CN113333772B - Preparation method of gold nanocluster and application of gold nanocluster in 2,4, 6-trinitrophenol detection - Google Patents

Preparation method of gold nanocluster and application of gold nanocluster in 2,4, 6-trinitrophenol detection Download PDF

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CN113333772B
CN113333772B CN202110682593.4A CN202110682593A CN113333772B CN 113333772 B CN113333772 B CN 113333772B CN 202110682593 A CN202110682593 A CN 202110682593A CN 113333772 B CN113333772 B CN 113333772B
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CN113333772A (en
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王勇
曾超
谢晨霞
张敏
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Nanchang University
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Abstract

The invention discloses a preparation method of a gold nanocluster and the gold nanocluster prepared by the method through a one-pot method by using isonicotinine as a stabilizer and citric acid-sodium citrate as a buffer solution. The invention discloses application of the gold nanocluster in 2,4, 6-trinitrophenol detection, when a high explosive (2, 4, 6-trinitrophenol) exists, the gold nanocluster can have an inner filtering effect with the gold nanocluster, so that fluorescence of the gold nanocluster is quenched, and the 2,4, 6-trinitrophenol can be sensitively and selectively detected on the basis. The gold nanocluster prepared by the method can be used as a high-efficiency and selective sensing 2,4, 6-trinitrophenol nano fluorescent probe.

Description

Preparation method of gold nanocluster and application of gold nanocluster in 2,4, 6-trinitrophenol detection
Technical Field
The invention belongs to the technical field of fluorescence sensing, and particularly relates to a preparation method of a gold nanocluster and application of the gold nanocluster in 2,4, 6-trinitrophenol detection.
Background
2,4, 6-Trinitrophenol (TNP) is named picric acid, which is widely used in industrial manufacturing, and the main application fields include medical research, rocket fuel, explosive manufacturing, leather dye manufacturing and the like, which make the Trinitrophenol (TNP) easily leaked into the ecological environment during the use process, while TNP is an environmental pollutant which pollutes soil along the way and rivers and lakes attached to the trinitrophenol, influences the survival of animals and plants, and further threatens the health of human beings. It is also a high explosive, and its explosive power is stronger than that of 2,4, 6-trinitrotoluene (TNT). Therefore, it is of great practical significance to develop a TNP detection method that is fast, highly sensitive, and easy to operate, in view of both environmental protection and social safety. According to the reports of relevant documents, the main traditional methods for detecting TNP include electrochemical method, raman spectroscopy, mass spectrometry, gas chromatography, liquid chromatography, fluorescence colorimetry and the like, all of which have characteristics of themselves, but are limited in laboratories, and most of them have fatal defects, such as low sensitivity, low selectivity, excessive dependence on large-scale instruments, slow detection speed, high cost and the like. With the rapid development of science and technology, the fluorescence method is favored by the majority of researchers by virtue of the advantages of high detection speed, good selectivity, high sensitivity, low cost and the like.
Metal nanoclusters are generally composed of several or even hundreds of atoms, the size of which is comparable to the fermi wavelength of an electron. The gold nanoclusters have unique molecular structures and excellent performance, are widely applied to the fields of luminescence, catalysis, cell imaging and the like, and are paid more and more attention by scientists. Researches show that most of gold nanoclusters are prepared from a ligand containing sulfydryl, and the preparation process is complicated and takes long time, so that a new and more convenient method needs to be established for synthesizing the gold nanoclusters.
Disclosure of Invention
Aiming at the defects and problems in the prior art, the invention aims to provide a preparation method of a gold nanocluster and application thereof in 2,4, 6-trinitrophenol detection.
The invention is realized by the following technical scheme:
the invention provides a preparation method of gold nanoclusters, which is used for preparing the gold nanoclusters by a one-pot method by taking chloroauric acid as a raw material, isonicotine as a stabilizer and citric acid-sodium citrate as a buffer solution, and comprises the following steps of:
s1, sequentially adding 20-120 parts by volume of 10mM chloroauric acid, 50-600 parts by volume of 40mM isonicotinite solution and 100-500 parts by volume of 20mM citric acid-sodium citrate solution into a container, wherein the pH value of the citric acid-sodium citrate solution is 3-7, adding a proper amount of distilled water, and uniformly mixing until the final volume is 1000 parts by volume;
and S2, carrying out ultrasonic treatment on the mixed solution prepared in the step S1 for 1min, and then putting the mixed solution into a water bath kettle at the temperature of 25-90 ℃ to heat for 0.5-2h to prepare the fluorescent gold nano-cluster solution.
Preferably, the chloroauric acid is used in an amount of 120 parts by volume in step S1; the using amount of the isonicotinic acid solution is 300 parts by volume; the dosage of the buffer solution is 100 parts by volume; the buffer solution had a pH of 6.
Preferably, the water bath heating temperature in the step S2 is 60 ℃; the reaction time was 1h.
The invention also provides application of the gold nanocluster as a nano fluorescent probe applied to 2,4, 6-trinitrophenol detection, wherein the application method comprises the following steps:
(1) Preparing a plurality of groups of detection solutions: adding 1980 parts by volume of distilled water into 10 parts by volume of the fluorescent gold nanocluster solution, mixing to form a detection solution, and preparing multiple groups by duplication;
(2) Mixing the detection solutions with 2,4, 6-trinitrophenol with different concentrations;
(3) Measuring the fluorescence emission spectrum of the mixed solution prepared in the step (2) at the excitation wavelength of 320 nm;
(4) According to the fluorescence intensity ratio F/F of the gold nanoclusters corresponding to TNP with different concentrations 0 To detect TNP, F and F 0 Fluorescence intensity of gold nanoclusters in the presence and absence of TNP, respectively.
Gold nanoclusterWhen the fluorescent nano-cluster is applied to TNP detection, the fluorescence intensity of the gold nano-cluster is gradually reduced along with the increase of the concentration of TNP, and the concentration of TNP and F/F 0 The kit has a good linear relation between 0.2 and 20 mu M, has a detection limit of 0.06 mu M, and can be used for high-sensitivity detection of TNP.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation of the gold nanocluster does not need harsh conditions, and is pollution-free and rapid.
(2) The gold nanocluster prepared by the method has high fluorescence property, good water solubility and good light stability, and can be used for high-sensitivity and selective detection of TNP.
Drawings
FIG. 1 is a three-dimensional fluorescence spectrum of gold nanoclusters of the present invention;
fig. 2 (a) is an ultraviolet-visible absorption spectrum of the gold nanoclusters, TNP and gold nanocluster + TNP, and fig. 2 (B) is an ultraviolet-visible absorption spectrum of TNP and excitation and emission spectra of the gold nanoclusters;
FIG. 3 is a graph of the fluorescence intensity of gold nanoclusters of the present invention as a function of different concentrations of TNP;
FIG. 4 is a selectivity plot of gold nanoclusters of the present invention.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
Example 1: preparation of gold nanoclusters
The gold nanoclusters are prepared by a one-pot method by using chloroauric acid as a raw material, isonicotin as a stabilizer and citric acid-sodium citrate as a buffer solution.
1. Optimization of preparation conditions: isonicotinine dosage, buffer solution pH, reaction temperature and time.
The result shows that the fluorescence intensity gradually increases with the increase of the dosage of the chloroauric acid and then tends to be balanced, and 120uL is optimal; the fluorescence intensity is gradually enhanced along with the increase of the dosage of the isonicotine and then tends to be balanced, and 300uL is optimal; when the citric acid-sodium citrate buffer solution is not added, the fluorescence intensity is almost zero, the fluorescence intensity is gradually enhanced along with the increase of the using amount of the citric acid-sodium citrate buffer solution and then gradually reduced, and the optimal 100uL is obtained; the fluorescence intensity gradually increases with the increase of the pH value and then decreases, and the pH value is optimal at 6; the fluorescence intensity gradually increases and then decreases with the increase of the reaction temperature, and the fluorescence intensity is optimal at 60 ℃; with increasing reaction time, the fluorescence gradually increases and then reaches equilibrium, 1h being optimal.
2. The gold nanoclusters were synthesized under optimal experimental conditions:
(1) A2 mL centrifuge tube was filled with 120. Mu.L of 10mM chloroauric acid, 300. Mu.L of 40mM isonicotinic acid solution, 100. Mu.L of 20mM citric acid buffer solution (pH 6), and distilled water to a final volume of 1mL.
(2) And (2) carrying out ultrasonic treatment on the solution obtained in the step (1) for 1min, and then placing the solution into a water bath kettle at the temperature of 60 ℃ for heating for 1h to obtain the fluorescent gold nanocluster solution.
The fluorescence property of the gold nanoclusters is inspected by a fluorescence spectrophotometer, and as can be seen from fig. 1, the synthesized gold nanoclusters can emit strong fluorescence under the excitation of 320nm, and the optimal emission wavelength is 430nm.
Example 2: interaction mechanism of gold nanoclusters and 2,4, 6-Trinitrophenol (TNP)
The interaction mechanism of the gold nanoclusters and TNP is characterized by using an ultraviolet visible-absorption spectrum and a fluorescence spectrum, and the result is shown in fig. 2.
As can be seen from fig. 2A, the experimental values of the gold nanoclusters and TNP ultraviolet absorption are almost identical to the theoretical values, which indicates that no new species are generated; as can be seen in fig. 2B, there is a large overlap between the uv-vis absorption of TNP and the excitation and emission wavelengths of the gold nanoclusters, indicating that an internal filtering effect occurs between the gold nanoclusters and TNP, resulting in fluorescence quenching.
Example 3: application of gold nanocluster to detection of 2,4, 6-Trinitrophenol (TNP)
Transferring 10 mu L of the fluorescent gold nanocluster solution prepared in the embodiment 1 into 1.98mL of distilled water, and sequentially and repeatedly preparing a plurality of groups of detection solutions; then 10uL of TNP with different concentrations were added to each set of detection solution, mixed uniformly, and the fluorescence emission spectrum at an excitation wavelength of 320nm was measured, and the result is shown in FIG. 3.
As can be seen from FIG. 3, as the concentration of TNP increases, the fluorescence emission peak of the gold nanoclusters is red-shifted, and the ratio of the fluorescence intensities (F/F) of the gold nanoclusters 0 F and F 0 The fluorescence intensity of the gold nanoclusters in the presence and absence of TNP) is gradually reduced, the concentration of TNP and F/F0 are in a good linear relation at 0.2-20 mu M, and the detection limit is 0.06 mu M.
Example 4: detection after addition of interferents
Substantially the same as in example 3, except that an interfering substance, which is a structural analogue of TNP (2, 4, 6-trinitrotoluene (TNT), phenol (PHE), 4-chlorotoluene, resorcinol, hydroquinone, resorcinol, phenol, nitrophenol, etc.) and possibly coexisting metal ions (Cr (III), cd (II), co (II), mn (II), pb (II), K (I), al (III), na (I), ca (II), zn (II), hg (II), ni (II), cu (II), etc.), was added to 2,4, 6-Trinitrophenol (TNP) at the same concentration, and then the fluorescence emission peak intensity at an excitation wavelength of 320nm was measured.
Calculating the ratio F/F of the gold nanocluster solution before and after the fluorescence peak after the interference substance is added 0 The results are shown in FIG. 4. The result shows that only 2,4, 6-trinitrophenol exists to enable the fluorescence of the gold nanocluster to be obviously quenched, and other structural analogs and metal ions can hardly enable the fluorescence intensity to be obviously reduced, which indicates that the substances can not interfere with the detection, and the technical scheme has good selectivity.
The foregoing description merely represents preferred embodiments of the present invention, which are described in some detail and detail, and should not be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, various changes, modifications and substitutions can be made without departing from the spirit of the present invention, and these are all within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.

Claims (6)

1. The preparation method of the gold nanocluster is characterized by comprising the following steps: the method comprises the steps of preparing gold nanoclusters by a one-pot method by using chloroauric acid as a raw material, isonicotin as a stabilizer and citric acid-sodium citrate as a buffer solution;
the method comprises the following steps:
s1, sequentially adding 20 to 120 volume parts of 10mM chloroauric acid, 50 to 600 volume parts of 40mM isonicotinic acid solution and 100 to 500 volume parts of 20mM citric acid-sodium citrate solution into a container, wherein the pH of the citric acid-sodium citrate solution is 3 to 7, and adding a proper amount of distilled water to uniformly mix until the final volume is 1000 volume parts;
and S2, carrying out ultrasonic treatment on the mixed solution prepared in the step S1 for 1min, and then putting the mixed solution into a water bath kettle at the temperature of 25-90 ℃ to heat for 0.5-2h to prepare the fluorescent gold nano-cluster solution.
2. The method for preparing gold nanoclusters according to claim 1, wherein: in the step S1, the volume of the chloroauric acid is 120 parts, the volume of the isonicotinic base solution is 300 parts, the volume of the citric acid-sodium citrate solution is 100 parts, and the pH value of the citric acid-sodium citrate solution is 6.
3. The method for preparing gold nanoclusters according to claim 1, wherein: in the step S2, the water bath temperature is 60 ℃, and the water bath reaction time is 1h.
4. Use of gold nanoclusters prepared by the method of any one of claims 1 to 3, characterized in that: the fluorogold nanocluster solution is used for detecting 2,4, 6-trinitrophenol.
5. The application according to claim 4, characterized in that the method of application comprises:
(1) Preparing a plurality of groups of detection solutions: adding 1980 parts by volume of distilled water into 10 parts by volume of the fluorescent gold nanocluster solution, mixing to form a detection solution, and repeating and preparing a plurality of groups;
(2) Mixing each group of detection solution with 2,4, 6-trinitrophenol with different concentrations uniformly;
(3) Measuring the fluorescence emission spectrum of the mixed solution prepared in the step (2) at the excitation wavelength of 320 nm;
(4) According to the fluorescence intensity ratio F/F of gold nano-clusters corresponding to different concentrations of 2,4, 6-trinitrophenol 0 Relationship between the two to detect 2,4, 6-trinitrophenol, F and F 0 The fluorescence intensity of the gold nanoclusters in the presence and absence of 2,4, 6-trinitrophenol, respectively.
6. Use according to claim 5, characterized in that: concentration of 2,4, 6-trinitrophenol and F/F of gold nanocluster 0 The linear relationship is formed in the range of 0.2-20 mu M, and the detection limit is 0.06 mu M.
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