coli was inoculated into a plate covered with LB-agar medium and incubated at 37 ℃ for 24 hours. Picking one escherichia coli colony in a plate to disperse in an LB liquid culture medium, shaking and incubating for 24 hours at a constant temperature of 37 ℃ by using a shaking table, wherein the shaking speed is 200 revolutions per minute, diluting an escherichia coli culture solution into 107CFU/mL by using the LB liquid culture medium for standby, and then randomly dividing the escherichia coli culture solution into two groups: experimental and control groups.
Experimental groups: the amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide prepared in example 1 were added to 5mL of escherichia coli diluent to prepare solutions containing amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide at different concentrations (0, 6.25, 12.5, 25, 50, 100 μ g/mL), and incubated for 10 minutes at 37 ℃ with shaking; and then adsorbing the magnetic nanoparticles in the mixed solution by using a magnet, measuring the OD600 value of the supernatant by using an ultraviolet spectrophotometer, and calculating the corresponding bacteria capturing efficiency.
Control group: adding the amino-modified magnetic mesoporous nanoparticles without being supported by hexadecyl trimethyl ammonium bromide into 5mL of escherichia coli diluent to prepare a solution containing 100 microgram/mL of amino-modified magnetic mesoporous nanoparticles without being supported by hexadecyl trimethyl ammonium bromide, and incubating the solution for 10 minutes at 37 ℃ by shaking; and then adsorbing the magnetic nanoparticles in the mixed solution by using a magnet, measuring the OD600 value of the supernatant by using an ultraviolet spectrophotometer, and calculating the corresponding bacteria capturing efficiency.
2. Results of the experiment
The process of the capture and separation of Escherichia coli in the experimental group is shown in FIG. 1, and the efficiency of the bacteria capture of Escherichia coli in the experimental group and the control group is shown in FIG. 2.
As can be seen from fig. 1, the amino-modified magnetic mesoporous nanoparticles supported on cetyltrimethylammonium bromide prepared in example 1 can trap and separate escherichia coli.
As can be seen from fig. 2, the solution containing the amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide at different concentrations (6.25, 12.5, 25, 50, 100 μ g/mL) in the experimental group significantly increased the bacterial trapping efficiency against escherichia coli as compared to the control group.
3. Conclusion of the experiment
The amino-modified magnetic mesoporous nanoparticles loaded with the hexadecyl trimethyl ammonium bromide can be used for capturing and separating escherichia coli and can be used as a bacterial capturing and separating material for the escherichia coli.
Experimental example 2Escherichia coli bacteriostasis experiment
1. Experimental methods
Experimental groups: mu.L of the E.coli bacterial suspension was added to 10mL of LB liquid medium solution containing various concentrations (0, 6.25, 12.5, 25, 50, 100. mu.g/mL) of the amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide prepared in example 1, and then incubated at 37 ℃ for 24 hours with shaking at a speed of 200 rpm; the growth inhibition rate of the bacteria was calculated by measuring the OD600 value of the supernatant after the magnetic nanoparticles were adsorbed by the magnet.
Control group: adding 100 mu L of escherichia coli bacterial suspension into 10mL of LB liquid culture medium solution containing 100 mu g/mL of amino-modified magnetic mesoporous nanoparticles without being supported by hexadecyl trimethyl ammonium bromide, and then performing shaking incubation at 37 ℃ for 24 hours at the shaking speed of 200 revolutions per minute; the growth inhibition rate of the bacteria was calculated by measuring the OD600 value of the supernatant after the magnetic nanoparticles were adsorbed by the magnet.
The Minimum Inhibitory Concentration (MIC) was obtained by the following method: mu.L of E.coli suspensions containing various concentrations (0, 6.25, 12.5, 25, 50, 100. mu.g/mL) of the amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide prepared in example 1 were uniformly spread on LB-agar plates and incubated at 37 ℃ for 24 hours, and the number of colonies of E.coli in the respective plates was observed.
2. Results of the experiment
The inhibitory effect of the experimental group on E.coli is shown in FIG. 4 (a).
As shown in fig. 4(a), the amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide prepared in example 1 have an inhibitory effect on escherichia coli, and the Minimum Inhibitory Concentration (MIC) is 50 μ g/mL.
3. Conclusion of the experiment
The amino-modified magnetic mesoporous nanoparticles loaded with the hexadecyl trimethyl ammonium bromide can inhibit the growth of escherichia coli and can be used as a bacteriostatic material for the escherichia coli.
Experimental example 3Staphylococcus aureus capture and separation experiment
Staphylococcus aureus was inoculated into a plate covered with LB-agar medium and incubated at 37 ℃ for 24 hours. Selecting a staphylococcus aureus colony in a plate to disperse in an LB liquid culture medium, shaking and incubating for 24 hours at a constant temperature of 37 ℃ by a shaking table at a shaking speed of 200 revolutions per minute, diluting a staphylococcus aureus culture solution into 107CFU/mL by the LB liquid culture medium for later use, and then randomly dividing the culture solution into two groups: experimental and control groups.
Experimental groups: the amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide prepared in example 1 were added to 5mL of staphylococcus aureus dilution to prepare solutions containing amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide at different concentrations (0, 6.25, 12.5, 25, 50, 100 μ g/mL), and incubated for 10 minutes at 37 ℃ with shaking; and then adsorbing the magnetic nanoparticles in the mixed solution by using a magnet, measuring the OD600 value of the supernatant by using an ultraviolet spectrophotometer, and calculating the corresponding bacteria capturing efficiency.
Control group: adding the amino-modified magnetic mesoporous nanoparticles without being supported by cetyl trimethyl ammonium bromide into 5mL of staphylococcus aureus diluent to prepare a solution containing 100 mu g/mL of amino-modified magnetic mesoporous nanoparticles without being supported by cetyl trimethyl ammonium bromide, and incubating the solution for 10 minutes at 37 ℃ in a shaking way; and then adsorbing the magnetic nanoparticles in the mixed solution by using a magnet, measuring the OD600 value of the supernatant by using an ultraviolet spectrophotometer, and calculating the corresponding bacteria capturing efficiency.
2. Results of the experiment
The process chart of the capture and separation of staphylococcus aureus in the experimental group is shown in figure 1, and the bacterial capture efficiency of the staphylococcus aureus in the experimental group and the control group is shown in figure 3.
As can be seen from fig. 1, the amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide prepared in example 1 can capture and separate staphylococcus aureus.
As can be seen from fig. 3, the solution containing the amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide at different concentrations (6.25, 12.5, 25, 50, 100 μ g/mL) in the experimental group significantly increased the bacterial trapping efficiency against staphylococcus aureus as compared to the control group.
3. Conclusion of the experiment
The amino-modified magnetic mesoporous nanoparticles loaded with the hexadecyl trimethyl ammonium bromide can capture and separate staphylococcus aureus, and can be used as a bacteria capture and separation material of the staphylococcus aureus.
Experimental example 4Staphylococcus aureus bacteriostasis test
1. Experimental methods
Experimental groups: mu.L of the Staphylococcus aureus bacterial suspension was added to 10mL of LB liquid medium solution containing various concentrations (0, 6.25, 12.5, 25, 50, 100. mu.g/mL) of the amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide prepared in example 1, and then incubated at 37 ℃ for 24 hours with shaking at 200 rpm; the growth inhibition rate of the bacteria was calculated by measuring the OD600 value of the supernatant after the magnetic nanoparticles were adsorbed by the magnet.
Control group: adding 100 mu L of staphylococcus aureus bacterial suspension into 10mL of LB liquid culture medium solution containing 100 mu g/mL of amino-modified magnetic mesoporous nanoparticles without hexadecyl trimethyl ammonium bromide loading, and then shaking and incubating for 24 hours at 37 ℃ with the shaking speed of 200 revolutions per minute; the growth inhibition rate of the bacteria was calculated by measuring the OD600 value of the supernatant after the magnetic nanoparticles were adsorbed by the magnet.
The Minimum Inhibitory Concentration (MIC) was obtained by the following method: mu.L of Staphylococcus aureus suspensions containing various concentrations (0, 6.25, 12.5, 25, 50, 100. mu.g/mL) of the amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide prepared in example 1 were uniformly spread on an LB-agar plate and incubated at 37 ℃ for 24 hours, and the number of colonies of Staphylococcus aureus on the corresponding plate was observed.
2. Results of the experiment
The inhibitory effect of the experimental group on staphylococcus aureus is shown in fig. 4 (b).
As shown in fig. 4(b), the amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide prepared in example 1 have an inhibitory effect on staphylococcus aureus, and the Minimum Inhibitory Concentration (MIC) is 100 μ g/mL.
3. Conclusion of the experiment
The amino-modified magnetic mesoporous nanoparticles loaded with the hexadecyl trimethyl ammonium bromide can inhibit the growth of staphylococcus aureus and can be used as a bacteriostatic material of the staphylococcus aureus.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims (7)

1. The application of the magnetic mesoporous nanoparticles in preparing the antibacterial material is characterized in that the magnetic mesoporous nanoparticles are amino-modified magnetic mesoporous nanoparticles carried by cetyl trimethyl ammonium bromide, and the magnetic mesoporous nanoparticles comprise:
(a) the mesoporous silica rod is embedded with the magnetic nanoparticles at one end of the silica rod;
(b) cetyltrimethylammonium bromide supported on the silica rods;
(c) functionalized amino groups on the surfaces of the magnetic nanoparticles;
the length of the silicon dioxide rod is 70-200 nm, the particle size of the magnetic nanoparticles is 50-150 nm, and the pore diameter of the mesopores is 1-3 nm.
2. The use according to claim 1, wherein the magnetic nanoparticles have a specific surface area of 500 to 800m2G, cumulative pore volume of not less than 0.3cm3(ii)/g; the magnetic response capacity of the magnetic nanoparticles is not less than 50 emu/g.
3. The use of claim 1 or 2, wherein the preparation of the amino-modified magnetic mesoporous nanoparticles supported by cetyltrimethylammonium bromide comprises the following steps:
and (2) ultrasonically dispersing 0.5-2 mL of magnetic nanoparticle aqueous solution with the concentration of 8-10 mg/mL, adding the aqueous solution into 8-12 mL of hexadecyl trimethyl ammonium bromide aqueous solution with the concentration of 4-6 mg/mL, fully dispersing, adding 0.1-1 mL of ammonia water, slowly adding 20-40 mu L of ethyl orthosilicate and 4-6 mu L of 3-aminopropyl trimethoxy silane, continuously stirring for 20-40 minutes, and cleaning with ethanol after the reaction is finished to obtain the amino-modified magnetic mesoporous nanoparticles supported by hexadecyl trimethyl ammonium bromide.
4. The use according to claim 3, wherein the preparation of the amino-modified magnetic mesoporous nanoparticles supported on cetyltrimethylammonium bromide comprises the following steps:
and (2) ultrasonically dispersing 1mL of the magnetic nanoparticle aqueous solution with the concentration of 8.6mg/mL, adding the magnetic nanoparticle aqueous solution into 10mL of hexadecyl trimethyl ammonium bromide aqueous solution with the concentration of 5mg/mL, fully dispersing, adding 0.5mL of ammonia water, slowly adding 30 mu L of ethyl orthosilicate and 5 mu L of 3-aminopropyl trimethoxy silane, continuously stirring for 30 minutes, and cleaning with ethanol after the reaction is finished to obtain the amino-modified magnetic mesoporous nanoparticles supported by the hexadecyl trimethyl ammonium bromide.
5. Use according to claim 3,
the magnetic nanoparticles are prepared by the following method: stirring a mixture of a magnetic precursor, polyacrylic acid and diethylene glycol at 100-1000 rpm for 20-40 minutes under the conditions of nitrogen protection and room temperature, heating to 220-270 ℃, and continuing stirring at 100-1000 rpm for 20-40 minutes to prepare a first reaction solution; and injecting 60-80 ℃ diethylene glycol solution of sodium hydroxide into the first reaction solution, and continuously stirring at 100-1000 rpm for 0.5-2 hours to react to obtain the magnetic nanoparticles.
6. The use according to claim 3, wherein the preparation of the amino-modified magnetic mesoporous nanoparticles supported on cetyltrimethylammonium bromide further comprises the following steps: and separating, washing and drying the magnetic nanoparticles.
7. The use according to claim 5,
the molar ratio of the polyacrylic acid to the magnetic precursor is 8-12: 1; the ratio of the volume of the diethylene glycol to the mole of the magnetic precursor is 30-40 mL/mmol.
CN201611183848.8A 2016-12-20 2016-12-20 Hexadecyl trimethyl ammonium bromide supported amino modified magnetic mesoporous nano particle and preparation method and application thereof Active CN108200907B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611183848.8A CN108200907B (en) 2016-12-20 2016-12-20 Hexadecyl trimethyl ammonium bromide supported amino modified magnetic mesoporous nano particle and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611183848.8A CN108200907B (en) 2016-12-20 2016-12-20 Hexadecyl trimethyl ammonium bromide supported amino modified magnetic mesoporous nano particle and preparation method and application thereof

Publications (2)

Publication Number Publication Date
CN108200907A CN108200907A (en) 2018-06-26
CN108200907B true CN108200907B (en) 2020-12-04

Family

ID=62603407

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201611183848.8A Active CN108200907B (en) 2016-12-20 2016-12-20 Hexadecyl trimethyl ammonium bromide supported amino modified magnetic mesoporous nano particle and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN108200907B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111557306B (en) * 2020-05-21 2021-05-18 中国热带农业科学院南亚热带作物研究所 Nano-drug preparation and application thereof in prevention and control of banana vascular wilt

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101723389A (en) * 2009-11-17 2010-06-09 陕西北美基因股份有限公司 Method for preparing magnetic silica microspheres with surfaces modified by cations
CN105079825A (en) * 2015-09-08 2015-11-25 中国科学院苏州生物医学工程技术研究所 Nanoparticle and preparation method and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101723389A (en) * 2009-11-17 2010-06-09 陕西北美基因股份有限公司 Method for preparing magnetic silica microspheres with surfaces modified by cations
CN105079825A (en) * 2015-09-08 2015-11-25 中国科学院苏州生物医学工程技术研究所 Nanoparticle and preparation method and application thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《磁性介孔二氧化硅纳米粒子担载黄连素及其体外抗肿瘤作用的研究》;王政;《吉林大学硕士学位论文》;20150401;摘要 *

Also Published As

Publication number Publication date
CN108200907A (en) 2018-06-26

Similar Documents

Publication Publication Date Title
Zhan et al. Efficient removal of pathogenic bacteria and viruses by multifunctional amine-modified magnetic nanoparticles
Jia et al. Versatile graphene-based photothermal nanocomposites for effectively capturing and killing bacteria, and for destroying bacterial biofilms
Zhang et al. High-performance magnetic antimicrobial Janus nanorods decorated with Ag nanoparticles
CN109836622B (en) Organic-inorganic hybrid nano antibacterial material and preparation method and application thereof
US9809476B2 (en) Biological composite material loaded with magnetic nanoparticles with core-shell structure, the preparation therefore and the application
Bromberg et al. Bactericidal core-shell paramagnetic nanoparticles functionalized with poly (hexamethylene biguanide)
Wang et al. Vancomycin-modified Fe3O4@ SiO2@ Ag microflowers as effective antimicrobial agents
Vo et al. Silver deposited carboxymethyl chitosan-grafted magnetic nanoparticles as dual action deliverable antimicrobial materials
CN100460338C (en) Silver/magnetic nanometer particle and its preparation method
Qian et al. Antimicrobial activity of Fe‐loaded chitosan nanoparticles
CN101717812B (en) Preparation method and application of Nisin modified magnetic nano particle
Ramteke et al. Synthesis and broad spectrum antibacterial activity of magnetite ferrofluid
CN110787186A (en) Ga3+PDA (personal digital Assistant) targeted synergistic antibacterial nano material as well as preparation and application thereof
TWI666270B (en) An antibacterial composite and method for preparing the same
CN108200907B (en) Hexadecyl trimethyl ammonium bromide supported amino modified magnetic mesoporous nano particle and preparation method and application thereof
CN104814036A (en) Poly(diallyldimethylammonium chloride) modified magnetic particle, preparation method thereof, and application thereof in bacterium removal
Mirahmadi‐Zare et al. Core–shell fabrication of an extra‐antimicrobial magnetic agent with synergistic effect of substrate ligand to increase the antimicrobial activity of Ag nanoclusters
CN106587291B (en) Preparation and application of yttrium oxide-ferroferric oxide composite nano antibacterial material
Chen et al. Novel composite unit with one pyridinium and three N-halamine structures for enhanced synergism and superior biocidability on magnetic nanoparticles
Sharma et al. A multifunctional recyclable adsorbent based on engineered MIL-125 (Ti) magnetic mesoporous composite for the effective removal of pathogens
CN106173806B (en) SiO (silicon dioxide)2Preparation method and application of artemisinin antibacterial nanoparticles
Chen et al. Magnetic nanoparticles modified with quaternarized N-halamine based polymer and their antibacterial properties
CN114469893B (en) Quaternary ammonium salt silicon dioxide nano-particles, preparation method and application
CN110237048B (en) PEG-modified magnetic/quaternized chitosan nanoparticles with peroxidase activity and preparation method and application thereof
Rahma et al. Quaternized N-chloramine coated magnetic nanoparticles: a trifecta of superior antibacterial activity, minimal residual toxicity and rapid site removal

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant