CN109604632A - The method for preparing nano Au particle as template using polymyxin e - Google Patents
The method for preparing nano Au particle as template using polymyxin e Download PDFInfo
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- CN109604632A CN109604632A CN201811571731.6A CN201811571731A CN109604632A CN 109604632 A CN109604632 A CN 109604632A CN 201811571731 A CN201811571731 A CN 201811571731A CN 109604632 A CN109604632 A CN 109604632A
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The present invention relates to a kind of methods for preparing nano Au particle as template using polymyxin e, polymyxin e solution is prepared first, a part of gold particle is restored as crystal seed using the reproducibility of polymyxin e, is added ascorbic acid reduction, is obtained the nano Au particle with photo-thermal effect.Specific steps are as follows: prepare the polymyxin e solution of 0.1-3mg/mL, prepare 0.01-10mg/mL chlorauric acid solution, prepare 0.1-10mg/mL ascorbic acid solution；Polymyxin e solution is uniformly mixed with chlorauric acid solution in the ratio that the molar ratio of polymyxin e solution and chlorauric acid solution is 1:0.1~10, mixed solution is put into metal bath, the phosphate buffered saline solution of pH=7.4 is added, distilled water is added, it is incubated, equivalent ascorbic acid solution is then added by several times, each interval time is 1-10min, solution becomes bluish violet from light yellow, obtains nano Au particle.Nano Au particle obtained has photothermal conversion performance, uniform particle sizes, and stability is preferable.
Description
Technical field
The invention belongs to technical field of metal material, it is related to a kind of preparing nano Au particle by template of polymyxin e
Method.
Background technique
Metal nanoparticle has in numerous areas such as molecular device, chemical/biological sensors, catalysis, photoelectron materials
Broad application prospect.The preparation of metal nanoparticle utilizes reducing agent metal salt, so generally based on sol-gel method
Sintering obtains nanoparticle afterwards, and the partial size for the nanoparticle that this method obtains is larger, and particle diameter distribution is wide, and is difficult to solve
Agglomeration traits.
In recent years, using the unique optical property of noble metal nano particles, photo-thermal therapy is carried out to cancer and has become research
Hot spot.Noble metal nano particles have plasma resonance ability, absorb luminous energy and are converted into thermal energy, part is made to increase temperature
Degree, to kill cancer cell.The photothermal conversion ability of noble metal nano particles depends on its shape and size.But prepare light
Hot-cast socket performance height and the high noble metal nano particles of biocompatibility still have certain difficulty.Wherein, nano Au particle
It is that a kind of current biocompatibility is higher, inert metal thermotherapeutic agents of photothermal conversion better performances.At this point, nano Au particle has
Special appearance, including spherical shell, rodlike, dendroid etc..Therefore, the photo-thermal therapy agent of the nano Au particle of special appearance has good
Good development and application prospect.
Currently, template is a kind of very important method for preparing nanoparticle.The characteristics of template is no matter to react
Occur in liquid phase or gas phase, nano Au particle can restore generation in the effective coverage of template.Moreover, template can be adjusted
The partial size and pattern of nano Au particle are controlled, and plays the role of stable nanoparticle.Nowadays, the template of use is mostly artificial synthesized
Organic polymer.Most macromolecules have toxicity, are not easily applicable to biosystem.And the bacteriolyze of good biocompatibility
The biological macromolecular templates such as enzyme, trypsase and bovine serum albumin(BSA) are hardly formed the nanoparticle of photothermal conversion performance.Cause
This, it is also necessary to further develop the nano Au particle that new template is prepared with high photothermal conversion performance.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of side that nano Au particle is prepared using polymyxin e as template
Method, first preparation polymyxin e solution restore a part of gold particle as crystal seed using the reproducibility of polymyxin e, add
Ascorbic acid reduction, obtains the nano Au particle with photo-thermal effect.Preparation condition is simple, easy to operate.And raw material green ring
It protects, the nano Au particle of preparation has good photo-thermal effect.
The present invention is implemented as follows:
A method of nano Au particle is prepared by template of polymyxin e comprising following steps:
S1, polymyxin e solution is prepared:
With the mass ratio of distilled water and polymyxins 1:0.1-3,0.1-3mg/mL polymyxin e solution is prepared；
S2, chlorauric acid solution is prepared:
With the mass ratio of distilled water and gold chloride 1:0.01-10,0.01-10mg/mL chlorauric acid solution is prepared；
S3, ascorbic acid solution is prepared:
With the mass ratio of distilled water and ascorbic acid 1:0.1-10,0.1-10mg/mL ascorbic acid solution is prepared；
S4, nano Au particle is prepared:
In the molar ratio of polymyxin e solution and chlorauric acid solution be 1:0.1~10 ratio by polymyxin e solution with
Chlorauric acid solution is uniformly mixed, and mixed solution is put into metal bath, and the phosphate buffered saline solution of pH=7.4 is added, and is added and is steamed
Distilled water is incubated, and equivalent ascorbic acid solution is then added by several times, and each interval time is 1-10min, and solution is from light yellow
Become bluish violet, obtains nano Au particle.
Preferably, in step S4, the dosage of phosphate buffered saline solution is 0-1000 μ L, and the dosage of distilled water is 0-1000 μ
L。
Preferably, the amount that ascorbic acid solution is added in step S4 every time is 5-50 μ L.
Preferably, the method incubated in metal bath specifically: revolving speed is 200~1000rpm, temperature 10 DEG C~40
0-120min is incubated at DEG C.
Compared with prior art, the invention has the following advantages:
1, preparation method of the invention is simple, and reaction condition is mild, easy to operate.
2, nano Au particle produced by the present invention has photothermal conversion performance, uniform particle sizes, and stability is preferable.
3, template polymyxin e itself of the invention has very high biocompatibility, and product can be used for biomedical neck
Domain.
Detailed description of the invention
Fig. 1 is the transmission plot of nano Au particle prepared by embodiment 1.
Fig. 2 is the full wavelength scanner figure of nano Au particle prepared by embodiment 1.
Fig. 3 is the temperature ramp-up curve of nano Au particle prepared by embodiment 1.
Fig. 4 is temperature profile of the nano Au particle of the preparation of embodiment 1 during 5 light irradiation cycles.
Fig. 5 is the transmission plot of nano Au particle prepared by embodiment 2.
Fig. 6 is the temperature ramp-up curve of nano Au particle prepared by embodiment 2 and distilled water comparison.
Fig. 7 is the transmission plot of nano Au particle prepared by embodiment 3.
Fig. 8 is the temperature ramp-up curve of nano Au particle prepared by embodiment 3 and distilled water comparison.
Specific embodiment
Below with reference to the attached drawing exemplary embodiment that the present invention will be described in detail, feature and aspect of performance.It is identical in attached drawing
Appended drawing reference indicate element functionally identical or similar.Although the various aspects of embodiment are shown in the attached drawings, remove
It non-specifically points out, it is not necessary to attached drawing drawn to scale.
The present invention prepares polymyxin e solution first, using the reproducibility of polymyxin e restore a part of gold particle as
Crystal seed adds ascorbic acid reduction, obtains the nano Au particle with photo-thermal effect.
A method of nano Au particle is prepared by template of polymyxin e comprising following steps:
S1, polymyxin e solution is prepared:
With the mass ratio of distilled water and polymyxins 1:0.1-3,0.1-3mg/mL polymyxin e solution is prepared；
S2, chlorauric acid solution is prepared:
With the mass ratio of distilled water and gold chloride 1:0.01-10,0.01-10mg/mL chlorauric acid solution is prepared；
S3, ascorbic acid solution is prepared:
With the mass ratio of distilled water and ascorbic acid 1:0.1-10,0.1-10mg/mL ascorbic acid solution is prepared；
S4, nano Au particle is prepared:
Polymyxin e solution is added in the centrifuge tube of 2mL, by the molar ratio of polymyxin e solution and chlorauric acid solution
Polymyxin e solution is uniformly mixed with chlorauric acid solution for the ratio of 1:0.1~10, mixed solution is put into metal bath,
The phosphate buffered saline solution 0-1000 μ L of pH=7.4 is added, the distilled water of 0-1000 μ L is added, revolving speed is 200~1000rpm,
0-120min is incubated at 10 DEG C~40 DEG C of temperature, equivalent ascorbic acid solution is then added by several times, each interval time is 1-
10min, solution become bluish violet from light yellow, obtain nano Au particle.
Preferably, the amount that ascorbic acid solution is added in step S4 every time is 5-50 μ L.
The solution in a small amount of above-mentioned steps S4 is taken, ultrafiltration centrifugation is carried out, excessive hydroboration is added in solution after centrifugation
Sodium, solution colour are in colorless and transparent, to show all to generate nano Au particles.
Embodiment 1
S1, polymyxin e solution is prepared:
It takes polymyxin e to be dissolved in distilled water, is configured to the polymyxin e solution that concentration is 3mg/mL；
S2, chlorauric acid solution is prepared:
With the mass ratio of distilled water and gold chloride 1:0.4, being configured to concentration is 0.4mg/mL chlorauric acid solution；
S3, ascorbic acid solution is prepared:
With the mass ratio of distilled water and ascorbic acid 1:1, being configured to concentration is 1mg/mL ascorbic acid solution；
S4, nano Au particle is prepared:
400 μ L polymyxin e solution are added in the centrifuge tube of 2mL, by rubbing for polymyxin e solution and chlorauric acid solution
Mixed solution is put into metal bath, adds than being that polymyxin e solution is uniformly mixed by the ratio of 1:1 with chlorauric acid solution by you
Enter the distilled water of the phosphate buffered saline solution 400 μ L and 400 μ L of pH=7.4, revolving speed 600rpm is incubated at 20 DEG C of temperature
Then equivalent ascorbic acid solution is added in 15min by several times, each interval time is 5min, and the amount being added every time is 20 μ L, solution
Become bluish violet from light yellow, obtains nano Au particle.
Morphology characterization is carried out to nano Au particle obtained using transmission electron microscope, as shown in Figure 1, nano Au particle
Pattern it is different, without obvious spherical morphology, partial size is about in 15-30nm.Using ultraviolet specrophotometer to nano Au particle
Full wavelength scanner is carried out, as shown in Fig. 2, nano Au particle has very wide absorption band in 700-800nm.
For the photo-thermal effect for studying nano Au particle, following experiment is set:
1) nano Au particle solution 1mL made from Example 1, is added the cuvette of 5mL；It is sent out using 808nm infrared light
Emitter is in 4W/cm2Under conditions of, the nano Au particle solution in cuvette is irradiated, records a solution temperature every 30s, and
Point and line chart is drawn, the photothermal conversion performance of nano Au particle is analyzed.Such as Fig. 3 it can be seen that nano Au particle solution in 750s from
Room temperature rises to 43.5 DEG C, it means that the luminous energy of NIR laser effectively can be converted to thermal energy by nano Au particle.
2) using 808nm infrared transmitter in 4W/cm2Under conditions of, irradiate the nano Au particle solution in cuvette
10min or so, temperature stop irradiation when rising to 45 DEG C nearby, allow its cooled to room temperature at room temperature, reuse
808nm infrared transmitter irradiating sample, rises its temperature again, in this way, circulation five times are observed its stable circulation performance.Such as
Shown in Fig. 4 after 5 solar thermochemical cycles are tested, sample still has higher photothermal conversion performance.To sum up, possessed by nano Au particle
Higher photothermal conversion performance and photo and thermal stability allow to as the PTT reagent in photo-thermal therapy of cancer.
Embodiment 2
S1, polymyxin e solution is prepared:
It takes polymyxin e to be dissolved in distilled water, is configured to the polymyxin e solution that concentration is 3mg/mL；
S2, chlorauric acid solution is prepared:
With the mass ratio of distilled water and gold chloride 1:0.4, being configured to concentration is 0.4mg/mL chlorauric acid solution；
S3, ascorbic acid solution is prepared:
With the mass ratio of distilled water and ascorbic acid 1:1, being configured to concentration is 1mg/mL ascorbic acid solution；
S4, nano Au particle is prepared:
400 μ L polymyxin e solution are added in the centrifuge tube of 2mL, by rubbing for polymyxin e solution and chlorauric acid solution
Mixed solution is put into metal bath, turns than being that polymyxin e solution is uniformly mixed by the ratio of 1:1 with chlorauric acid solution by you
Speed is 500rpm, incubates 60min at 25 DEG C of temperature, and then addition equivalent ascorbic acid solution, each interval time are by several times
5min, the amount being added every time are 20 μ L, and solution becomes bluish violet from light yellow, obtains nano Au particle.
Morphology characterization is carried out to nano Au particle obtained using transmission electron microscope, as shown in figure 5, nano Au particle
Pattern there is irregular protrusion, partial size is about in 100-200nm.
For the photo-thermal effect for studying nano Au particle, following experiment is set:
Nano Au particle solution 1mL made from Example 2, is added the cuvette of 5mL；Use 808nm infrared light emission
Device irradiates the nano Au particle solution in cuvette under conditions of 4W/cm2, records a solution temperature every 30s, to steam
Distilled water is comparison, carries out same detection, and draw point and line chart, analyzes the photothermal conversion performance of nano Au particle.As Fig. 6 can be seen
Nano Au particle solution rises to 45.6 DEG C from 22.4 DEG C in 750s out, and as a control group, distilled water solution is not shown
Radiation is obvious responsed to, and temperature is only increased to 27 DEG C from 22.5 DEG C in 750s.This illustrates that nano Au particle is coarse
Surface texture results in very big internal field's enhancing, to allow light of the nano Au particle more effectively by NIR laser
Thermal energy can be converted to.
Embodiment 3
S1, polymyxin e solution is prepared:
It takes polymyxin e to be dissolved in distilled water, is configured to the polymyxin e solution that concentration is 3mg/mL；
S2, chlorauric acid solution is prepared:
With the mass ratio of distilled water and gold chloride 1:0.4, being configured to concentration is 0.4mg/mL chlorauric acid solution；
S3, ascorbic acid solution is prepared:
With the mass ratio of distilled water and ascorbic acid 1:1, being configured to concentration is 1mg/mL ascorbic acid solution；
S4, nano Au particle is prepared:
400 μ L polymyxin e solution are added in the centrifuge tube of 2mL, by rubbing for polymyxin e solution and chlorauric acid solution
Mixed solution is put into metal bath, adds than being that polymyxin e solution is uniformly mixed by the ratio of 1:1 with chlorauric acid solution by you
Enter phosphate buffered saline solution 800 μ L, the revolving speed 200rpm of pH=7.4, incubate 60min at 25 DEG C of temperature, is then added by several times
Equivalent ascorbic acid solution, each interval time are 5min, and the amount being added every time is 20 μ L, and solution becomes royal purple from light yellow
Color obtains nano Au particle.
Morphology characterization is carried out to nano Au particle obtained using transmission electron microscope, as shown in fig. 7, nano Au particle
There is obvious irregular protrusion at edge, and partial size is about in 40-100nm.
For the photo-thermal effect for studying nano Au particle, following experiment is set:
Nano Au particle solution 1mL made from Example 3, is added the cuvette of 5mL；Use 808nm infrared light emission
Device is in 4W/cm2Under conditions of, the nano Au particle solution in cuvette is irradiated, records a solution temperature every 30s, to steam
Distilled water is comparison, carries out same detection, and draw point and line chart, the photothermal conversion performance of nano Au particle is analyzed, as Fig. 8 can be seen
Nano Au particle solution rises to 42.8 DEG C from 23.5 DEG C in 750s out, and as a control group, distilled water solution is not shown
Radiation is obvious responsed to, and temperature is only increased to 27 DEG C from 22.5 DEG C in 750s.This illustrates that nano Au particle surface is prominent
Oval tip out results in bigger internal field's enhancing, to allow nano Au particle effectively by NIR laser
Luminous energy is converted to thermal energy.
To sum up, the invention has the following advantages that
Preparation method of the invention is simple, first preparation polymyxin e solution, is restored using the reproducibility of polymyxin e
A part of gold particle adds ascorbic acid reduction, obtains the nano Au particle with photo-thermal effect, reaction condition as crystal seed
Mildly, main reaction process is carried out using metal bath, and easy to operate.
Nano Au particle produced by the present invention is with photothermal conversion performance, the nano Au particle uniform particle sizes prepared every time,
And stability is preferable.
Template polymyxin e of the invention itself has very high biocompatibility, and product can be used for field of biomedicine.
Finally, it should be noted that above-described each embodiment is merely to illustrate technical solution of the present invention, rather than it is limited
System；Although the present invention is described in detail referring to the foregoing embodiments, those skilled in the art should understand that: its
It can still modify to technical solution documented by previous embodiment, or part of or all technical features are carried out
Equivalent replacement；And these modifications or substitutions, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution
Range.
Claims (4)
1. a kind of method for preparing nano Au particle as template using polymyxin e, it is characterised in that: itself the following steps are included:
S1, polymyxin e solution is prepared:
With the mass ratio of distilled water and polymyxins 1:0.1-3,0.1-3mg/mL polymyxin e solution is prepared；
S2, chlorauric acid solution is prepared:
With the mass ratio of distilled water and gold chloride 1:0.01-10,0.01-10mg/mL chlorauric acid solution is prepared；
S3, ascorbic acid solution is prepared:
With the mass ratio of distilled water and ascorbic acid 1:0.1-10,0.1-10mg/mL ascorbic acid solution is prepared；
S4, nano Au particle is prepared:
It is in the ratio that the molar ratio of polymyxin e solution and chlorauric acid solution is 1:0.1~10 that polymyxin e solution and chlorine is golden
Acid solution is uniformly mixed, and mixed solution is put into metal bath, and the phosphate buffered saline solution of pH=7.4 is added, and distilled water is added,
It is incubated, equivalent ascorbic acid solution is then added by several times, each interval time is 1-10min, and solution becomes from light yellow
Bluish violet obtains nano Au particle.
2. the method according to claim 1 for preparing nano Au particle as template using polymyxin e, it is characterised in that: step
In rapid S4, the dosage of phosphate buffered saline solution is 0-1000 μ L, and the dosage of distilled water is 0-1000 μ L.
3. the method according to claim 2 for preparing nano Au particle as template using polymyxin e, it is characterised in that: step
The amount that ascorbic acid solution is added in rapid S4 every time is 5-50 μ L.
4. the method according to claim 1 for preparing nano Au particle as template using polymyxin e, it is characterised in that:
The method incubated in metal bath specifically: revolving speed is 200~1000rpm, incubates 0-120min at 10 DEG C~40 DEG C of temperature.
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