CN113523296B - Preparation method of gold-lead fluorescent nano-cluster and application of gold-lead fluorescent nano-cluster in sodium-dependent detection - Google Patents
Preparation method of gold-lead fluorescent nano-cluster and application of gold-lead fluorescent nano-cluster in sodium-dependent detection Download PDFInfo
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Abstract
The invention discloses a preparation method of gold-lead nanoclusters, which belongs to the technical field of fluorescence sensing and is characterized in that the gold-lead nanoclusters are prepared by a one-step method by taking chloroauric acid as a raw material, adenosine as a stabilizer, ascorbic acid as a reducing agent and lead acetate as a doping agent. The gold-lead nanocluster prepared by the invention is formed based on an aggregation-induced fluorescence enhancement principle, and has the advantages of good fluorescence property, good water solubility, high fluorescence quantum yield and the like. The invention also discloses application of the gold-lead nano-cluster in sodium-dependent detection, and when sodium-dependent exists in the solution, the gathered gold-lead nano-cluster can be dispersed, so that the fluorescence of the gold-lead nano-cluster is quenched. With the increase of the concentration of the sodium metiram, the fluorescence intensity of the gold-lead nano cluster is gradually reduced, and the ultra-sensitive and selective detection of the sodium metiram is realized.
Description
Technical Field
The invention belongs to the technical field of fluorescence sensing, and particularly relates to a preparation method of a gold-lead fluorescence nano-cluster and application of the gold-lead fluorescence nano-cluster in sodium metiram detection.
Background
The sodium metiram belongs to dithiocarbamate bactericides, has the characteristics of low price, high efficiency, broad spectrum and the like, and is widely used for preventing and treating plant diseases and insect pests in agricultural production. However, since metabolites of such pesticides are very harmful to the environment and human body, there is a strong need for a method for detecting such pesticides. At present, methods for detecting sodium metiram mainly comprise liquid chromatography, liquid chromatography tandem mass spectrometry, gas chromatography tandem mass spectrometry and the like, but the methods usually require large expensive instruments and equipment, are complicated and time-consuming in operation process, and require professional personnel to operate, so that the use is limited. The fluorescence sensing technology has the advantages of simple operation, high sensitivity, low cost, high analysis speed and the like, so the development of the sodium metiram fluorescence sensing analysis method has important significance in an environment monitoring method.
In recent years, metal nanoclusters such as gold, silver, and copper nanoclusters have received great attention due to excellent physical, optical, and electrical properties, and also exhibit wide application prospects in many fields such as catalysis, sensing, cell imaging, and drug delivery. Currently, much research has been focused on the research of gold and silver nanoclusters, and little has been done on gold and lead nanoclusters. However, a report that a gold-lead nano cluster is quickly and environmentally synthesized based on a phenomenon that aggregation-induced fluorescence enhancement occurs after lead ions are added and sodium metiram is detected based on the synthesized gold-lead nano cluster is not yet found.
Disclosure of Invention
Aiming at the defects and difficulties in the prior art, the invention aims to provide a preparation method of a gold-lead fluorescent nano-cluster and application thereof in sodium-metiram detection, and the preparation method has the advantages of high sensitivity, rapidness and good selectivity in detection.
The invention is realized by the following technical scheme:
the invention provides a preparation method of a gold-lead fluorescent nano-cluster, which takes chloroauric acid as a raw material, adenosine as a stabilizer, ascorbic acid as a reducing agent and lead acetate as a doping agent to prepare the gold-lead nano-cluster by a one-step method, and comprises the following steps:
s1, sequentially adding 20-140 parts by volume of 10mM chloroauric acid, 20-120 parts by volume of 10mM lead acetate, 40-360 parts by volume of 25mM adenosine, 50 parts by volume of 20mM citric acid-sodium citrate buffer solution and 20-120 parts by volume of 10mM ascorbic acid into a container, wherein the pH of the buffer solution is 3-8, and adding a proper amount of ultrapure water to uniformly mix, wherein the final volume is 1000 parts by volume;
and S2, reacting the mixed solution obtained in the step S1 at 25-90 ℃ for 0-6h, centrifuging for 15min at 12500rpm/min, taking the lower-layer precipitate, and dissolving in water to obtain the gold-lead nanoclusters.
Preferably, the chloroauric acid is used in an amount of 80 parts by volume in step S1; the using amount of the lead acetate is 80 parts by volume; the dosage of adenosine is 280 volume parts; the pH of the buffer solution is 5; the using amount of the ascorbic acid is 70 parts by volume; the reaction temperature in the step S2 is 60 ℃; the reaction time was 1h.
The invention also provides application of the gold-lead fluorescent nano-cluster, and the gold-lead nano-cluster is used for detecting sodium metiram.
The specific application method comprises the following steps:
(1) Adding 10 parts by volume of gold-lead nanocluster solution into 1980 parts by volume of acetic acid-sodium acetate diluted buffer solution, mixing to form detection solution, and repeating for preparing multiple groups;
(2) Mixing the detection solutions with sodium metiram solutions with different concentrations, and reacting at room temperature for 3min;
(3) Measuring the fluorescence emission spectrum of the solution with the excitation wavelength of 300nm for the mixed solution prepared in the step (2);
(4) According to the fluorescence intensity ratio F/F of the gold-lead nano cluster corresponding to sodium metiram with different concentrations at 510nm 0 Relationship between them to detect sodium, F and F 0 The fluorescence intensity of the gold nanoclusters in the presence and absence of sodium metiram, respectively.
With the increase of the concentration of sodium metiram, the fluorescence intensity of the gold-lead nano cluster at 510nm is gradually weakened, and the ratio (F) of the concentration of sodium metiram to the fluorescence intensity of the gold-lead nano cluster 0 [ solution ] F, F and F 0 Respectively, the fluorescence intensity with or without the sodium-metiram) is in good linear relation in the range of 0.1nM-30nM, the detection limit is 30pM, and the method can be used for the ultra-sensitive detection of the sodium-metiram.
Preferably, the concentration of the acetic acid-sodium acetate diluted buffer solution is 10mM, and the pH value is 6.
Compared with the prior art, the invention has the beneficial effects that:
(1) The method takes adenosine as a stabilizing agent, citric acid-sodium citrate as a buffer solution, ascorbic acid as a reducing agent and lead acetate as a doping agent, and synthesizes the gold-lead nano-cluster in one step based on the principle of aggregation-induced fluorescence enhancement, wherein the gold-lead nano-cluster has water solubility, high fluorescence quantum yield and good light stability.
(2) The gold-lead nano-cluster constructed sensor prepared by the invention is used for sodium-metiram ultra-sensitive detection and has the advantages of high sensitivity, rapidness and good selectivity in detection.
Drawings
FIG. 1 is an ultraviolet-visible absorption spectrum of gold-lead nanoclusters of the present invention;
FIG. 2 is an excitation and emission fluorescence spectrum of gold-lead nanoclusters of the present invention;
FIG. 3 is a transmission electron microscope image of gold-lead nanoclusters of the present invention;
FIG. 4A is the emission spectrum of Au-Pb nanoclusters with sodium metiram of different concentrations; FIG. 4B shows a view of the present invention F 0 A linear plot of/F vs. sodium;
FIG. 5 is a diagram showing the selectivity of gold-lead nanoclusters of the present invention.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
Example 1 preparation of gold-lead nanoclusters
The method takes chloroauric acid as a raw material, adenosine as a stabilizer, ascorbic acid as a reducing agent and lead acetate as a doping agent to prepare the gold-lead nanoclusters by a one-step method.
(1) Optimizing the dosage of the chloroauric acid, the lead acetate, the adenosine and the ascorbic acid, the pH value of the citric acid-sodium citrate buffer solution, the reaction temperature and the reaction time.
The result shows that the fluorescence is gradually enhanced and then gradually balanced with the increase of the dosage of the chloroauric acid, and the optimal dosage is 80 mu L; with the increase of the dosage of the lead acetate, the fluorescence is gradually enhanced and then gradually balanced, and the optimal dosage is 80 mu L; with the increase of the dosage of adenosine, the fluorescence is gradually enhanced and then gradually balanced, and the optimal dosage is 280 mu L; the citric acid-sodium citrate buffer solution has weak fluorescence under the condition of pH 3, and has strong fluorescence under the condition of other pH, and the optimal pH is 5; with the increase of the dosage of the ascorbic acid, the fluorescence is firstly enhanced and then weakened, and the optimal dosage is 70 mu L; with the increase of the reaction temperature, the fluorescence is firstly enhanced and then gradually weakened, and the optimal reaction temperature is 60 ℃; as the reaction time increases, the fluorescence first increases and then gradually equilibrates, with the optimal reaction time being 1h.
(2) Preparing gold-lead nanoclusters under the optimal conditions: 80 mu L of 10mM chloroauric acid, 80 mu L of 10mM lead acetate, 280 mu L of 25mM adenosine, 50uL of 20mM citric acid-sodium citrate buffer solution, pH 5, 70 mu L of 10mM ascorbic acid and finally adding a proper amount of ultrapure water to ensure that the total volume is 1mL, uniformly mixing, reacting at 60 ℃ for 1h, centrifuging for 15min at 12500rpm/min, taking the lower-layer precipitate and dissolving in water to obtain the gold-lead nanoclusters.
FIG. 1 is an ultraviolet-visible absorption spectrum of gold-lead nanoclusters, and an absorption peak at 300nm indicates that the gold-lead nanoclusters are formed. As shown in the excitation and emission fluorescence spectrograms of the gold-lead nanoclusters in FIG. 2, under the excitation of 300nm, the emission wavelength is 510nm, and meanwhile, bright green fluorescence can be seen from the photo graphs, which proves that the gold-lead nanoclusters of green fluorescence are synthesized by the method. FIG. 3 shows that the gold-lead nanoclusters are nearly spherical and are formed by aggregation of many 2-3nm small circular particles, and the fluorescence of the gold-lead nanoclusters is proved to be aggregation-induced fluorescence enhancement.
Example 2 sodium-metiram detection application of gold-lead nanoclusters
(1) Adding 10 mu L of gold-lead nano cluster solution into 1980 mu L of acetic acid-sodium acetate diluted buffer solution (the concentration is 10mM, and the pH value is 6), and sequentially and repeatedly preparing a plurality of groups of detection solutions; then respectively adding 10 mu L of sodium metiram solution with different concentrations into each group of detection solution, uniformly mixing, reacting for 3min at room temperature, measuring the fluorescence of the solution with the excitation wavelength of 300nm, as shown in figure 4, with the increase of the concentration of sodium metiram, the fluorescence intensity of the gold-lead nano cluster at 510nm is gradually weakened, and the ratio of the concentration of sodium metiram to the fluorescence intensity of the gold-lead nano cluster (F) 0 [ solution ] F, F and F 0 Respectively, the fluorescence intensity with or without the sodium-metiram) is in good linear relation in the range of 0.1nM-30nM, the detection limit is 30pM, and the method can be used for the ultra-sensitive detection of the sodium-metiram.
(2) In the aspect of selectivity of the gold-lead nano-cluster on sodium metiram detection, other pesticides, metal ions and anions include sodium metiram, phoxim, phenmedipham, diflubenzuron, fenthion, carboxim, thiram, maneb, aldicarb, fe 3+ 、Co 2+ 、Ni 2+ 、Cu 2 + 、Zn 2+ 、Mn 2+ 、Pb 2+ 、Cd 2+ 、Mg 2+ 、Ca 2+ 、CO 3 2- 、SO 4 2- 、HCO 3 2- 、P 3 O 4 2- 、F - And Cl - The detection of the sodium-acetate complex is not interfered by the gold-lead nano-cluster (shown in figure 5), which shows that the gold-lead nano-cluster has good selectivity for the detection of the sodium-acetate complex.
The foregoing merely represents preferred embodiments of the invention, which are described in some detail and detail, and therefore should not be construed as limiting the scope of the invention. It should be noted that various changes, modifications and substitutions may be made by those skilled in the art without departing from the spirit of the invention, and all are intended to be included within the scope of the invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
Claims (7)
1. The preparation method of the gold-lead fluorescent nano-cluster is characterized by comprising the following steps: the method takes chloroauric acid as a raw material, adenosine as a stabilizing agent, ascorbic acid as a reducing agent and lead acetate as a doping agent to prepare the gold-lead nanoclusters by a one-step method; the method comprises the following steps:
s1, sequentially adding 20-140 parts by volume of 10mM chloroauric acid, 20-120 parts by volume of 10mM lead acetate, 40-360 parts by volume of 25mM adenosine, 50 parts by volume of 20mM citric acid-sodium citrate buffer solution and 20-120 parts by volume of 10mM ascorbic acid into a container, wherein the pH of the buffer solution is 3-8, and adding a proper amount of ultrapure water to uniformly mix until the final volume is 1000 parts by volume;
and S2, reacting the mixed solution obtained in the step S1 at 25-90 ℃ for 0-6h, centrifuging for 15min at 12500rpm, taking the lower-layer precipitate, and dissolving in water to obtain the gold-lead nano cluster.
2. The method for preparing gold-lead fluorescent nanoclusters according to claim 1, wherein the method comprises the following steps: the dosage of the chloroauric acid in the step S1 is 80 parts by volume; the using amount of the lead acetate is 80 parts by volume; the dosage of adenosine is 280 volume parts; the pH of the buffer solution is 5; the ascorbic acid was used in an amount of 70 parts by volume.
3. The method for preparing gold-lead fluorescent nanoclusters according to claim 1, wherein the method comprises the following steps: the reaction temperature in the step S2 is 60 ℃; the reaction time was 1h.
4. The application of the gold-lead fluorescent nano-cluster prepared by the method of any one of claims 1 to 3, which is characterized in that: the gold-lead nano-cluster is used for detecting sodium metiram.
5. The application according to claim 4, characterized in that the application method comprises:
(1) Preparing a plurality of groups of detection solutions: adding 10 parts by volume of gold-lead nanocluster solution into 1980 parts by volume of acetic acid-sodium acetate diluted buffer solution, mixing to form detection solution, and repeating for preparing multiple groups;
(2) Mixing the detection solutions with sodium metiram solutions with different concentrations, and reacting at room temperature for 3min;
(3) Measuring the fluorescence emission spectrum of the solution with the excitation wavelength of 300nm for the mixed solution prepared in the step (2);
(4) According to the fluorescence intensity ratio F/F of the gold-lead nano cluster corresponding to sodium metiram with different concentrations at 510nm 0 Relationship between them to detect sodium, F and F 0 The fluorescence intensity of the gold nanoclusters in the presence and absence of sodium metiram, respectively.
6. Use according to claim 5, characterized in that: the concentration of the acetic acid-sodium acetate diluted buffer solution in the step (1) is 10mM, and the pH value is 6.
7. Use according to claim 5, characterized in that: with the increase of the concentration of sodium metiram, the fluorescence intensity of the gold-lead nano cluster at 510nm is gradually weakened, and the concentration of sodium metiram and F of the gold-lead nano cluster solution 0 the/F is in a linear relation in a range of 0.1nM to 30nM, and the detection limit is 30 pM.
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| ZA2022/01277A ZA202201277B (en) | 2021-06-19 | 2022-01-27 | Method for preparing gold-lead fluorescent nanocluster and application in nabam detection |
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