CN106862586B - One kind is mixed59Fe nanometer gold bar and preparation method thereof - Google Patents
One kind is mixed59Fe nanometer gold bar and preparation method thereof Download PDFInfo
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- CN106862586B CN106862586B CN201710044927.9A CN201710044927A CN106862586B CN 106862586 B CN106862586 B CN 106862586B CN 201710044927 A CN201710044927 A CN 201710044927A CN 106862586 B CN106862586 B CN 106862586B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K51/00—Preparations containing radioactive substances for use in therapy or testing in vivo
- A61K51/02—Preparations containing radioactive substances for use in therapy or testing in vivo characterised by the carrier, i.e. characterised by the agent or material covalently linked or complexing the radioactive nucleus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
Abstract
The invention discloses one kind to mix59Fe nanometer gold bar and preparation method thereof mixes in the synthesis process of nanometer gold bar59Fe, radioactive activity is up to 0.2bq to 20bq.Due to59Fe is mixed in synthesis,59Fe comes into inside nanometer gold bar, and golden stick weave in, thus marked using this method point more simple in label it is more firm.Simultaneously59Fe half-life period is longer to can be used for carrying out long-term observation, obtains more experimental datas.
Description
Technical field
The invention belongs to nano biological effect and security technology areas, are related to nano material in the research of biological toxicological effect
Application, and in particular to one kind is mixed59Fe nanometer gold bar and preparation method thereof.
Background technique
The development of nanotechnology promotes a batch with the birth of the properties nano materials such as unique light, electricity, magnetic, noble metal nano
Material, especially gold nano grain, height-adjustable optical characteristics can greatly enhance the absorption to visible light and near infrared light,
Based on its good optical property and surface chemistry ability, researcher can be by other imaging molecule probes, such as nucleic probe64Cu and111In, optical probe ICG, magnetic resonance probe Fe3O4Multifunctional nano probe is constructed Deng label gold nano-material, is realized
Living imaging and Therapy study.
Currently, mark in nano material using radioactive isotope as tracer, material is grasped in vivo
Metabolic process is relatively common (i.e. tracer method).Since radioactive isotope can constantly emit penetrating with certain feature
Line (such as gamma-rays), therefore by radioactive detection methods, the nano material containing radionuclide can be tracked at any time in body
The motion change situation of interior or external position and its quantity.Tracer method has high sensitivity (10 simultaneously-14-10-18),
The features such as measurement method is simple and easy to do, can accurately quantify, and positions and meets the physiological condition of institute's research object.But some materials
In radioactive isotope half-life short (such as198Au only has 2.8 days half-life period), cause putting for material in the very short time
Penetrating property intensity just drops to an extremely low value, this is to probe into the long-term metabolic approach of material to bring difficulty.
Summary of the invention
In view of the above-mentioned problems, the invention proposes one kind to mix59Fe nanometer gold bar (59Fe-GNRs) and preparation method thereof, it is real
It is longer the incorporation half-life period in GNRs has been showed59Fe carries out radioactive label to nanometer gold bar.
To achieve the goals above, the invention adopts the following technical scheme:
One kind is mixed59The preparation method of Fe nanometer gold bar, comprising the following steps:
1) by HAuCl4Solution is mixed with CTAB solution, and NaBH is added under stiring4, stop after being vigorously stirred, be prepared
Golden kind of solution；
2) by AgNO3Solution and59FeCl3HCl is added in the mixed solution of CTAB and NaOL that (i.e. golden stick growth is molten simultaneously
Liquid) and stir, HAuCl is then added4Solution is simultaneously vigorously stirred to colourless, is added concentrated hydrochloric acid and is adjusted pH to 1-2；
3) ascorbic acid is added in the solution after adjusting pH to step 2), is vigorously stirred mixing, is eventually adding golden kind of solution,
It stirs evenly, the aged overnight at 25-30 DEG C, growth is mixed59Fe nanometer gold bar.
Further, step 3) further includes that will grow mixing of obtaining59It is washed 1-3 times after the centrifuge separation of Fe nanometer gold bar.
Preferably, the revolving speed being centrifuged is 8000-10000rpm, time 15-20min.
Further, gold kind solution described in step 1) is using preceding standing 30min or more.
Further, in step 1), CTAB solution, HAuCl4Solution and NaBH4Molar ratio be 2000: 5: 12.
Preferably, NaBH4Molar concentration be 0.01-0.02M, the speed being vigorously stirred be 400rpm or more, more Gao Yue
It is good, there is bubble generation to be advisable.
Further, in step 2), the molar ratio of CTAB and NaOL is 47: 1 to 69: 1 in mixed solution.
Further, the AgNO of addition3Molar concentration of the solution in the mixed solution of CTAB and NaOL is 0.48-0.9 μ
M。
Further, it in step 2), may be optionally added59FeCl3The amount of HCl is 10-1000Bq, corresponding final
What growth obtained mixes59Radiation activity in Fe nanometer gold bar can from 0.2Bq to 20Bq,59FeCl3The additional amount of HCl is higher, puts
Penetrating property counts higher.
Preferably, step 1) and 2) in, HAuCl4The molar concentration of solution is 0.5-1mM, the molar concentration of CTAB solution
For 0.2-0.3M.
Further, in step 3), the ascorbic acid being added in the solution after every 100mL step 2) adjusting pH is 0.32-
0.48mmol, the speed being vigorously stirred be 400rpm or more (without the higher the better in the case of too many bubble), time 30s-1min,
The amount for golden kind of the solution being then added is 80-160 μ L, mixing time 30s-1min.
Preferably, the molar concentration of ascorbic acid is 0.16mM.
The present invention also provides a kind of mixing by above method preparation59Fe nanometer gold bar.
Further,59The radiation activity of Fe can be from 0.2Bq to 20Bq.
Beneficial effects of the present invention are as follows:
The present invention mixes in the synthesis process of nanometer gold bar59(radioactive activity can increase Fe with incorporation, can be from
0.2bq to 20bq, is shown in Table 1, according to59The GNRs of different demands activity can be obtained in the variation of the amount of Fe), it will59FeCl3
Same AgNO3Can get when solution is added golden stick growth solution simultaneously maximum incorporation (59FeCl3When for same concentration), while not
The pattern of golden stick can be changed.Due to59Fe is mixed in synthesis,59Fe comes into inside nanometer gold bar, interweaves with golden stick
Together, therefore using this method point more simple in label it is more firm to mark.Simultaneously59Fe half-life period is longer (45 days), uses it
Instead of half-life short198Au (2.8 days) marking nano gold stick, can be used for carrying out long-term observation, obtains more experimental datas.
It is added in nanometer gold bar synthesis59FeCl3It need to consider that it is added the time and whether can change the shape of nanometer gold bar
Looks.Since gold nanorods are in growth course and its exclusive, foreign ion is easily excluded, and therefore, different time points is selected to be added59FeCl3And its it is important, by our exploration,59FeCl3It is added, is first mixed with gold kind, with HAuCl in gold kind synthesis4It is molten
Liquid is first mixed or is added prior to silver nitrate solution, and doping is added simultaneously with silver nitrate far fewer than in the growth-promoting media stage, mixes
Miscellaneous ratio is at least 10 times of other times section or more (see Table 1 for details).On the other hand, other ions are added and also easily change golden stick
Pattern, therefore, when considering xenogenesis radioactive element marker material, be nearly all with label realize, but put label easily
It falls off, causes to be enriched in some organ, bring illusion to research.We allow in synthesis59Fe enters nanometer gold bar in synthesis
Inside avoids label to the full extent and falls off, while finding to adulterate59After Fe and have not been changed golden stick looks, optical property is not yet
Change (see Fig. 1, Fig. 2), this brings possibility for further zoopery observation.
Detailed description of the invention
Fig. 1 is to be added without59The nanometer gold bar synthesized when Fe is mixed with what the present invention obtained59Fe nanometer gold bar
(59Fe-GNRs) comparison under Electronic Speculum.Figure (a) is not mix59The nanometer gold bar synthesized when Fe, figure (b) are
What the present invention obtained mixes59Fe nanometer gold bar (59Fe—GNRs)。
Fig. 2 is the UV absorption spectrogram of gold nanorods.Abscissa is absorbing wavelength, and ordinate is absorbance value.
Fig. 3 is the schematic diagram in mouse tail vein injection exposed material.
Specific embodiment
Realization process of the invention is described in further details below with reference to attached drawing, but is not limited to this.(1)
Nanometer gold bar is synthesized, and is mixed in the synthesis process on a small quantity59Fe is obtained59Fe—GNRs。
Synthetic method is as follows:
1. the preparation of gold medal kind solution
5mL CTAB (0.2M) solution and 5mL HAuCl4(0.5mM) solution mixes (molar ratio 400: 1), under stiring
The ice bath NaBH of 0.6mL brand-new is added4(0.01M) solution, after being vigorously stirred (revolving speed is big as far as possible, at least above 400rpm) 2min
Stop, golden kind of solution is prepared.Seed solution needs to stand 30min or more before use.
2. the preparation of growth-promoting media and golden stick synthesis
At 30 DEG C, 3.6 mL AgNO are added simultaneously to (50mL) in the solution of CTAB containing 1.4g and 0.246g NaOL3
Solution (4mM) and 100 μ L59FeCl3(radiation activity is 10Bq) simultaneously stirs 15min, and 50mL HAuCl is then added4Solution
(1mM) and it is vigorously stirred 90min, adds concentrated hydrochloric acid and adjust pH to 1.5.
It is stirred for 15min after adjusting pH, is added 0.25mL ascorbic acid (0.064M), is vigorously stirred 30s, is eventually adding
Golden kind of the solution of 80 μ L, stirs 30s, and 12h or more (general to stay overnight) is aged at 30 DEG C and is used for the growth of gold nanorods.Jenner
Rice stick is centrifugated at 10000rpm, and for several times with secondary water washing.
The gold nanorods of acquisition are placed in gamma spectrometer (ORTEC company of the GEM-20180-P type U.S.), radioactivity is obtained
Activity spectrogram obtains radioactive activity after spectrum unscrambling, and compared with back end, and wherein environment back end is without counting,59The counting rate of Fe-GNR
For 0.221/second, it is added59Fe amount is 6.5 × 10-4(being shown in Table 1).
Table 1 be environment back end (BG) with59Fe-GNR counts comparison
| Number | Sample | Nucleic | Energy (volt) | Counting rate (a/second) | Error |
| \ | BG | \ | \ | \ | \ |
| A | 59Fe-Au seeds-GNRs-1 | FE-59 | 1099.01 | 0.0180 | 13.0% |
| B | 59Fe-Au seeds-GNRs-2 | FE-59 | 1098.69 | 0.0205 | 20.3% |
| C | 59Fe-GNRs-1 | FE-59 | 1100.18 | 0.221 | 6.7% |
| D | 59Fe-GNRs-2 | FE-59 | 1099.63 | 2.96 | 6.5% |
In upper table, A is to be added in gold kind synthesis59FeCl3, B is59FeCl3Golden stick growth solution is added with gold kind
In, C, D are59FeCl3With AgNO3It is added in golden stick growth solution, is added in A, B, C together59FeCl3Radioactive activity is
10Bq, D 1000Bq.
As seen from the above table, it is added in different periods59FeCl3It is right59The incorporation of Fe has a significant impact, same radiation activity
's59FeCl3With AgNO3It is obtained in the golden stick growth solution of addition together59Fe incorporation is maximum, meanwhile,59FeCl3Amount increase
Also it can improve in nanometer gold bar59The incorporation of Fe.
What is finally obtained mixes59The SEM of Fe nanometer gold bar schemes as shown in Figure 1, it is about 74.08 ± 5.31nm, wide by about 20.64
± 1.38nm, draw ratio are about 1: 3.6, and undoped59The SEM of the common golden stick of Fe schemes comparison, and pattern has no significant change.
As shown in Fig. 2, its length characteristic peak is 760nm, optical characteristics still has the ultraviolet absorption spectrum of gold nanorods,
It has not been changed.
(2) tail vein injection is carried out to mouse59The observation of marker material can be realized in Fe-GNRs.
By what is synthesized59Fe-GNRs is added in 5% BSA solution (BSA solution is excessive) and is placed on shaking table,
180rpm to 200rpm shakes under room temperature one day and is modified (table 2 is modification front and back potential change) to golden stick, after modification
It is centrifugated under 3000rpm, removes supernatant liquor, precipitating is resuspended in water.BSA has preferable biocompatibility, through BSA
After modification, golden stick can be easier to enter animal tissue's organ, facilitate observation.
Table 2 is the potential change that front and back nanometer gold bar is modified through BSA
As can be seen from Table 2, the current potential of nanometer gold bar becomes -11.27mV from 22.6mV after BSA is modified.
The golden stick modified through BSA is exposed to mouse (as shown in Figure 3) by tail vein injection, it next can be according to normal
The blood sampling of Physiological Experiment means is advised, liver kidney is taken to be placed in the enrichment situation for observing material in gamma spectrometer.
Claims (10)
1. one kind is mixed59The preparation method of Fe nanometer gold bar, comprising the following steps:
1) by HAuCl4Solution is mixed with CTAB solution, and NaBH is added under stiring4, stop after being vigorously stirred, gold kind be prepared
Solution；
2) by AgNO3Solution and59FeCl3HCl is added in the mixed solution of CTAB and NaOL and stirs simultaneously, is then added
HAuCl4Solution is simultaneously vigorously stirred to colourless, is added concentrated hydrochloric acid and is adjusted pH to 1-2；
3) ascorbic acid is added in the solution after adjusting pH to step 2), is vigorously stirred mixing, is eventually adding golden kind of solution, stirring
Uniformly, the aged overnight at 25-30 DEG C, growth are mixed59Fe nanometer gold bar.
2. one kind as described in claim 1 is mixed59The preparation method of Fe nanometer gold bar, which is characterized in that step 3) further include by
What growth obtained mixes59It is washed 1-3 times after the centrifuge separation of Fe nanometer gold bar.
3. one kind as described in claim 1 is mixed59The preparation method of Fe nanometer gold bar, which is characterized in that gold described in step 1)
Kind solution is using preceding standing 30min or more.
4. one kind as described in claim 1 is mixed59The preparation method of Fe nanometer gold bar, which is characterized in that in step 1), CTAB is molten
Liquid, HAuCl4Solution and NaBH4Molar ratio be 2000: 5: 12.
5. one kind as described in claim 1 is mixed59The preparation method of Fe nanometer gold bar, which is characterized in that in step 2), mix molten
The molar ratio of CTAB and NaOL is 47: 1 to 69: 1 in liquid.
6. one kind as described in claim 1 is mixed59The preparation method of Fe nanometer gold bar, which is characterized in that in step 2), addition
AgNO3Molar concentration of the solution in the mixed solution of CTAB and NaOL is 0.48-0.9 μM.
7. one kind as described in claim 1 is mixed59The preparation method of Fe nanometer gold bar, which is characterized in that in step 2), be added
's59FeCl3The amount of HCl is 10-1000Bq.
8. one kind as described in claim 1 is mixed59The preparation method of Fe nanometer gold bar, which is characterized in that in step 3), often
The ascorbic acid being added in solution after 100mL step 2) adjusting pH is 0.32-0.48mmol, golden kind of the solution being then added
Amount is 80-160 μ L.
9. the preparation of the preparation method as described in claim 1-8 any one is mixed59Fe nanometer gold bar.
10. mixing as claimed in claim 959Fe nanometer gold bar, which is characterized in that59The radiation activity of Fe is 0.2-20Bq.
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Citations (6)
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| CN1380132A (en) * | 2002-03-22 | 2002-11-20 | 上海交通大学 | Liposome and inorganic material core-shell type nano composite particle and its preparation method and application |
| WO2013074822A1 (en) * | 2011-11-15 | 2013-05-23 | The Regents Of The University Of California | Templated synthesis of metal nanorods in silica nanotubes |
| CN103884693A (en) * | 2012-12-20 | 2014-06-25 | 江南大学 | Preparation method for monodispersed and low-biotoxicity gold nanorods, and use for detection of allergen |
| CN104117075A (en) * | 2014-07-30 | 2014-10-29 | 西安电子科技大学 | Gold nanorod multifunctional probe-based nuclide-cerenkov luminescence-CT multi-mode imaging method |
| CN105033276A (en) * | 2015-07-28 | 2015-11-11 | 同济大学 | Method for in situ synthesis of gold nanorods/graphene oxide composite material |
| CN105618730A (en) * | 2014-10-28 | 2016-06-01 | 深圳先进技术研究院 | Small-size gold nanorod and preparation method and applications thereof |
-
2017
- 2017-01-20 CN CN201710044927.9A patent/CN106862586B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1380132A (en) * | 2002-03-22 | 2002-11-20 | 上海交通大学 | Liposome and inorganic material core-shell type nano composite particle and its preparation method and application |
| WO2013074822A1 (en) * | 2011-11-15 | 2013-05-23 | The Regents Of The University Of California | Templated synthesis of metal nanorods in silica nanotubes |
| CN103884693A (en) * | 2012-12-20 | 2014-06-25 | 江南大学 | Preparation method for monodispersed and low-biotoxicity gold nanorods, and use for detection of allergen |
| CN104117075A (en) * | 2014-07-30 | 2014-10-29 | 西安电子科技大学 | Gold nanorod multifunctional probe-based nuclide-cerenkov luminescence-CT multi-mode imaging method |
| CN105618730A (en) * | 2014-10-28 | 2016-06-01 | 深圳先进技术研究院 | Small-size gold nanorod and preparation method and applications thereof |
| CN105033276A (en) * | 2015-07-28 | 2015-11-11 | 同济大学 | Method for in situ synthesis of gold nanorods/graphene oxide composite material |
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