CN110885678B - Gold nanocluster self-assembly and preparation method thereof and luminescent material - Google Patents
Gold nanocluster self-assembly and preparation method thereof and luminescent material Download PDFInfo
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- CN110885678B CN110885678B CN201910916080.8A CN201910916080A CN110885678B CN 110885678 B CN110885678 B CN 110885678B CN 201910916080 A CN201910916080 A CN 201910916080A CN 110885678 B CN110885678 B CN 110885678B
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/58—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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Abstract
The invention provides a gold nanocluster self-assembly, which comprises a first construction unit and a second construction unit, and is characterized in that the first construction unit is a gold nanocluster protected by a mercaptan ligand, and the second construction unit is a supermolecule macrocycle. The red luminescence of the gold nanoclusters is enhanced by supramolecular self-assemblies.
Description
Technical Field
The invention relates to the technical field of luminescence, in particular to a gold nanocluster self-assembly body, a preparation method of the gold nanocluster self-assembly body and a luminescent material.
Background
In recent years, fluorescent gold nanoclusters as a novel metal nanomaterial have attracted much attention due to the advantages of low toxicity, easy preparation, high fluorescence yield, strong optical stability, excellent biocompatibility and the like.
Gold nanoclusters generally have an ultra-small diameter size below 3nm, and mercaptide ligand protected Au nanoclusters (SR-AuNCs) are generally the ideal choice for bioimaging due to their good biocompatibility, solubility and optical properties. However, their relatively low luminescence quantum yield (QY, most reported AuNCs at room temperature is less than 15%) presents a non-negligible obstacle to practical application compared to Quantum Dots (QDs) and organic dyes.
At present, reports of QY exceeding 15%, especially in aqueous solutions, are still rare.
Therefore, a new gold nanocluster self-assembly is needed to overcome the above-mentioned drawbacks of the existing gold nanocluster materials.
Disclosure of Invention
The invention aims to provide a gold nanocluster self-assembly, which is based on self-assembly of host and guest between supermolecule macrocycle and thiol ligand protected gold nanoclusters (FGGC-AuNCs), and enhances red luminescence of the gold nanoclusters through supermolecule self-assembly.
In order to achieve the above object, the present invention provides a gold nanocluster self-assembly, comprising a first building unit and a second building unit, wherein the first building unit is a thiol ligand protected gold nanocluster, and the second building unit is a supramolecular macrocycle.
In one embodiment of the invention, the thiol ligand is a polypeptide.
In one embodiment of the invention, the polypeptide is phenylalanine-glycine-cysteine (FGGC).
In an embodiment of the present invention, the first building element is Au 22 (FGGC) 18 。
In one embodiment of the invention, the supramolecular macrocycle is at least one of cyclodextrin, pillararene, calixarene or cucurbit [ n ] urea.
In an embodiment of the present invention, the gold nanocluster self-assembly is a host-guest inclusion complex, wherein the first building unit is a guest and the second building unit is a host.
In one embodiment of the present invention, the gold nanocluster self-assembly is FGGC-AuNCs @ CB [7 ].
The invention also provides a luminescent material, which comprises the gold nanocluster self-assembly body.
The invention also provides a preparation method of the gold nanocluster self-assembly, which takes the supermolecule macrocycle as a main body and the gold nanocluster protected by the mercaptan ligand as an object, and the gold nanocluster self-assembly is formed by wrapping and connecting the gold nanocluster protected by the mercaptan ligand and the main object of the supermolecule macrocycle in an autonomous manner.
In an embodiment of the present invention, the preparation method includes: a step of forming thiol ligand-protected gold nanoclusters; and a step of forming a gold nanocluster self-assembly; in the step of forming the thiol ligand protected gold nanoclusters, polypeptide is used as a thiol ligand, tetrachloroauric acid is mixed with an aqueous solution of the thiol ligand, the pH value is adjusted to 11-12, then an aqueous solution of sodium borohydride is slowly added until the color of the solution becomes orange red, acid is added to quench the sodium borohydride, the reaction is carried out at room temperature until the reaction is complete, and the thiol ligand protected gold nanoclusters are obtained after purification.
In one embodiment of the present invention, in the step of forming thiol ligand protected gold nanoclusters, an acid is added to the system to adjust the pH to 2.5 to quench the sodium borohydride.
In one embodiment of the present invention, in the step of forming thiol ligand-protected gold nanoclusters, the purification is performed by thin layer chromatography.
In a preferred embodiment of the present invention, a method for preparing the gold nanocluster self-assembly is provided, which includes the following steps:
(1) step of Forming thiol ligand-protected gold nanoclusters
Mixing tetrachloroauric acid with an aqueous solution of a thiol ligand by taking polypeptide as the thiol ligand, adjusting the pH value to 11-12, slowly adding an aqueous solution of sodium borohydride until the color of the solution becomes orange red, adding acid to enable the pH value of the system to be 2.5 to quench sodium borohydride, reacting at room temperature until the solution is complete, and purifying by using a thin-layer chromatography to obtain gold nanoclusters (FGGC-AuNCs) protected by the thiol ligand; and the number of the first and second groups,
(2) step of Forming gold nanocluster self-Assembly
And (2) adding the gold nanoclusters protected by the mercaptan ligand obtained in the step (1) into the supermolecule macrocycle to obtain the gold nanocluster self-assembly with high emission efficiency.
In the invention, based on self-assembly of host and object between supermolecule macrocycle and thiol ligand protected gold nanoclusters (FGGC-AuNCs), red luminescence of the gold nanoclusters is enhanced through supermolecule self-assembly effect. Because the supermolecule macrocycle and the FGGC-AuNCs are combined under various non-covalent interactions, so that a stable host-guest complex is obtained, and the supermolecule macrocycle forms a firm 'outer wall' on the gold nanoclusters. Meanwhile, the limited domain formed between the supermolecule large rings effectively inhibits the rotation and vibration of the ligand on the surface of the gold nanocluster. Therefore, when the FGGC-AuNCs and the supermolecule macrocycle are assembled in the aqueous solution at room temperature, the red luminescence of the FGGC-AuNCs can be obviously enhanced by the self-assembly method, and the gold nanoclusters with ultrahigh fluorescence quantum yield are obtained.
In contrast, the fluorescence quantum yield of a normal gold nanocluster without binding of supramolecular macrocycles by host-guest interactions is only 8%. The invention forms the gold nanocluster with ultrahigh quantum efficiency by self-assembly of the host and the guest between the supermolecule macrocycle and the FGGC-AuNCs, and can provide practical application for living cell imaging.
It is noted that the self-assembly structure of the present invention also has great potential, and provides a new idea for exploring the light emitting mechanism of gold nanoclusters and for alternative methods for adjusting other important properties of gold nanoclusters (such as energy and electron transfer, catalysis, etc.).
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 shows Au nanoclusters according to an embodiment of the present invention 22 (FGGC) 18 Mass spectrogram of (1);
FIG. 2A and FIG. 2B are Au nanoclusters according to an embodiment of the present invention 22 (FGGC) 18 Ultraviolet absorption spectrum and fluorescence emission spectrum.
FIG. 3 shows gold nanoparticles of example 2 of the present inventionCluster Au 22 (FGGC) 18 Adding CB [7]]The fluorescence intensity and quantum yield are enhanced.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
The following disclosure provides many different embodiments or examples for implementing different features of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. Moreover, the present invention may repeat reference numerals and/or reference letters in the various examples, which have been repeated for purposes of simplicity and clarity and do not in themselves dictate a relationship between the various embodiments and/or configurations discussed. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art may recognize applications of other processes and/or uses of other materials.
Host-guest self-assembly, as used herein, is generally defined as the encapsulation behavior between small motifs (organic molecules or ions) with specific molecular structures and macrocyclic molecules such as Cyclodextrins (CD), pillararylenes, calixarenes, and cucurbit [ n ] ureas. The application of host-guest assembly is widely ranging from single-molecule materials to bulk materials, but there is little research on developing materials based on supramolecular interactions between supramolecular macrocycles and ultra-small nanoclusters. Therefore, it is crucial to develop an efficient and easy method to improve the light emitting efficiency of gold nanoclusters in an aqueous solution at room temperature through host-guest action.
In this embodiment, a gold nanocluster self-assembly is provided. The gold nanocluster self-assembly includes a supramolecular macrocycle as a subject, and a thiol ligand-protected gold nanocluster (Au) as a guest 22 (FGGC) 18 ) (ii) a Such as, but not limited to, cyclodextrins, pillararenes, calixarenes, or cucurbit [ n [ ]]Urea. In this embodiment, the gold nanocluster self-assembly is a host-guest inclusion complex, and is formed by FGGC-supramolecular macrocyclic host-guest inclusion self-assembly connection.
In this embodiment, the preparation process of the gold nanocluster self-assembly is as follows:
the preparation method specifically comprises the following steps:
(1) formation of thiol ligand protected gold nanoclusters (Au) 22 (FGGC) 18 ) Step (2) of
Quickly weighing 25mg of polypeptide phenylalanine-glycine-cysteine (FGGC) in a 5ml weighing bottle, weighing 3mg of sodium borohydride in a 20ml weighing bottle, adding 20ml of water to prepare a sodium borohydride solution, and transferring 50 mul of HAuCl by using a 100 mul liquid transferring gun 4 Putting the solution into a 50ml round-bottom flask, adding 2ml of deionized water, then placing the round-bottom flask on a magnetic stirring table for stirring, adding 1ml of deionized water into a weighing bottle containing FGGC, shaking uniformly, quickly dissolving FGGC, quickly sucking the solution into the round-bottom flask by using a disposable dropper, finding that the solution is changed from yellow to colorless, continuously adding 22ml of deionized water into the round-bottom flask, and after vigorously stirring for 1 minute, adjusting the pH of the reaction solution to 11-12 by using a 1M NaOH aqueous solution. After stirring for 2 minutes, the addition of sodium borohydride solution was started. And (3) sucking 25ul of sodium borohydride solution each time, dropwise adding the sodium borohydride solution into the round-bottom flask in a small amount for multiple times, controlling the time to be 25ul of sodium borohydride solution every 1-2 minutes, completing dropwise adding about half an hour, and changing the solution from colorless to orange-red after dropwise adding into the round-bottom flask, namely finishing the dropwise adding. Thereafter, the remaining NaBH is quenched by adjusting the pH to 2.5 by addition of 1M HCl 4 This process has a color change from orange-red to brown-green. The reaction solution was then stirred at room temperature at 400rpm/min for 12 hours to form an orange-red AuNCs solution. Orange-red colour formedThe mass spectrum characterization of AuNCs is shown in figure 1, and the structural formula of the gold nanocluster protected by the primarily obtained thiol ligand is Au 22 (FGGC) 18 。
Then, the gold nanocluster Au obtained by the reaction is subjected to reaction 22 (FGGC) 18 The solution is divided into 6 ultrafiltration centrifugal filter tubes (4mL, 10KD), centrifuged in a centrifuge at 9000rpm/min for 10min, the liquid in the centrifuge tubes is taken out by a disposable pipette and filled in a 5mL weighing bottle to prepare a classical developing solvent, and the ratio of the developing solvent to the organic phase of n-butanol/water/acetic acid is 4: 1: 5, Rf about 0.3, and separating the centrifuged gold nanocluster solution by thin layer chromatography (PTLC) to obtain purified Au 22 (FGGC) 18 And (3) solution.
For the gold nanocluster Au obtained in the step 22 (FGGC) 18 Detecting to obtain the ultraviolet-visible absorption spectrogram and the fluorescence emission spectrogram shown in fig. 2A and fig. 2B. As can be seen from FIG. 2, the gold nanoclusters Au are shown in this step 22 (FGGC) 18 Has an absorption peak at 515nm and an emission peak at 660 nm.
(2) Step of forming gold nanocluster self-assembly (FGGC-AuNCs @ CB [7])
The gold nanoclusters Au obtained after purification are orange red 22 (FGGC) 18 Adding calabash [ n ]]Urea (CB [7]]) Thus obtaining the gold nanocluster self-assembly (FGGC-AuNCs @ CB [7]) with high-efficiency emission efficiency]). FIG. 3 shows different CB [7]]Gold nanocluster self-assembly (FGGC-AuNCs @ CB [7]) obtained under concentration adding condition]) Fluorescence intensity and quantum yield enhancement profile of (a). As shown in FIG. 3, with the addition of CB [7]]Increase in concentration of gold nanoclusters of Au 22 (FGGC) 18 The emission intensity and the quantum yield of the quantum well are continuously enhanced as shown in figure 3. And the 0 point in the horizontal axis direction in fig. 3 is the fluorescence quantum yield of the gold nanocluster without the host-guest interaction combined with the supramolecular macrocycle in the prior art, and the fluorescence quantum yield is only 8%. The gold nanocluster self-assembly (FGGC-AuNCs @ CB [7]) of the present invention]) The gold nanocluster with ultrahigh quantum efficiency is formed by self-assembly of host and guest between supermolecule macrocycle and FGGC-AuNCs, the fluorescence quantum yield reaches 51 percent, and the gold nanocluster can be aliveCellular imaging provides practical applications.
The present invention has been described in relation to the above embodiments, which are only exemplary of the implementation of the present invention. It must be noted that the disclosed embodiments do not limit the scope of the invention. Rather, modifications and equivalent arrangements included within the spirit and scope of the claims are included within the scope of the invention.
Claims (6)
1. A gold nanocluster self-assembly comprises a first construction unit and a second construction unit, and is characterized in that the first construction unit is a gold nanocluster protected by a thiol ligand, and the second construction unit is a supermolecule macrocycle;
the gold nanocluster self-assembly body is a host-guest inclusion complex, wherein the first construction unit is a guest, the second construction unit is a host, and the gold nanoclusters protected by the thiol ligand are in inclusion self-assembly connection with the host-guest inclusion complex of the supermolecule macrocycle to form the gold nanocluster self-assembly body;
the thiol ligand is a polypeptide; the polypeptide is phenylalanine-glycine-cysteine;
the supermolecule macrocycle is at least one of cyclodextrin, pillared aromatic hydrocarbon, calixarene or cucurbit [ n ] urea.
2. A light emitting material comprising the gold nanocluster self assembly of claim 1.
3. The method for preparing the gold nanocluster self-assembly according to claim 1, wherein the method comprises the steps of taking a supermolecular macrocycle as a main body, taking the gold nanocluster protected by a thiol ligand as an object, and carrying out inclusion self-assembly connection on the gold nanocluster protected by the thiol ligand and the main object of the supermolecular macrocycle to form the gold nanocluster self-assembly.
4. The method of preparing a gold nanocluster self assembly of claim 3, wherein the method of preparing comprises:
a step of forming thiol ligand-protected gold nanoclusters, and,
forming a gold nanocluster self-assembly; wherein, the first and the second end of the pipe are connected with each other,
in the step of forming the gold nanocluster protected by the thiol ligand, polypeptide is used as the thiol ligand, tetrachloroauric acid is mixed with the aqueous solution of the hydrophobic ligand, the pH value is adjusted to 11-12, then the aqueous solution of sodium borohydride is slowly added until the color of the solution becomes orange red, acid is added to quench the sodium borohydride, the reaction is carried out at room temperature until the reaction is complete, and the gold nanocluster protected by the thiol ligand is obtained after purification.
5. The method of preparing a gold nanocluster self assembly as recited in claim 4, wherein in the step of forming thiol ligand protected gold nanoclusters, an acid is added to the system to adjust the pH to 2.5 to quench the sodium borohydride.
6. The method of preparing gold nanocluster self-assembly as claimed in claim 4, wherein in the step of forming thiol ligand protected gold nanoclusters, purification is performed by thin layer chromatography.
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CN114085666B (en) * | 2021-12-14 | 2023-09-08 | 安徽大学 | Preparation method of oligopeptide-protected gold cluster assembly material and application of oligopeptide-protected gold cluster assembly material in detection of ferric ions |
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