CN113305297A - Laser-assisted seed-free gold nanorod synthesis method - Google Patents
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000001308 synthesis method Methods 0.000 title description 5
- 239000000243 solution Substances 0.000 claims abstract description 68
- 238000003756 stirring Methods 0.000 claims abstract description 25
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 14
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 13
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 12
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 101710134784 Agnoprotein Proteins 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- LOKCTEFSRHRXRJ-UHFFFAOYSA-I dipotassium trisodium dihydrogen phosphate hydrogen phosphate dichloride Chemical compound P(=O)(O)(O)[O-].[K+].P(=O)(O)([O-])[O-].[Na+].[Na+].[Cl-].[K+].[Cl-].[Na+] LOKCTEFSRHRXRJ-UHFFFAOYSA-I 0.000 claims abstract description 6
- 239000002953 phosphate buffered saline Substances 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 230000001678 irradiating effect Effects 0.000 claims abstract description 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 13
- 229910004042 HAuCl4 Inorganic materials 0.000 claims description 7
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000008363 phosphate buffer Substances 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 239000008188 pellet Substances 0.000 abstract description 3
- 206010028980 Neoplasm Diseases 0.000 description 5
- 239000010931 gold Substances 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000012377 drug delivery Methods 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 230000001404 mediated effect Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002872 contrast media Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 229940124447 delivery agent Drugs 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000007626 photothermal therapy Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
- 238000000479 surface-enhanced Raman spectrum Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
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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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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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Abstract
The invention discloses a preparation method of a laser-assisted seedless gold nanorod, which comprises the following steps: step A, adding AgNO into CTAB solution under the condition of slowly stirring at 60 DEG C3Aqueous solution, then HAuCl is added4A solution; step B, adding ascorbic acid solution under vigorous stirring, and adding NaBH after a certain time4Continuously and violently stirring the solution for a certain time, and then adjusting the stirring speed to be slow stirring; step C, irradiating the reaction solution by using pulse laser in the whole process of the step A and the step B; transferring the mixed solution after standing to an Eppendorf tube, and centrifuging to remove supernatant to obtain solution precipitate; resuspending the solution pellet in phosphate buffered saline to obtainAnd (4) gold nanorods.
Description
Technical Field
The invention relates to the technical field of nano material preparation. Specifically, the invention relates to a laser-assisted seed-free gold nanorod synthesis method.
Background
During the last decade, the field of gold nanomaterials has developed significantly. Anisotropic plasmonic gold nanoparticles have been the subject of much research due to their unique optical and electronic properties. For example, gold nano-materials have strong absorbance in the near infrared region, and the coupling efficiency is higher or the surface-enhanced raman spectrum signal is obviously enhanced. Among the different gold nanomaterials, the preparation of Gold Nanorods (GNRs) is of great interest. Longitudinal Surface Plasmon Resonance (LSPR) can be tuned by changing the aspect ratio of the gold nanorods. This unique plasmonic property makes GNRs ideal candidates for wide-ranging applications such as photothermal therapy, drug delivery, tumor detection, imaging, and sensing.
For example, GNRs are small in size but have a large surface area and therefore can be used to carry drugs and enhance the stability and solubility of drugs, and they can deliver unstable drugs to areas of the body that are otherwise inaccessible and become effective drug delivery agents. While GNRs have better absorption and scattering capabilities compared to other molecular species, so they can also be used for bio-imaging and for the production of new biomedical sensors and contrast agents. In addition, the GNR has the capacity of converting absorbed light into heat in a non-radiation process, so that the gold nanorods are enriched in the tumor by a certain method, the tumor is locally heated to kill tumor tissues under the irradiation of laser with specific wavelength, and surrounding normal tissues are not affected by the gold nanorods, so that the gold nanorods can be used for photo-thermal treatment of cancer.
At present, the preparation method of the gold nanorod mainly comprises electrochemical, photochemical, seed-mediated, template method and the like. The most common method is mainly a seed-mediated method, which is mainly divided into two steps: a first step of seed solution preparation; and secondly, growing the gold nanorods by using a seed solution.
Disclosure of Invention
The invention discloses a synthesis method of gold nanorods, which utilizes the assistance of pulse laser, does not need to prepare seed solution, shortens the synthesis of the gold nanorods into one step, and greatly improves the preparation efficiency.
According to one aspect of the present invention, there is provided a method for preparing a laser-assisted seedless gold nanorod, comprising:
step A, adding AgNO into CTAB solution under the condition of slowly stirring at 60 DEG C3Aqueous solution, then HAuCl is added4A solution;
step B, adding ascorbic acid solution under vigorous stirring, and adding NaBH after a certain time4Continuously and violently stirring the solution for a certain time, and then adjusting the stirring speed to be slow stirring;
step C, irradiating the reaction solution by using pulse laser in the whole process of the step A and the step B;
transferring the mixed solution after standing to an Eppendorf tube, and centrifuging to remove supernatant to obtain solution precipitate;
and (3) resuspending the solution precipitate in phosphate buffer saline to obtain the gold nanorods.
In one embodiment of the invention, the AgNO3The concentration of the aqueous solution is 0.01Mol/L, the concentration of the CTAB solution is 0.1Mol/L, and the HAuCl4The concentration of the solution is 0.01Mol/L, the concentration of the ascorbic acid is 0.1Mol/L, and the NaBH is added4The concentration of the solution was 0.02 Mol/L.
In one embodiment of the invention, the ratio of the amounts of the solutions is AgNO3:CTAB:HAuCl4Ascorbic acid NaBH4＝180:9500:500:55:4。
In one embodiment of the invention, the pulse length of the pulse laser is 7ns, the frequency is 1Hz, the wavelength is 808nm, and the laser irradiation area is 5cm2For 1 hour.
In one embodiment of the invention, in step A, 180. mu.L of 0.01M AgNO is added3The aqueous solution was added to 9.5mL of a CTAB solution with a concentration of 0.1M, and then 0.5mL of HAuCl with a concentration of 0.01M was added4A solution; in step B, 55. mu.L of 0.1M ascorbic acid solution was added, and 5s later 4. mu.L of 0.02M NaBH4The solution was stirred slowly after 30 seconds.
In one embodiment of the invention, the centrifugation speed is 8500rpm and lasts 15 minutes.
In one embodiment of the invention, the pH of the phosphate buffered saline is 7.4.
In one embodiment of the present invention, the preparation method does not require a step of preparing a seed solution.
The method disclosed by the embodiment of the invention does not need to prepare seed solution, and the gold nanorods are synthesized in one step, so that the method has the advantages of simplicity, convenience and quickness in operation.
Drawings
To further clarify the above and other advantages and features of embodiments of the present invention, a more particular description of embodiments of the invention will be rendered by reference to the appended drawings. It is appreciated that these drawings depict only typical embodiments of the invention and are therefore not to be considered limiting of its scope. In the drawings, the same or corresponding parts will be denoted by the same or similar reference numerals for clarity.
Fig. 1 illustrates a method of preparing a laser assisted seedless gold nanorod composite according to one embodiment of the invention.
FIG. 2 shows a TEM image of a gold nanorod formed by an embodiment of the present invention.
FIG. 3 shows a UV-Vis spectrum of a gold nanorod solution formed by an embodiment of the invention.
Detailed Description
In the following description, the invention is described with reference to various embodiments. One skilled in the relevant art will recognize, however, that the embodiments may be practiced without one or more of the specific details, or with other alternative and/or additional methods, materials, or components. In other instances, well-known structures, materials, or operations are not shown or described in detail to avoid obscuring aspects of embodiments of the invention. Similarly, for purposes of explanation, specific numbers, materials and configurations are set forth in order to provide a thorough understanding of the embodiments of the invention. However, the invention may be practiced without specific details. Further, it should be understood that the embodiments shown in the figures are illustrative representations and are not necessarily drawn to scale.
Reference in the specification to "one embodiment" or "the embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment.
In the embodiment of the invention, the laser-assisted seedless gold nanorod synthesis method is disclosed, and the synthesis of the gold nanorods is shortened into one step by using the assistance of pulse laser without preparing a seed solution, so that the preparation efficiency is greatly improved.
Fig. 1 shows a flow diagram of a method for preparing laser-assisted seedless gold nanorods, according to one embodiment of the invention.
As shown in fig. 1, first, in step 101, a solution is mixed. AgNO is slowly stirred in a water bath at 60 DEG C3The aqueous solution was added to CTAB solution, followed by HAuCl4And (3) solution. Wherein the stirring speed of the slow stirring is not higher than 600 rpm. In one embodiment of the invention, the AgNO3The concentration of the aqueous solution is 0.01Mol/L, the concentration of the CTAB solution is 0.1Mol/L, and the HAuCl4The concentration of the solution was 0.01 Mol/L.
Next, at step 102, under vigorous stirring, ascorbic acid solution is added and after a specified time NaBH is added4The solution is stirred vigorously for a certain time, and then the stirring speed is adjusted to be slow. Wherein the stirring speed of the vigorous stirring is not less than 1000 rpm. In one embodiment of the invention, the concentration of the ascorbic acid is 0.1Mol/L, and the NaBH is4The concentration of the solution was 0.02 Mol/L.
In yet another embodiment of the present invention, the ratio of the amounts of the solutions is AgNO3:CTAB:HAuCl4:AA:NaBH4＝180:9500:500:55:4。
In step 103, the reaction solution is irradiated with a pulsed laser throughout the reaction of steps 101 and 102.
In one embodiment of the invention, the pulsesThe pulse length of the laser is 7ns, the frequency is 1Hz, the wavelength is 808nm, and the laser irradiation area is 5cm2For 1 hour. The pulsed laser is Nd-YAG pump Optical Parametric Oscillator (OPO) laser (Quantel Brilliant B with Rainbow OPO, Les Ulis France).
Next, at step 104, a precipitate is obtained. The mixed solution was transferred to an Eppendorf tube and centrifuged, and then the supernatant was removed to obtain a solution precipitate. In one embodiment of the invention, the centrifugation speed is 8500rpm for 15 minutes; and
finally, at step 105, gold nanorods are obtained and stored. Resuspending the solution precipitate in phosphate buffer saline to obtain gold nanorods; in one embodiment of the invention, the solution pellet is resuspended in 10ml of phosphate buffered saline at pH 7.4. In one embodiment of the present invention, the prepared gold nanorod solution may be stored in a refrigerator at 4 ℃.
Next, gold nanorods formed by the method disclosed in the embodiments of the present invention were studied by using ultraviolet-visible light (UV-Vis) absorption spectroscopy and TEM transmission electron microscopy.
Example 1
Under slow stirring in a 60 ℃ water bath, 180. mu.L of 0.01M AgNO was added3The aqueous solution was added to 9.5mL of a 0.1M CTAB solution. Then, 0.5mL of 0.01M HAuCl was added4And (3) solution. While stirring vigorously, 55. mu.L of 0.1M Ascorbic Acid (AA) solution was added, and after 5s 4. mu.L of 0.02M NaBH4And (3) solution. After 30s, the stirring speed was adjusted to slow stirring. During the whole reaction process, the reaction solution was irradiated with pulsed laser for 1 hour.
After one hour, the solution was transferred to an Eppendorf tube and centrifuged at 8500rpm for 15 minutes. The supernatant was then removed and the pellet resuspended in 10mL Phosphate Buffered Saline (PBS) (pH 7.4). And (4) storing the gold nanorod solution in a refrigerator at 4 ℃.
FIG. 2 shows a TEM image of a gold nanorod formed by an embodiment of the present invention. As can be seen from FIG. 2, the formed gold nanorods have stable structure and uniform size.
FIG. 3 shows a UV-Vis spectrum of a gold nanorod solution formed by an embodiment of the invention. As can be seen from FIG. 3, the absorbance peak of the solution appears at the wavelength of 526nm and 808nm, 526nm corresponds to the longitudinal absorption peak of the gold nanorod, and 808nm corresponds to the transverse absorption peak of the gold nanorod, thereby verifying the effectiveness of the embodiment of the invention.
While various embodiments of the present invention have been described above, it should be understood that they have been presented by way of example only, and not limitation. It will be apparent to persons skilled in the relevant art that various combinations, modifications, and changes can be made thereto without departing from the spirit and scope of the invention. Thus, the breadth and scope of the present invention disclosed herein should not be limited by any of the above-described exemplary embodiments, but should be defined only in accordance with the following claims and their equivalents.
Claims (8)
1. A preparation method of a laser-assisted seedless gold nanorod comprises the following steps:
step A, adding AgNO into CTAB solution under the condition of slowly stirring at 60 DEG C3Aqueous solution, then HAuCl is added4A solution;
step B, adding ascorbic acid solution under vigorous stirring, and adding NaBH after a certain time4Continuously and violently stirring the solution for a certain time, and then adjusting the stirring speed to be slow stirring;
step C, irradiating the reaction solution by using pulse laser in the whole process of the step A and the step B;
transferring the mixed solution after standing to an Eppendorf tube, and centrifuging to remove supernatant to obtain solution precipitate;
and (3) resuspending the solution precipitate in phosphate buffer saline to obtain the gold nanorods.
2. The method of preparing laser-assisted seedless gold nanorods according to claim 1, wherein the AgNO is3The concentration of the aqueous solution is 0.01Mol/L, the concentration of the CTAB solution is 0.1Mol/L, and the HAuCl4The concentration of the solution is 0.01Mol/L, the concentration of the ascorbic acid is 0.1Mol/L, and the NaBH is added4The concentration of the solution was 0.02 Mol/L.
3. The method of claim 2, wherein the ratio of the amount of each solution is AgNO3:CTAB:HAuCl4Ascorbic acid NaBH4＝180:9500:500:55:4。
4. The method for preparing laser-assisted seedless gold nanorods according to claim 1, wherein the pulse laser has a pulse length of 7ns, a frequency of 1Hz, a wavelength of 808nm, and a laser irradiation area of 5cm2For 1 hour.
5. The method for preparing laser-assisted seedless gold nanorods according to claim 1, wherein in step A, 180. mu.L of 0.01M AgNO at a concentration3The aqueous solution was added to 9.5mL of a CTAB solution with a concentration of 0.1M, and then 0.5mL of HAuCl with a concentration of 0.01M was added4A solution; in step B, 55. mu.L of 0.1M ascorbic acid solution was added, and 5s later 4. mu.L of 0.02M NaBH4The solution was stirred slowly after 30 seconds.
6. The method for preparing laser-assisted seedless gold nanorods according to claim 1, wherein the centrifugation rotation speed is 8500rpm and lasts 15 minutes.
7. The method of preparing laser-assisted seedless gold nanorods according to claim 1, wherein the phosphate buffered saline has a pH of 7.4.
8. The method of preparing laser-assisted seedless gold nanorods according to claim 1, wherein the preparation method does not require a step of preparing a seed solution.
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