CN115197698A - Nitrogen and sulfur co-doped carbon quantum dot and preparation method and application thereof - Google Patents
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Abstract
The invention belongs to the technical field of fluorescent probes, and particularly relates to a nitrogen and sulfur co-doped carbon quantum dot and a preparation method and application thereof. The preparation method of the nitrogen and sulfur co-doped carbon quantum dot comprises the following steps: mixing sodium lignosulfonate, ethylenediamine and water, and carrying out hydrothermal reaction to obtain the nitrogen-sulfur co-doped carbon quantum dot. The nitrogen and sulfur co-doped carbon quantum dot provided by the invention can be directly used for detecting the total manganese content in a sample to be detected. The data of the embodiment show that when the nitrogen-sulfur co-doped carbon quantum dot provided by the invention is used for detecting total manganese, the sensitivity is high, the reproducibility is good, and the interference of other ions is avoided.
Description
Technical Field
The invention belongs to the technical field of fluorescent probes, and particularly relates to a nitrogen and sulfur co-doped carbon quantum dot and a preparation method and application thereof.
Background
Manganese (Mn), an element ubiquitous in rock formations and soils, is also an essential nutrient for humans and animals and plants. The manganese element can cause obvious harm to human bodies, animals and plants when being taken insufficiently or excessively. Manganese deficiency symptoms can affect reproductive performance, and may cause congenital malformations in later generations, abnormal bone and cartilage formation, and impaired glucose tolerance. In addition, manganese deficiency can cause neurasthenia syndrome and affect intelligence development. Manganese deficiency will also lead to a decrease in insulin synthesis and secretion, affecting carbohydrate metabolism. Manganese is also an anticancer substance, and has inhibitory effect on virus-induced tumor and chemical carcinogenesis.
Currently, the main methods for detecting Mn include: atomic Absorption Spectroscopy (AAS), inductively coupled plasma atomic emission spectroscopy (ICP-AES), inductively coupled plasma mass spectroscopy (ICP-MS), electrochemical methods (EC), and the like. The methods have respective unique advantages, but have certain defects, such as high requirements on sample pretreatment, complex and expensive instruments and devices, time and labor consumption, high cost and the like, and limit the application of the methods in rapid detection. The fluorescence method has the advantages of fast response, low cost, high sensitivity and the like. Some fluorescent probes have been reported for detecting Mn, but these probes are selective for Mn (VII) or Mn (II). This means that if such probes are used for the detection of total manganese in an environmental medium, it is necessary to convert Mn (VII) in the sample to be tested to Mn (II) or Mn (II) to Mn (VII), and they cannot be used directly for the detection of total manganese.
Disclosure of Invention
In view of this, the invention aims to provide a nitrogen and sulfur co-doped carbon quantum dot, and a preparation method and application thereof.
In order to achieve the purpose, the invention provides a nitrogen and sulfur co-doped carbon quantum dot, and the preparation method of the nitrogen and sulfur co-doped carbon quantum dot comprises the following steps:
mixing sodium lignosulfonate, ethylenediamine and water, and carrying out hydrothermal reaction to obtain the nitrogen-sulfur co-doped carbon quantum dot.
Preferably, the volume ratio of the mass of the sodium lignin sulfonate to the volume of the ethylenediamine is 0.04-0.06 g:0.2mL.
Preferably, the temperature of the hydrothermal reaction is 150-170 ℃ and the time is 3.5-4.5 h.
Preferably, after the hydrothermal reaction, the method further comprises the steps of cooling and filtering the product obtained by the hydrothermal reaction in sequence, and drying the supernatant obtained by filtering.
The invention also provides a preparation method of the nitrogen and sulfur co-doped carbon quantum dot, which comprises the following steps: mixing sodium lignosulfonate, ethylenediamine and water, and carrying out hydrothermal reaction to obtain nitrogen and sulfur co-doped carbon quantum dots;
the mass ratio of the sodium lignin sulfonate to the ethylenediamine is (0.04-0.06 g): 0.2mL;
the temperature of the hydrothermal reaction is 150-170 ℃, and the time is 3.5-4.5 h.
The invention also provides application of the nitrogen and sulfur co-doped carbon quantum dot in detecting total manganese.
The invention also provides a method for detecting total manganese by using the nitrogen and sulfur co-doped carbon quantum dots, which comprises the following steps:
digesting a sample to be detected to obtain a liquid to be detected;
mixing the liquid to be tested with the nitrogen and sulfur co-doped carbon quantum dot liquid, testing the fluorescence intensity of the mixed system to obtain the actually-measured fluorescence intensity F, and obtaining the initial fluorescence intensity F according to a preset linear curve 0 And the ratio F of the fluorescence intensity F 0 Obtaining the concentration of total manganese in the sample to be detected;
the predetermined linear curve is F 0 /F Standard of reference And the linear relationship curve of the total manganese concentration;
said F Standard of merit The fluorescence intensity obtained by nitrogen and sulfur co-doped carbon quantum dot solution containing different concentrations of total manganese is tested.
Preferably, the excitation wavelength at which the fluorescence intensity is measured is 402nm.
The invention provides a nitrogen and sulfur co-doped carbon quantum dot, and a preparation method of the nitrogen and sulfur co-doped carbon quantum dot comprises the following steps: mixing sodium lignosulfonate, ethylenediamine and water, and carrying out hydrothermal reaction to obtain the nitrogen-sulfur co-doped carbon quantum dot. The nitrogen and sulfur co-doped carbon quantum dot provided by the invention can be directly used for detecting the total manganese content in a sample to be detected. The data of the embodiment show that when the nitrogen and sulfur co-doped carbon quantum dot provided by the invention is used for detecting total manganese, the sensitivity is high, the reproducibility is good, and the interference of other ions is avoided.
Drawings
Fig. 1 is an ultraviolet spectrum and a fluorescence spectrum of the nitrogen and sulfur co-doped carbon quantum dot prepared in example 1;
FIG. 2 is an excitation wavelength dependent spectrum of the nitrogen and sulfur co-doped carbon quantum dot prepared in example 1;
FIG. 3 is a graph showing the fluorescence intensity variation of nitrogen and sulfur co-doped carbon quantum dot solution titrated by manganese single element standard solution in example 2;
FIGS. 4 and 5 are linear graphs of manganese concentration and nitrogen and sulfur co-doped carbon quantum dot fluorescence intensity;
FIG. 6 is a diagram showing the results of an interference experiment of metal elements on total manganese detection;
FIG. 7 is a graph showing the results of an interference test of amino acids on total manganese detection.
FIG. 8 is a graph of the results of an interference test of anions on total manganese detection.
Detailed Description
The invention provides a nitrogen and sulfur co-doped carbon quantum dot, and a preparation method of the nitrogen and sulfur co-doped carbon quantum dot, which comprises the following steps:
mixing sodium lignosulfonate, ethylenediamine and water, and carrying out hydrothermal reaction to obtain the nitrogen-sulfur co-doped carbon quantum dot.
In the present invention, the ratio of the mass of the sodium lignosulfonate to the volume of the ethylenediamine is preferably 0.04 to 0.06g:0.2mL, more preferably 0.05g:0.2mL.
In the present invention, the temperature of the hydrothermal reaction is preferably 150 to 170 ℃, and more preferably 160 ℃. In the present invention, the hydrothermal reaction time is preferably 3.5 to 4.5 hours, and more preferably 4 hours.
In the invention, after the hydrothermal reaction, the method further comprises the steps of sequentially cooling and filtering the product obtained by the hydrothermal reaction, and drying the supernatant obtained by filtering. In the present invention, the cooling is preferably to room temperature; the filtration preferably comprises medium speed filter paper filtration and 0.22 μm membrane filtration in sequence. In the present invention, the drying is preferably freeze-drying, and the temperature of the freeze-drying is preferably-80 ℃. In the present invention, the drying time is not particularly limited, and the drying can be completed.
The invention also provides a preparation method of the nitrogen and sulfur co-doped carbon quantum dot, which comprises the following steps: mixing sodium lignosulfonate, ethylenediamine and water, and carrying out hydrothermal reaction to obtain the nitrogen-sulfur co-doped carbon quantum dot.
The invention also provides application of the nitrogen and sulfur co-doped carbon quantum dot in detecting total manganese.
The invention also provides a method for detecting total manganese by using the nitrogen and sulfur co-doped carbon quantum dots, which comprises the following steps:
digesting a sample to be detected to obtain a liquid to be detected;
mixing the liquid to be tested with the nitrogen and sulfur co-doped carbon quantum dot liquid, testing the fluorescence intensity of the mixed system to obtain the actually-measured fluorescence intensity F, and obtaining the initial fluorescence intensity F according to a preset linear curve 0 And the ratio F of the fluorescence intensity F 0 Obtaining the concentration of total manganese in the sample to be detected;
the predetermined linear curve is F 0 /F Standard of merit A linear relationship curve with total manganese concentration;
said F Standard of merit The fluorescence intensity obtained by nitrogen and sulfur co-doped carbon quantum dot solution containing different concentrations of total manganese is tested.
In the invention, the digestion preferably comprises mixing a sample to be detected with concentrated nitric acid, and acidifying, wherein the mass concentration of the concentrated nitric acid is preferably 60-68%, and more preferably 65-67%.
In the present invention, the obtaining of the predetermined linear curve preferably includes the steps of:
mixing manganese single element standard solutions with different concentrations with the nitrogen and sulfur co-doped carbon quantum dot solution, and testing the fluorescence intensity F Standard of merit With F 0 /F Standard of merit Taking the total manganese concentration in the manganese single element standard solution as a vertical coordinate and taking the total manganese concentration in the manganese single element standard solution as a horizontal coordinate to obtain a linear equation;
in the present invention, the excitation wavelength at which the fluorescence intensity is measured is preferably 402nm; the emission wavelength at which the fluorescence intensity is measured is preferably 492nm.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
0.05g of sodium lignosulfonate was weighed, 10mL of ultrapure water was added, ultrasonic dispersion was carried out for 20min, then 0.2mL of ethylenediamine was added to the obtained dispersion, and hydrothermal reaction was carried out in a high-pressure reaction vessel at 160 ℃ for 4h to obtain a NS-CQDs solution.
After the reaction kettle is cooled to room temperature, preliminarily filtering the carbon quantum dot solution obtained in the step (1) by using medium-speed filter paper to remove large particles; then, further filtration was carried out with a 0.22 μm filter to obtain a yellow supernatant, which was freeze-dried (temperature-80 ℃ C.) to obtain NS-CQDs powder.
FIG. 1 is a UV absorption spectrum of an aqueous solution of NS-CQDs diluted to 1mg/mL of powder of NS-CQDs prepared in example 1, as can be seen from FIG. 1: two distinct absorption peaks at 243nm and 330nm, respectively, are formed by aromatic sp 2 The carbon is caused by surface defects generated by pi → pi transition and N doping. The optimal excitation and emission peaks for NS-CQDs are at 402nm and 492nm, respectively.
FIG. 2 the emission spectrum of NS-CQDs prepared in example 1 at different excitation wavelengths, red-shifted from 476nm to 519nm when the excitation wavelength was changed from 350nm to 460nm, indicating that NS-CQDs have excitation wavelength dependence.
Example 2
1. Preparation of solutions
(1) Amino acid stock solution
Respectively weighing proper amount of glycine, serine, valine, methionine, histidine, glutathione, tryptophan, arginine, cysteine, aspartic acid, threonine, glutamic acid, lysine, glutamine, alanine, leucine, isoleucine, phenylalanine, tyrosine and proline, adding 5mL of ultrapure water, and ultrasonically dissolving to prepare the amino acid stock solution with the concentration of 0.1 mol/L.
(2) Anion stock solution
Separately weighing appropriate amount of anion (Na) 2 SO 3 ，Na 2 SO 4 ，Na 2 HPO 4 ，NaNO 3 ，NaNO 2 ，NaHCO 3 ，Na 2 CO 3 ，NaSCN，NaBr，NaI，NaF，NaClO 4 ，NaHS，NaHSO 3 ，Na 2 S 2 O 3 ，NaH 2 PO 4 NaCl) compound, 5mL of ultrapure water was added, and ultrasonic dissolution was carried out to prepare an anion stock solution of 0.1 mol/L.
(3) 1000 mug/mL standard solution of metal single element
Standard solutions of the respective metal elements (Ag, co, zn, ca, cu, cd, pb, ba, cr, fe, la, ni, al, mg, hg) are commercially available at a mass concentration of 1000. Mu.g/mL.
(4) Stock solution of 10mg/mLNS-CQDs
Accurately weighing 0.1g of NS-CQDs powder in a beaker, and adding 10mL of ultrapure water for dissolving to obtain NS-CQDs stock solution with the concentration of 10 mg/mL.
(5) 1mg/mLNS-CQDs solution
Stock NS-CQDs at 10mg/mL was diluted to 1.0mg/mL with ultrapure water.
2. Preparation of a standard curve:
(1) Measuring the initial fluorescence intensity F of 1.0mg/mL NS-CQDs solution at 492nm 0 。
(2) Dropwise adding a manganese single element standard solution into the NS-CQDs solution in the step (1), recording the fluorescence intensity at 492nm, and recording as F Standard of merit 。
(3) Fluorescence intensity (F) was fitted using Origin software 0 /F Standard of merit ) Linear equation between change and manganese concentration in manganese single element standard solution.
FIG. 3 is a graph showing the change of fluorescence intensity with the addition of the manganese single element standard solution in step (2), and it can be seen from FIG. 3 that: with the addition of manganese element, the fluorescence of NS-CQDs at 492nm is gradually quenched.
FIGS. 4 and 5 show the change in fluorescence intensity at 492nm of NS-CQDs F 0 A linear relation graph between the concentration of manganese and the concentration of F, wherein when the linear range is 0.25-2.25 mg/L, the linear equation is F 0 /F Standard of merit ＝0.22815c+1.07316，R 2 =0.9984; when the linear range is 5.0-25.0 mg/L, the linear equation is as follows: f 0 /F Standard of merit ＝0.0.01438c+1.5085，R 2 =0.9966; in the formula, F 0 And F Standard of reference The minimum detection limit is 6.9 mug/L, which is the fluorescence intensity before and after the manganese standard solution is added.
Example 3
(1) The initial fluorescence intensity F of a NS-CQDs solution (2 mL) at a concentration of 1.0mg/mL was measured 0 。
(2) Adding 1 mu L of metal single element standard solution with the concentration of 1000 mu g/mL into the NS-CQDs solution in the step (1), measuring the fluorescence intensity of the mixed solution, and recording the fluorescence intensity as F 1 ；
(3) To the solution obtained in step (2), 1. Mu.L of a manganese single element standard solution having a concentration of 1000. Mu.g/mL, at which the concentration of total manganese was 0.5. Mu.g/mL, was added, and the fluorescence intensity at 492nm of the mixed solution was measured and was counted as F 2 。
F 1 /F 0 Calculating to obtain a black histogram, F 2 /F 1 The grey bar chart is obtained by calculation, the experimental result is shown in figure 6, and figure 6 shows that the detection method is not interfered by metal ions.
Example 4
(1) The initial fluorescence intensity F of a NS-CQDs solution (2 mL) at a concentration of 1.0mg/mL was measured 0 。
(2) Adding 20 μ L of 0.1mol/L amino acid stock solution into the NS-CQDs solution obtained in step (1), wherein the amino acid concentration is 0.99mmol/L, and measuring the fluorescence intensity of the mixed solution, and recording the fluorescence intensity as F 1 ；
(3) To the solution obtained in step (2), 22. Mu.L of a 1000. Mu.g/mL standard solution of manganese single element was added so that the manganese concentration was 0.196mmol/L, and the fluorescence intensity at 492nm of the mixed solution was measured and was counted as F 2 。
F 2 /F 1 The grey bar chart was calculated and the experimental results are shown in figure 7, which shows that the detection method is not interfered by amino acids in figure 7.
Example 5
(1) The initial fluorescence intensity F of a NS-CQDs solution (2 mL) at a concentration of 1.0mg/mL was measured 0 。
(2) Adding 20 mu L of anion stock solution with the concentration of 0.1mol/L into the NS-CQDs solution in the step (1),at this time, the anion concentration was 0.99mmol/L, and the fluorescence intensity of the mixed solution was measured and recorded as F 1 ；
(3) Adding 22. Mu.L of 1000. Mu.g/mL manganese single element standard solution to the solution obtained in the step (2), wherein the manganese concentration is 0.196mmol/L, and measuring the fluorescence intensity of the mixed solution at 492nm as F 2 ；
F 2 /F 1 The grey bar chart is calculated, the experimental result is shown in figure 8, and the detection method is not interfered by anions shown in figure 8.
Example 6
(1) Collecting surface water samples of northern river and eastern river in Luliang city, acidifying with concentrated nitric acid to reduce precipitation and absorption on container wall, and obtaining water sample to be detected.
(2) 50mL of water sample to be detected is taken, 5mL of concentrated nitric acid and 3mL of concentrated hydrochloric acid are added to be digested on a hot plate until the water sample is nearly dry. Dissolving the residue after digestion with dilute nitric acid, diluting to 50mL with ultrapure water, filtering with 0.45 μm microporous membrane, and storing for later use.
(3) To 1.8mL of ultrapure water was added 200. Mu.L of a stock solution of NS-CQDs at 10mg/mL to obtain a solution of NS-CQDs at a concentration of 1.0mg/mL, and the initial fluorescence intensity F at 492nm of the solution of NS-CQDs at 1.0mg/mL was measured 0 ；
(4) Taking 1.8mL of water sample to be detected, adding 200 mu L of 10mg/mLNS-CQDs stock solution, mixing uniformly, measuring the fluorescence intensity at 492nm, and recording as F;
f is to be 0 The result is shown in table 1, and the table 1 shows that the method for detecting the total manganese by using the prepared NS-CQDs can be used for detecting the actual water sample, has the relative standard deviation of less than 6.58 percent and has good reproducibility.
TABLE 1 Total manganese content in five surface water samples
| Sample (I) | Total manganese content (mg/L) | Relative standard deviation (n = 6) (%) |
| 1 | 0.11 | 6.58 |
| 2 | 0.18 | 4.26 |
| 3 | 0.21 | 3.81 |
| 4 | 0.17 | 5.73 |
| 5 | 0.24 | 3.65 |
Example 7
(1) To 1.8mL of ultrapure water was added 200. Mu.L of a 10mg/mLNS-CQDs stock solution to obtain a NS-CQDs solution having a concentration of 1.0mg/mL, and the initial fluorescence intensity F at 492nm was measured 0 ；
(2) Taking 4.5mL of water sample to be detected, adding 0.5mL of NS-CQDs solution with the concentration of 10mg/mL, uniformly mixing, adding 10 mu L of manganese single element standard solution with the concentration of 1000 mu g/mL, taking 2mL of mixed solution, measuring the fluorescence intensity at 492nm, and recording as F;
(3) F is to be 0 And substituting the/F into a linear equation, and calculating to obtain the standard recovery rate of the manganese in the actual sample.
The results are shown in Table 2, and Table 2 shows that the recovery rate of manganese in the five water samples is between 96.33% and 102.17%, and the relative standard deviation is less than 4.03%, which indicates that NS-CQDs can be used for detecting manganese in actual samples, and the method has good reproducibility.
Table 2 experimental results of standard recovery of total manganese in five water samples in example 5
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The nitrogen and sulfur co-doped carbon quantum dot is characterized in that the preparation method of the nitrogen and sulfur co-doped carbon quantum dot comprises the following steps:
mixing sodium lignosulfonate, ethylenediamine and water, and carrying out hydrothermal reaction to obtain the nitrogen-sulfur co-doped carbon quantum dot.
2. The nitrogen-sulfur co-doped carbon quantum dot according to claim 1, wherein the volume ratio of the mass of the sodium lignosulfonate to the volume of the ethylenediamine is 0.04-0.06 g:0.2mL.
3. The nitrogen and sulfur co-doped carbon quantum dot according to claim 1, wherein the hydrothermal reaction temperature is 150-170 ℃ and the hydrothermal reaction time is 3.5-4.5 h.
4. The nitrogen and sulfur co-doped carbon quantum dot according to any one of claims 1 to 3, wherein after the hydrothermal reaction, the method further comprises the steps of sequentially cooling and filtering a product obtained by the hydrothermal reaction, and drying a supernatant obtained by filtering.
5. The preparation method of the nitrogen and sulfur co-doped carbon quantum dot as claimed in any one of claims 1 to 3, which is characterized by comprising the following steps: mixing sodium lignosulfonate, ethylenediamine and water, and carrying out hydrothermal reaction to obtain nitrogen and sulfur co-doped carbon quantum dots;
the mass ratio of the sodium lignosulphonate to the ethylenediamine is 0.04-0.06 g:0.2mL;
the temperature of the hydrothermal reaction is 150-170 ℃ and the time is 3.5-4.5 h.
6. The application of the nitrogen and sulfur co-doped carbon quantum dot in detecting total manganese in claim 1.
7. A method for detecting total manganese by using the nitrogen and sulfur co-doped carbon quantum dots as claimed in any one of claims 1 to 4, which is characterized by comprising the following steps:
providing a nitrogen and sulfur co-doped carbon quantum dot solution, testing the fluorescence intensity of the nitrogen and sulfur co-doped carbon quantum dot solution to obtain initial fluorescence intensity F 0 ；
Digesting a sample to be detected to obtain a liquid to be detected;
mixing the liquid to be tested with the nitrogen and sulfur co-doped carbon quantum dot liquid, testing the fluorescence intensity of the mixed system to obtain the actually-measured fluorescence intensity F, and obtaining the initial fluorescence intensity F according to a preset linear curve 0 And the ratio F of the fluorescence intensity F 0 Obtaining the concentration of total manganese in the sample to be detected;
the predetermined linear curve is F 0 /F Standard of merit And the linear relationship curve of the total manganese concentration;
said F Standard of merit The fluorescence intensity obtained by nitrogen and sulfur co-doped carbon quantum dot solution containing different concentrations of total manganese is tested.
8. The method of claim 7, wherein the excitation wavelength at which the fluorescence intensity is measured is 402nm.
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| CN116120925A (en) * | 2023-01-30 | 2023-05-16 | 陕西科技大学 | High-yield nitrogen-sulfur co-doped fluorescent carbon quantum dot and preparation method and application thereof |
| CN116120925B (en) * | 2023-01-30 | 2024-01-26 | 陕西科技大学 | High-yield nitrogen-sulfur co-doped fluorescent carbon quantum dot and preparation method and application thereof |
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