CN111795958B - Specific detection of Ag + Preparation of CdSe quantum dot, detection method and application thereof - Google Patents
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Abstract
The invention discloses a specific detection Ag + The preparation of the CdSe quantum dots, and the detection method and the application thereof; the detection method comprises the following steps: the concentration is 3.4 multiplied by 10 ‑10 M～3.4×10 ‑9 Adjusting the pH of the aqueous dispersion of the CdSe quantum dots of M to 7-9, and adding Ag with different concentration gradients + Uniformly mixing the solution to obtain a mixed reaction system; based on this, a detection Ag was constructed + A concentration ratio-type fluorescent probe; measuring the fluorescence intensity ratio of the mixed reaction system at 510nm and 650nm to obtain Ag in the mixed reaction system + The concentration is the abscissa, and the fluorescence intensity ratio I of the mixed reaction system is used 650 /I 510 As ordinate, Ag was obtained + Concentration-fluorescence intensity ratio curve; according to Ag + Concentration-fluorescenceCalculating Ag in the system to be measured according to the light intensity ratio curve + And (4) concentration. The detection method has the advantages of simple operation, high selectivity and low detection limit, can be used for rapid, low-cost and high-sensitivity detection of silver ions in water, and has bright application prospect.
Description
Technical Field
The invention relates to the field of nanotechnology, in particular to a method for specifically detecting Ag + The preparation of CdSe quantum dots, and the detection method and application thereof.
Background
Silver ion is found everywhere in life, and plays an important role in modern life. Widely applied to the aspects of sterilization, photographing, cosmetics and the like, but people have more understanding that: silver ion is a heavy metal element and is toxic. In recent decades, with the large-scale development of industry, various metals have been widely used in various fields such as petroleum, chemical industry, aviation, agriculture, and the like. Many industrial waste water is directly discharged without being treated, so that the problem of metal ion pollution caused by the waste water is serious day by day, and the content of heavy metal in part of water bodies exceeds the standard. Ag in water + The excessive content can cause the pathological changes of a plurality of animals and plants and even death. At the same time, Ag + Can enter human body for enrichment through skin absorption, biological accumulation and other effects. In vivo Ag + The increase of the content can stimulate the change of eyes, skin, breath and blood cells, and also can cause a series of diseases such as kidney injury, gastropathy, epilepsy and the like, and Ag in the body of children + Excessive content can also cause growth retardation. The content of silver ions in drinking water is less than 0.1mg/L according to the regulations of the world health organization. Therefore, it is very important to accurately monitor the content of silver ions.
The conventional methods for detecting metal ions include: electrochemical method, mass spectrometry, atomic absorption spectrometry, and fluorescence spectrometry. At present, fluorescence spectroscopy (especially quantum dots as fluorescent probes) is widely applied to metal ion detection in various fields due to the advantages of high sensitivity, high selectivity and low cost.
Most common fluorescent probes are mostly quenchingFluorescent probes of the type, monomodal, which limit the detection limit and selectivity to some extent; or the detection mechanism is complex, so that the method is difficult to popularize and use in a large range. And the existing CdSe quantum dot pairs are aligned to Ag + The detection selectivity is poor, and the interference of other ions cannot be effectively avoided, so that accurate detection cannot be achieved.
Disclosure of Invention
It is an object of the present invention to address at least the above-mentioned deficiencies and to provide at least the advantages which will be described hereinafter.
Another object of the present invention is to provide a method for detecting Ag using specificity + The CdSe quantum dots are detected to improve Ag + Sensitivity and selectivity of detection.
Another objective of the invention is to provide a method for specifically detecting Ag + The preparation method of the CdSe quantum dot.
Another objective of the invention is to provide a method for detecting Ag specifically + The CdSe quantum dots are applied as silver ion fluorescent probes.
The scheme provided by the invention is as follows:
ag detection by utilizing specificity + The CdSe quantum dots detection method comprises the following steps:
the concentration is 3.4 multiplied by 10 -10 M～3.4×10 -9 Adjusting the pH of the aqueous dispersion of the CdSe quantum dots to 7-9, and then adding Ag with different concentration gradients + Uniformly mixing the solution to obtain a mixed reaction system with corresponding concentration; based on this, a detection Ag was constructed + Concentration ratio-type fluorescent probes;
measuring the fluorescence intensity ratio of the mixed reaction system at 510nm and 650nm to obtain Ag in the mixed reaction system + The concentration is the abscissa, and the fluorescence intensity ratio I of the mixed reaction system is used 650 /I 510 As ordinate, Ag was obtained + Concentration-fluorescence intensity ratio curve;
measuring the fluorescence intensity ratio of the system to be measured at 510nm and 650nm according to Ag + Calculating Ag in the system to be measured according to the concentration-fluorescence intensity ratio curve + And (4) concentration.
In the technical scheme, Ag is added near 510nm of CdSe quantum dot fluorescence peak + Then, the fluorescence of the CdSe quantum dots at 510nm is weakened, the fluorescence at 650nm is enhanced, and based on the weakening, the detection of Ag in water is constructed + Concentration ratio type fluorescent probe. By the pair I 650 /I 510 And Ag + The concentration relation can realize the rapid and efficient specific detection of silver ions. The detection method eliminates errors by constructing a ratio type probe (the ratio of two fluorescence peaks), overcomes the defects of a quenching type fluorescence probe and a single-peak fluorescence probe, and obtains more reliable data, more excellent selectivity and lower detection limit. The detection method can effectively avoid more interference ions, so the method has high selectivity and sensitivity, and can detect Ag in the water phase + More sensitive and stronger selectivity.
With Ag + With CdSe quantum dots to Ag 2 Se quantum dot conversion, which is shown on a fluorescence spectrogram as the fluorescence is gradually enhanced at 650 nm. And with Ag + Increasing and red shift. By variation of two peaks (I) 650 /I 510 ) To rapidly detect silver ions. By adding common metal ions for comparison, experiments show that: the phenomenon can be caused only by silver ions, and the specificity is strong. The method has the advantages of simple operation, high selectivity and low detection limit, can be used for rapid, low-cost and high-sensitivity detection of silver ions in water, and has bright application prospect.
Preferably, the specific detection of Ag is performed + In the method for detecting CdSe quantum dots, the concentration of the aqueous dispersion of CdSe quantum dots is 3.4 × 10 -10 M, pH 9.
Preferably, the specific detection of Ag is performed + In the method for detecting CdSe quantum dots, the aqueous dispersion of CdSe quantum dots and Ag + The reaction time of the solution is 30 seconds, and the temperature is 20-25 ℃ room temperature.
Preferably, the specific detection of Ag is performed + In the method for detecting CdSe quantum dots, Ag is contained in the mixed reaction system + Concentration of the solutionThe degree is in the range of 0.01 to 4 μ M.
The specificity is used for detecting Ag + The preparation method of the CdSe quantum dot comprises the following steps:
adding CdCl 2 ·2H 2 Dissolving O and N-acetyl-L-cysteine (NAC) or Glutathione (GSH) in ultrapure water, and adjusting pH to 9; then adding NaHSe solution, stirring, and introducing N 2 Heating to obtain the specific detection Ag + CdSe quantum dots of (a);
wherein, CdCl 2 ·2H 2 The molar ratio of O and N-acetyl-L-cysteine (NAC) is 1: 1.14; or CdCl 2 ·2H 2 The molar ratio of O to Glutathione (GSH) is 1: 1.14.
the preparation method has simple synthesis steps, and the Cd precursor is prepared without ice bath stirring and N is introduced 2 The prepared CdSe quantum dot has better fluorescence property by selecting a specific ligand and a specific molar ratio, and is more suitable for Ag + Specific detection of (3).
Preferably, the specific detection of Ag + In the preparation method of the CdSe quantum dot, the NaHSe solution is obtained by the following steps: mixing Se powder and NaBH 4 Mixing evenly, injecting ultrapure water, and stirring at the room temperature of 20-25 ℃.
Preferably, the specific detection of Ag + In the preparation method of the CdSe quantum dot, the Ag is detected by the specificity + The particle diameter of the CdSe quantum dot is 2.9 +/-1.0 nm.
Ag for specific detection + The CdSe quantum dots are applied as silver ion fluorescent probes.
A construction method of ratio type probe for detecting Ag by using specificity + The CdSe quantum dot comprises the following steps:
adding a series of Ag with different concentrations into CdSe quantum dots + To make CdSe quantum dots to Ag 2 Se quantum dots are converted and expressed as follows on a fluorescence map: decrease in fluorescence intensity at 510nm, 650nmThe intensity of fluorescence at (a) increases;
passing the fluorescence intensity ratio I at 510nm and 650nm 650 /I 510 With Ag + And (3) constructing a ratio type fluorescent probe for detecting silver ions according to the concentration relation.
The invention at least comprises the following beneficial effects:
the invention utilizes CdSe quantum dots with fluorescence peak near 510nm, and adds Ag + Then, the fluorescence of the CdSe quantum dots at 510nm is weakened, the fluorescence at 650nm is enhanced, and based on the weakening, the detection of Ag in water is constructed + Concentration ratio type fluorescent probe. By the pair I 650 /I 510 And Ag + The concentration relation can realize the rapid and efficient specific detection of silver ions. The detection method eliminates errors through the ratio of two fluorescence peaks, overcomes the defects of quenching type fluorescent probes and single-peak fluorescent probes, and obtains more reliable data, more excellent selectivity and lower detection limit. The detection method can effectively avoid more interference ions, so the method has high selectivity and sensitivity, and can detect Ag in the water phase + More sensitive and stronger selectivity.
The invention obtains a CdSe quantum dot probe with high sensitivity by a (two peak values are changed) ratio type. Compared with the traditional CdSe quantum dot unimodal probe, the probe has good water solubility and can effectively avoid more interfering ions, so that the detection mechanism has high selectivity and high sensitivity, and the Ag in the water phase is detected + More sensitive and stronger selectivity.
The detection method of the invention is different from the traditional detection method: the invention can be applied to the Ag in a water system + Detection, has attractive application prospect.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a fluorescent spectrum of CdSe quantum dots modified by different ligands synthesized in example 1;
FIG. 2 is a fluorescence spectrum of CdSe quantum dots obtained by reacting for different times during NAC modification in example 1;
FIG. 3 is a graph of UV-Vis and fluorescence spectra of NAC-modified CdSe quantum dots;
FIG. 4 is a graph of dynamic light scattering of NAC-modified CdSe quantum dots;
FIG. 5 is a chart of the study of the optimal reaction time;
FIG. 6 is a graph of the reaction of common metal ions added to CdSe quantum dots;
FIG. 7 is a plot of the fluorescence spectra of the system over a linear range, after addition of CdSe quantum dots at different silver ion concentrations;
FIG. 8 is a graph of Ag after reaction of different silver ion concentrations with CdSe quantum dots in a linear range + And the ratio of fluorescence intensities I 650 /I 510 Linear regression graph of (a).
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
It is to be noted that the experimental procedures described in the following examples are conventional ones unless otherwise specified, and the reagents and materials described therein are commercially available without otherwise specified.
Example 1
Synthesizing CdSe quantum dots by an aqueous phase method:
39.5mg of Se powder and 40mg of NaBH are accurately weighed 4 The mixture was mixed well, 2mL of ultrapure water was injected, and the mixture was stirred at room temperature for 30min to obtain a colorless transparent NaHSe solution.
N-acetyl-L-cysteine (NAC) and Glutathione (GSH) are respectively used as ligands; respectively adding 38.4mg of CdCl 2 ·2H 2 O and 27.5mg of NAC or 47.2mg of GSH were dissolved in 80mL of ultrapure water, the pH was adjusted to 9, the mixture was stirred at room temperature, 170. mu.L of a freshly prepared NaHSe solution was added thereto, the mixture was stirred for 2 hours, and N was added thereto 2 Heating for 12h, cooling to obtain NAC modified quantum dots and GSH modified quantum dots respectively, and purifying to obtain the quantum dots for experiment.
Wherein, the fluorescence spectrum of the CdSe quantum dots synthesized by different ligands is shown in figure 1; when NAC is used for modification, CdSe quantum dots obtained in different reaction times are shown in FIG. 2; the ultraviolet-fluorescence spectrum and dynamic light scattering pattern of the NAC modified CdSe quantum dots are shown in FIGS. 3 and 4.
The UV-Vis spectrum shows: the quantum dots have absorption peaks at 478nm, which also indicates the successful synthesis of the quantum dots. The hydrated particle size of the obtained CdSe quantum dot is about 5.6nm through dynamic light flash measurement, which shows that the particle size is uniform and the quantum dot is successfully synthesized.
Example 2
The difference from example 1 is that the pH was adjusted to 7.
Example 3
The difference from example 1 is that the pH was adjusted to 8.
Example 4
Ag detection by utilizing specificity + The CdSe quantum dots detection method comprises the following steps:
the concentration obtained in example 1 was 3.4X 10 -10 Adjusting pH of aqueous dispersion of NAC modified CdSe quantum dots of M to 9, and adding Ag with different concentration gradients + Uniformly mixing the solution to obtain a mixed reaction system with corresponding concentration; based on the method, a method for detecting Ag in water is constructed + Concentration ratio type fluorescent probe.
Measuring the fluorescence intensity ratio of the mixed reaction system at 510nm and 650nm to obtain Ag in the mixed reaction system + The concentration is the abscissa, and the fluorescence intensity ratio I of the mixed reaction system is used 650 /I 510 As ordinate, Ag was obtained + Concentration-fluorescence intensity ratio curve;
measuring the fluorescence intensity ratio of the system to be measured at 510nm and 650nm according to Ag + Calculating Ag in the system to be measured according to the concentration-fluorescence intensity ratio curve + And (4) concentration.
Example 5
Optimum quantum dot concentration experiment of CdSe quantum dot for silver ion detection
30-180 muL (15 muL interval) of NAC modified and pure prepared in example 1 is added into deionized waterCdSe quantum dots after being converted, and then Ag is added + Respectively obtaining mixed reaction systems with the total volume of 2mL and different quantum dot concentrations, wherein Ag is contained in the mixed reaction systems + The concentration is unified to 10 mu M, the fluorescence intensity of each mixed reaction system at 510nm and 650nm is recorded, the concentration of quantum dots in each mixed reaction system is taken as the abscissa, and the fluorescence intensity ratio I of each mixed reaction system is taken as 650 /I 510 And obtaining a quantum dot concentration-fluorescence intensity ratio curve as a vertical coordinate. The optimal quantum dot concentration is 3.4 multiplied by 10 -10 M。
Example 6
Optimum pH experiment for detecting silver ions by CdSe quantum dots
Using the NAC-modified CdSe quantum dots prepared in example 1 as quantum dots, the optimum quantum dot concentration was 3.4X 10 -10 Under M condition, the optimum pH was investigated. Setting the concentration of quantum dots to be 3.4 multiplied by 10 under different pH values (3-11) respectively -10 M and silver ion concentration of 10 mu M, recording the fluorescence intensity of each mixed reaction system at 510nm and 650nm, taking the pH in the mixed reaction system as a horizontal ordinate, and taking the fluorescence intensity ratio I of the mixed reaction system 650 /I 510 The results of the experiments at different pH values are compared as ordinate. The system works best at pH 9.
Example 7
Optimum reaction time experiment of CdSe quantum dot pair silver ion detection
Using the NAC-modified CdSe quantum dots prepared in example 1 as quantum dots, the optimum quantum dot concentration was 3.4X 10 -10 Under the condition that M and the optimum pH value are 9, the optimum reaction time of the CdSe quantum dot probe on silver ion detection is researched. Separately mixing CdSe quantum dots with Ag of different concentrations + (0, 2, 4. mu.M) to obtain a mixed reaction system. According to the fluorescence intensity ratio I of each mixed reaction system 650 /I 510 As ordinate and incubation time as abscissa, the fluorescence intensity ratio I of the time-mixed reaction system is obtained 650 /I 510 Curve line. The results of the experiment are shown in FIG. 5, and the curve tends to be horizontal after 30 seconds of reaction, indicating that the reaction is rapid.
Example 8
CdSe quantum dot pair silver ion detection selectivity experiment
The NAC modified CdSe quantum dots prepared in example 1 are used as quantum dots, and the optimal quantum dot concentration is 3.4 multiplied by 10 -10 M, optimum pH 9 and optimum reaction time of 30 seconds, and performing selectivity experiments on common metals. Respectively adding common metal ions (Pb) 2+ 、Hg 2+ 、Cd 2+ 、Ni + 、Cr 3+ 、Zn 2+ 、Al 3+ 、Mn 2+ 、Na + 、Ca 2+ 、Ba 2+ 、 Cu 2+ 、Co 2+ 、Fe 3+ 、K + 、Mg 2+ 、Ag + ) Adding the purified CdSe quantum dots (the silver ion concentration is 10 mu M, and the other is 100 mu M) of 2mL to form mixed reaction systems, and taking the fluorescence intensity ratio I of each mixed reaction system 650 /I 510 Is a vertical coordinate, the concentration of each ion is a horizontal coordinate, and the fluorescence intensity ratio I of each metal ion concentration-mixed reaction system is obtained 650 /I 510 Curve line. The results are shown in FIG. 6, Ag + The concentration of (A) is only one tenth of that of other metals, but Ag + The selectivity of the CdSe quantum dots is still greatly superior to that of other ions, which shows that the CdSe quantum dots have high selectivity on silver ions.
Example 9
Construction of ratiometric probes
Using the NAC modified CdSe quantum dots prepared in example 1, a series of different concentrations of Ag were added to the CdSe quantum dots + To make CdSe quantum dots to Ag 2 Se quantum dots are converted and expressed as follows on a fluorescence map: the fluorescence intensity at 510nm is reduced, and the fluorescence intensity at 650nm is increased; passing the fluorescence intensity ratio I at 510nm and 650nm 650 /I 510 With Ag + And (3) constructing a ratio type fluorescent probe for detecting silver ions according to the concentration relation.
Example 10
Working curve of CdSe quantum dot pair silver ion detection
Using the NAC-modified CdSe quantum dots prepared in example 1 as quantum dots, the optimum quantum dot concentration was 3.4X 10 -10 M, optimum pH 9 and optimum reaction time 30 seconds, Ag is added in different concentrations + Forming different mixed reaction systems, and constructing and obtaining a ratio type fluorescent probe based on the different mixed reaction systems; the fluorescence intensities at 510nm and 650nm of the mixed reaction system were recorded separately, as shown in FIG. 7, for Ag in the mixed reaction system + The concentration is the abscissa, and the fluorescence intensity ratio I of the mixed reaction system is used 650 /I 510 As ordinate, Ag was obtained + Concentration-fluorescence intensity ratio curve. The results are shown in FIG. 7, Ag + Has stronger quenching effect on the fluorescence of CdSe quantum dots at 510nm with Ag + The fluorescence of the CdSe quantum dots at 510nm is quenched more obviously due to the increase of the concentration, and the fluorescence of the CdSe quantum dots at 650nm is increased continuously. As shown in FIG. 8, the CdSe quantum dot probe has a linear range of 0.01-4 μ M for silver ion detection, a detection limit of 1.7 nM, and a correlation coefficient R 2 ＝0.9883。
While embodiments of the invention have been disclosed above, it is not intended that they be limited to the applications set forth in the specification and examples. It can be applied to all kinds of fields suitable for the present invention. Additional modifications will readily occur to those skilled in the art.
Claims (3)
1. Ag detection by utilizing specificity + The CdSe quantum dot detecting method is characterized by comprising the following steps:
the concentration is 3.4 multiplied by 10 -10 The pH of the aqueous dispersion of the CdSe quantum dots of M is adjusted to 9, and then Ag with different concentration gradients is respectively added + Uniformly mixing the solution to obtain a mixed reaction system with corresponding concentration; thereby constructing a detection Ag + A concentration ratio-type fluorescent probe;
measuring the fluorescence intensity ratio of the mixed reaction system at 510nm and 650nm to obtain Ag in the mixed reaction system + Concentration is abscissa, and the ratio of fluorescence intensity of the mixed reaction systemI 650 /I 510 As ordinate, Ag was obtained + Concentration-fluorescence intensity ratio curve;
according to Ag + Concentration-fluorescence intensityCalculating Ag in the system to be measured by the ratio curve + Concentration;
wherein, the aqueous dispersion of CdSe quantum dots and Ag + The reaction time of the solution is 30 seconds, and the temperature is 20-25 ℃ room temperature;
ag in the mixed reaction system + The concentration range of the solution is 0.01-4 mu M;
the preparation method of the CdSe quantum dot comprises the following steps:
adding CdCl 2 •2H 2 Dissolving O and N-acetyl-L-cysteine or glutathione in ultrapure water, adjusting pH = 7 or 8 or 9; then adding NaHSe solution, stirring, and introducing N 2 Heating to obtain the specific detection Ag + CdSe quantum dots of (a);
wherein, CdCl 2 •2H 2 The molar ratio of O and N-acetyl-L-cysteine or glutathione is 1: 1.14.
2. the method of claim 1 using specific detection of Ag + The detection method of the CdSe quantum dots is characterized in that the NaHSe solution is obtained by the following steps: mixing Se powder and NaBH 4 Mixing evenly, injecting ultrapure water, and stirring at the room temperature of 20-25 ℃.
3. The method of claim 2 using specific detection of Ag + The CdSe quantum dots are used for detecting, and the method is characterized in that Ag is detected specifically + The particle diameter of the CdSe quantum dot is 2.9 +/-1.0 nm.
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