CN102319435A - Mesoporous silica compound particles containing gold nanorods, preparation method and application thereof - Google Patents
Mesoporous silica compound particles containing gold nanorods, preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of high molecular materials, particularly relating to environmental-responsive mesoporous silica compound particles containing gold nanorods, a preparation method and an application thereof. The preparation method comprises the following steps of: at first, preparing gold nanorods by using a seeded growth method; then coating a layer of mesoporous silica on the surfaces of the gold nanorods by using a stabilizer cetyltrimethyl ammonium bromide on the surfaces of the gold nanorods as a template; and finally, depositing an environmental-responsive type polymer on the surfaces of the gold nanorods by using a template polymerization method, to obtain the compound particles with the surfaces modified by temperature-sensitive polymers. The method provided by the invention is simple and the raw materials are easy to obtain. The prepared compound particles can be used for loading drugs; and because the gold nanorods absorb near infrared light, phase inversion is carried out on the temperature-sensitive polymers on the surfaces of the mesoporous silica compound particles through the generated photo-thermal effect, so that the loaded drugs are released. According to the method provided by the invention, the obtained product has wide application prospect in the field of drug controlled release.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of mesoporous silicon oxide compound particle that is used for controlled release drug.
Background technology
Metaporous silicon dioxide material is a kind of duct ordered arrangement; Pore size is generally 2 ~ 50nm, and the narrow material that distributes, because it has excellent biological compatibility; Medicine carrying efficient is high; Bigger specific surface area and pore volume, thus better chemical and heat stability and surface be rich in the silicon hydroxyl and be beneficial to advantages such as further functionalization, be widely used at medicine carrying and drug release field.But; Metaporous silicon dioxide material is during as pharmaceutical carrier; The targeting that can not realize medicine discharges, thus discharge polymer with environment-responsive and compound can the realization of mesoporous silicon oxide to controlled delivery of pharmaceutical agents, thus reduce medicine to Normocellular toxic and side effects.
The functional nano particle of environment-responsive can be to external environment condition such as light, temperature, and pH, magnetic etc. make fast reaction, and make self physicochemical properties change the nanoparticle of control drug release.Wherein, The temperature sensitivity nanoparticle has attracted vast research worker; Because the temperature of cancerous tumours cell is usually above normal cell; Temperature sensitive polymer just can be realized rapid release cancer therapy drug at high temperature, and low temperature slowly discharges the function of medicine down, thereby reduces medicine effectively to Normocellular infringement.In all temperature sensitive polymers, the research that gathers (N-Isopropylacrylamide) is more extensive.But the application of independent gathering (N-Isopropylacrylamide) material is relatively limited to, because its phase transition temperature is fixed 32
oC so many research worker are regulated its phase transition temperature through introducing other comonomer, thereby enlarges its range of application.
Nanometer gold rod (draw ratio is 2～20) two ends have strong enhancing electric field; Show different plasma bands of a spectrum at major axis with short-axis direction; Has horizontal and vertical biabsorption peak; Anisotropic gold nanorods has chemistry and optic anisotropy simultaneously; Gold nanorods surface plasma resonance characteristic that more special is and based on the strong absorption and the characteristics of luminescence of surface plasma resonance, vertical plasma absorption band of nanometer gold rod can be adjusted near infrared region, efficiently luminous energy is converted into heat energy.The gold rod is introduced in the nano particle of temperature sensitivity, and with laser irradiation a period of time of certain intensity and wavelength, golden rod can be converted into heat energy to the luminous energy that absorbs.The excellent photo-thermal effect of gold through the near-infrared laser irradiation can make the generation of the polymer of temperature sensitivity change mutually, thereby loaded drugs is discharged, and realizes that controlled delivery of pharmaceutical agents discharges.
With regard to the compound particle that environment-responsive contains the nanometer gold rod, present bibliographical information seldom mainly adopts the physically trapping method through electrostatic interaction.This method reaction exists a problem to be exactly, and the interaction of coating is more weak, can not steady in a long-termly exist, especially under the physiological environment of harshness.
Summary of the invention
The objective of the invention is to propose the mesoporous silicon oxide compound particle that a kind of environment-responsive contains the nanometer gold rod.
The environment-responsive that the present invention proposes contains the method for preparing of the mesoporous silicon oxide compound particle of nanometer gold rod, is a kind of method at aqueous phase matrix polymerization finishing environment-responsive polymer.The phase transition temperature of polymer can be controlled, realizes that the fixed point of medicine discharges, and in the preparation process, introduce the meso-porous titanium dioxide silicon structure cleverly.Its preparation process is following:
Step 1 is a raw material with the gold chloride, is Reducing agent with the sodium borohydride, and the gold ion that at first reduces obtains the gold seeds that diameter is 3～4nm.With the silver ion in the silver nitrate is assisting ion, is surfactant with the cetyl ammonium bromide, is weak reductant with the ascorbic acid, joins gold seeds solution, can obtain the nanometer gold rod;
Step 2 is with improved Stober method coating mesoporous silicon dioxide outside the nanometer gold rod.Specifically be template with the cetyl trimethyl ammonium bromide, the pH value that adds ammonia (mass concentration is 25%) and ethyl orthosilicate conditioned reaction solution is 9～12.38～42
oC is reaction 2～24h down.Reaction solution is dispersed in the ethanol 60～80
oC adds the silica-based propyl methacrylate of 3-trimethoxy down, reaction 3～5h; Remove the silica-based propyl methacrylate of unreacted 3-trimethoxy through centrifugation method, product is dispersed in the ammonium nitrate alcoholic solution that concentration is 8～12mg/mL 60～80
oC reaction 5h～8 h down removes template;
Step 3 is utilized the polymer of matrix polymerization product surface deposition environment-responsive of gained in step 2.Specifically be with product in the step 2 through the centrifugation method purification, be dispersed in the water, add the N-Isopropylacrylamide, quality for the coating of not removing template 5～7 times of nanometer gold rod of mesoporous silicon oxide; Add N hydroxymethyl acrylamide, quality for the coating of not removing template 1～3 times of nanometer gold rod of mesoporous silicon oxide; Add N, N-methylene acrylamide, quality is 0.4～0.6 times of nanometer gold rod that has coated mesoporous silicon oxide; Logical nitrogen 25～35 minutes adds 1 potassium peroxydisulfate, and quality is 0.4～0.6 times of nanometer gold rod that has coated mesoporous silicon oxide, and 60～80
oC continues reaction 4h～6 h down, and reaction is carried out post processing with centrifugation method after finishing, and obtains phase transition temperature 34
oC～40
oThe finishing of C the mesoporous silicon oxide compound particle that contains nanometer gold rod of temperature sensitive polymer.
The inventive method is simple, and raw material is easy to get.The environment-responsive compound particle can be through the proportioning of control various polymerization thing, the phase transition temperature of telomerized polymer.The fixed point that the compound particle of preparation can be applicable to medicine discharges, as the carrier of drug targeting release.Because nanometer gold rod adsorbing close infrared light, the photo-thermal effect of generation can make the temperature sensitive polymer on mesoporous silicon oxide compound particle surface take place to change mutually, thereby loaded drugs is discharged.The product that the inventive method obtains has very big application prospect in medicine sustained release field.
The present domestic method for preparing external environment response gold rod mainly adopts the physically trapping method, and comparatively speaking, the present invention has following characteristics:
(1) the polymer phase transition temperature can be controlled;
(2) the prepared composite particle is highly stable, and has excellent biological compatibility;
(3) introduce mesoporous silicon oxide cleverly and improve nanoparticle medicine carrying efficient, make method for preparing become simple to operation simultaneously.
Description of drawings
The transmission electron microscope photo of Fig. 1, nanometer gold rod.
The transmission electron microscope photo of Fig. 2, mesoporous silicon oxide clad nano gold rod.
Fig. 3, environment-responsive contain the transmission electron microscope photo of the mesoporous silicon oxide compound particle of nanometer gold rod, and background dyes with phosphotungstic acid.
The specific embodiment
Embodiment 1: with the gold chloride is raw material, is Reducing agent with the sodium borohydride, and the gold ion that at first reduces obtains the gold seeds that diameter is 3～4nm.With the silver ion in the silver nitrate is assisting ion, is surfactant with the cetyl ammonium bromide, is weak reductant with the ascorbic acid, adds gold seeds solution and can obtain golden excellent nanoparticle as shown in Figure 1 afterwards; With improved Stober method coating mesoporous silicon dioxide silicon outside the gold rod, be template with the cetyl trimethyl ammonium bromide, the pH value that adds ammonia (25%) and ethyl orthosilicate conditioned reaction solution is 10.40
oC is reaction 2～24h down.Reaction solution is dispersed in the ethanol 60～80
oC adds the silica-based propyl methacrylate of 3-trimethoxy down, behind reaction 3～5h, removes the silica-based propyl methacrylate of unreacted 3-trimethoxy through centrifugation method, product is dispersed in the ammonium nitrate alcoholic solution that concentration is 10mg/mL 60～80
oC reaction 6h down removes template, obtains the golden excellent nanoparticle of the coating mesoporous silicon dioxide shown in Fig. 2 transmission electron microscope photo.Add N-Isopropylacrylamide 90mg, N hydroxymethyl acrylamide 10mg, N,N methylene bis acrylamide 5mg adds potassium peroxydisulfate 10mg, under the nitrogen atmosphere, 60～80
oC is reaction 5h down, and reaction is carried out post processing with centrifugation method after finishing, and obtains phase transition temperature 34
oThe environment-responsive of C shown in Fig. 3 transmission electron microscope photo contains the mesoporous silicon oxide compound particle of nanometer gold rod.
Embodiment 2: with the gold chloride is raw material, is Reducing agent with the sodium borohydride, and the gold ion that at first reduces obtains the gold seeds that diameter is 3～4nm.With the silver ion in the silver nitrate is assisting ion, is surfactant with the cetyl ammonium bromide, is weak reductant with the ascorbic acid, and adding after the gold seeds solution can golden excellent nanoparticle; With improved Stober method coating mesoporous silicon dioxide outside the gold rod, be template with the cetyl trimethyl ammonium bromide, the pH value that adds ammonia (25%) and ethyl orthosilicate conditioned reaction solution is 10.40
oC is reaction 2～24h down.Reaction solution is dispersed in the ethanol 60～80
oC adds the silica-based propyl methacrylate of 3-trimethoxy down, behind reaction 3～5h, removes the silica-based propyl methacrylate of unreacted 3-trimethoxy through centrifugation method, product is dispersed in the ammonium nitrate alcoholic solution that concentration is 10mg/mL 60～80
oC reaction 6h down removes template.Add N-Isopropylacrylamide 85mg, N hydroxymethyl acrylamide 15mg, N,N methylene bis acrylamide 5mg adds potassium peroxydisulfate 10mg, under the nitrogen atmosphere, 60～80
oC is reaction 5h down, and reaction is carried out post processing with centrifugation method after finishing, and obtains phase transition temperature 38
oThe environment-responsive of C contains the mesoporous silicon oxide compound particle of nanometer gold rod.
Embodiment 3: with the gold chloride is raw material, is Reducing agent with the sodium borohydride, and the gold ion that at first reduces obtains the gold seeds that diameter is 3～4nm.With the silver ion in the silver nitrate is assisting ion, is surfactant with the cetyl ammonium bromide, is weak reductant with the ascorbic acid, and adding after the gold seeds solution can golden excellent nanoparticle; With improved Stober method coating mesoporous silicon dioxide outside the gold rod, be template with the cetyl trimethyl ammonium bromide, the pH value that adds ammonia (25%) and ethyl orthosilicate conditioned reaction solution is 10.40
oC is reaction 2～24h down.Reaction solution is dispersed in the ethanol 60～80
oC adds the silica-based propyl methacrylate of 3-trimethoxy down, behind reaction 3～5h, removes the silica-based propyl methacrylate of unreacted 3-trimethoxy through centrifugation method, product is dispersed in the ammonium nitrate alcoholic solution that concentration is 10mg/mL 60～80
oC reaction 6h down removes template.Add N-Isopropylacrylamide 80mg, N hydroxymethyl acrylamide 20mg, N,N methylene bis acrylamide 5mg adds potassium peroxydisulfate 10mg, under the nitrogen atmosphere, 60～80
oC is reaction 5h down, and reaction is carried out post processing with centrifugation method after finishing, and obtains phase transition temperature 40
oThe environment-responsive of C contains the mesoporous silicon oxide compound particle of nanometer gold rod.
Embodiment 4: the amycin aqueous solution of preparation 1mg/mL.Get a certain amount of amycin solution and mix with the mesoporous silicon oxide compound particle carrier that contains the nanometer gold rod, the mass ratio of medicine and carrier is 0.3, stirs 12～24h under the room temperature, and centrifugalize is washed 3 times with deionized water repeatedly, obtains the compound particle of medicine carrying.The supernatant of collecting is used for the uv absorption test, and drawing carrying drug ratio is 14%, and envelop rate is 62%.
Embodiment 5: the tetrasulfonic acid base peptide cyanines zinc aqueous solution of preparation 1mg/mL.Getting a certain amount of tetrasulfonic acid base peptide cyanines zinc solution mixes with the mesoporous silicon oxide compound particle carrier that contains the nanometer gold rod; The mass ratio of medicine and carrier is 0.3, stirs 12～24h under the room temperature, centrifugalize; Wash repeatedly 3 times with deionized water, obtain the compound particle of medicine carrying.Collect supernatant and be used for fluorometric investigation, the carrying drug ratio that draws tetrasulfonic acid base peptide cyanines zinc is 13%, and envelop rate is 50%.
Claims (7)
1. an environment-responsive contains the method for preparing of the mesoporous silicon oxide compound particle of nanometer gold rod, it is characterized in that concrete steps are following:
Step 1 is a raw material with the gold chloride, is Reducing agent with the sodium borohydride, and the gold ion that at first reduces obtains the gold seeds that diameter is 3～4nm; With the silver ion in the silver nitrate is assisting ion, is surfactant with the cetyl ammonium bromide, is weak reductant with the ascorbic acid, behind the adding gold seeds solution, promptly obtains golden excellent nanoparticle;
Step 2 with improved Stober method coating mesoporous silicon dioxide outside the gold rod, the steps include: with the cetyl trimethyl ammonium bromide to be template, and the pH value that adds ammonia and ethyl orthosilicate conditioned reaction solution is 9～12; 38-42
oC is reaction 2～24h down; Reaction solution is dispersed in the ethanol 60～80
oC adds the silica-based propyl methacrylate of 3-trimethoxy down, reaction 3～5h; Remove the silica-based propyl methacrylate of unreacted 3-trimethoxy through centrifugation method, product is dispersed in the ammonium nitrate alcoholic solution that concentration is 8～12 mg/mL 60～80
oC reaction 5h～8 h down removes template;
Step 3; Utilize the polymer of matrix polymerization product surface deposition environment-responsive of gained in step 2; The steps include: product in the step 2 through the centrifugation method purification; Be dispersed in the water, add the N-Isopropylacrylamide, quality is 5～7 times of the gold rod of the coating mesoporous silicon dioxide of not removing template; Add N hydroxymethyl acrylamide, quality is 1～3 times of the gold rod of the coating mesoporous silicon dioxide of not removing template; Add N, N-methylene acrylamide, quality is 0.4～0.6 times of gold rod of coating mesoporous silicon dioxide, and logical nitrogen 25～35 minutes adds 1 potassium peroxydisulfate, and quality is 0.4～0.6 times of gold rod of coating mesoporous silicon dioxide, 60～80
oC continues reaction 0.4～0.6h down, and reaction is carried out post processing with centrifugation method after finishing, and obtains phase transition temperature 34
oC～40
oThe finishing of C the gold rod that contains mesoporous silicon oxide of temperature sensitive polymer.
2. environment-responsive according to claim 1 contains the method for preparing of the mesoporous silicon oxide compound particle of nanometer gold rod; It is characterized in that: in the step 2; Get the golden rod that 5ml do not remove the coating mesoporous silicon dioxide of template and be dispersed in the 50ml ethanol 60～80
oC adds the silica-based propyl methacrylate of 0.5ml 3-trimethoxy down with two keys in the finishing; Reaction 3～5h; Remove the silica-based propyl methacrylate of unreacted 3-trimethoxy through centrifugation method, product is dispersed in the ammonium nitrate alcoholic solution that 40ml concentration is 10mg/mL 60～80
oC reaction 6h down removes template, and product through the centrifugation method purification, is dispersed in the water.
3. environment-responsive according to claim 1 and 2 contains the method for preparing of the mesoporous silicon oxide compound particle of nanometer gold rod, it is characterized in that: in the step 3, add N-Isopropylacrylamide 90mg; N hydroxymethyl acrylamide 10mg; N,N methylene bis acrylamide 5mg adds potassium peroxydisulfate 10mg; Under the nitrogen atmosphere, 60～80
oC is reaction 5h down, and reaction is carried out post processing with centrifugation method after finishing, and obtains phase transition temperature 34
oThe environment-responsive of C contains the mesoporous silicon oxide compound particle of nanometer gold rod.
4. environment-responsive according to claim 1 and 2 contains the method for preparing of the mesoporous silicon oxide compound particle of nanometer gold rod, it is characterized in that: in the step 3, add N-Isopropylacrylamide 85mg; N hydroxymethyl acrylamide 15mg; N,N methylene bis acrylamide 5mg adds potassium peroxydisulfate 10mg; Under the nitrogen atmosphere, 60～80
oC is reaction 5h down, and reaction is carried out post processing with centrifugation method after finishing, and obtains phase transition temperature 38
oThe environment-responsive of C contains the mesoporous silicon oxide compound particle of nanometer gold rod.
5. environment-responsive according to claim 1 and 2 contains the method for preparing of the mesoporous silicon oxide compound particle of nanometer gold rod, it is characterized in that: in the step 3, add N-Isopropylacrylamide 80mg; N hydroxymethyl acrylamide 20mg; N,N methylene bis acrylamide 5mg adds potassium peroxydisulfate 10mg; Under the nitrogen atmosphere, 60～80
oC is reaction 5h down, and reaction is carried out post processing with centrifugation method after finishing, and obtains phase transition temperature 40
oThe environment-responsive of C contains the mesoporous silicon oxide compound particle of nanometer gold rod.
6. the environment-responsive for preparing like the described method of one of claim 1 to 5 contains the mesoporous silicon oxide compound particle of nanometer gold rod.
7. environment-responsive as claimed in claim 6 contains the application of the mesoporous silicon oxide compound particle of nanometer gold rod as the slow releasing agent of medicine sustained release.
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Cited By (11)
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| CN103495175A (en) * | 2013-10-14 | 2014-01-08 | 北京工业大学 | Preparation method of thermo-sensitive drug sustained and controlled release mesoporous composite |
| CN104707998A (en) * | 2015-03-13 | 2015-06-17 | 盐城工学院 | Nanometer golden rod used for detecting bovine serum albumin and preparation method and application thereof |
| CN106944615A (en) * | 2017-05-11 | 2017-07-14 | 洛阳理工学院 | A kind of preparation method of solid coated with silica gold nanorods composite nano materials |
| CN108079297A (en) * | 2018-01-16 | 2018-05-29 | 复旦大学 | A kind of application of up-conversion luminescence-thermochemotherapy composite Nano probe and preparation method thereof and therapeutic alliance Programmed control |
| CN108479111A (en) * | 2018-04-03 | 2018-09-04 | 佛山科学技术学院 | A kind of surface finish nano SiO2Solid phase micro extraction probe preparation method and application |
| CN108526478A (en) * | 2017-03-01 | 2018-09-14 | 苏州大学 | Nanogold-mesoporous silicon oxide composite material and preparation method |
| US10143988B2 (en) | 2015-05-08 | 2018-12-04 | North Carolina State University | Method for synthesizing non-spherical nanostructures |
| CN109358195A (en) * | 2018-11-06 | 2019-02-19 | 枣庄学院 | More empty silica shell nano enzymes of a kind of hollow plation nanocages core-and its preparation method and application |
| CN112957345A (en) * | 2021-02-07 | 2021-06-15 | 济南国科医工科技发展有限公司 | Light-operated drug release degradable temperature-sensitive mesoporous silicon nanoparticle system |
| CN113368237A (en) * | 2021-05-26 | 2021-09-10 | 西北工业大学 | Nano composite material with photo-thermal response controllable drug release and preparation method thereof |
| CN113509903A (en) * | 2020-04-09 | 2021-10-19 | 石河子大学 | Photostimulation response type material and preparation method and application thereof |
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| CN103495175A (en) * | 2013-10-14 | 2014-01-08 | 北京工业大学 | Preparation method of thermo-sensitive drug sustained and controlled release mesoporous composite |
| CN104707998A (en) * | 2015-03-13 | 2015-06-17 | 盐城工学院 | Nanometer golden rod used for detecting bovine serum albumin and preparation method and application thereof |
| US10143988B2 (en) | 2015-05-08 | 2018-12-04 | North Carolina State University | Method for synthesizing non-spherical nanostructures |
| CN108526478A (en) * | 2017-03-01 | 2018-09-14 | 苏州大学 | Nanogold-mesoporous silicon oxide composite material and preparation method |
| CN106944615A (en) * | 2017-05-11 | 2017-07-14 | 洛阳理工学院 | A kind of preparation method of solid coated with silica gold nanorods composite nano materials |
| CN108079297A (en) * | 2018-01-16 | 2018-05-29 | 复旦大学 | A kind of application of up-conversion luminescence-thermochemotherapy composite Nano probe and preparation method thereof and therapeutic alliance Programmed control |
| CN108479111A (en) * | 2018-04-03 | 2018-09-04 | 佛山科学技术学院 | A kind of surface finish nano SiO2Solid phase micro extraction probe preparation method and application |
| CN109358195A (en) * | 2018-11-06 | 2019-02-19 | 枣庄学院 | More empty silica shell nano enzymes of a kind of hollow plation nanocages core-and its preparation method and application |
| CN113509903A (en) * | 2020-04-09 | 2021-10-19 | 石河子大学 | Photostimulation response type material and preparation method and application thereof |
| CN113509903B (en) * | 2020-04-09 | 2022-06-28 | 石河子大学 | Photostimulation response type material and preparation method and application thereof |
| CN112957345A (en) * | 2021-02-07 | 2021-06-15 | 济南国科医工科技发展有限公司 | Light-operated drug release degradable temperature-sensitive mesoporous silicon nanoparticle system |
| CN112957345B (en) * | 2021-02-07 | 2022-03-08 | 济南国科医工科技发展有限公司 | Light-operated drug release degradable temperature-sensitive mesoporous silicon nanoparticle system |
| CN113368237A (en) * | 2021-05-26 | 2021-09-10 | 西北工业大学 | Nano composite material with photo-thermal response controllable drug release and preparation method thereof |
| CN113368237B (en) * | 2021-05-26 | 2022-11-01 | 西北工业大学 | Nano composite material with photo-thermal response controllable drug release and preparation method thereof |
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Application publication date: 20120118 |