CN111286325A - Carbon quantum dot emitting yellow fluorescence and preparation method and application thereof - Google Patents
Carbon quantum dot emitting yellow fluorescence and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000002795 fluorescence method Methods 0.000 title description 2
- ZAJAQTYSTDTMCU-UHFFFAOYSA-N 3-aminobenzenesulfonic acid Chemical compound NC1=CC=CC(S(O)(=O)=O)=C1 ZAJAQTYSTDTMCU-UHFFFAOYSA-N 0.000 claims abstract description 15
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Abstract
The invention discloses a preparation method of carbon quantum dots emitting yellow fluorescence, which comprises the following steps: 1) adding amino acid and aminobenzenesulfonic acid into water and uniformly mixing; 2) carrying out hydrothermal reaction in a hydrothermal reaction kettle at the reaction temperature of 100-240 ℃ for 2-10 h; 3) and after the reaction is finished, centrifuging the obtained product, taking supernate, dialyzing and drying to obtain the carbon quantum dots emitting yellow fluorescence. The carbon quantum which emits yellow fluorescence and is prepared by the inventionThe spot can be used for detecting iron ions (Fe) in a fluorescent and colorimetric dual mode3+)。
Description
Technical Field
The invention belongs to the field of biomedical materials, and relates to a carbon quantum dot emitting yellow fluorescence, and a preparation method and application thereof.
Background
Fluorescence sensing is widely used in the related fields of ion, small molecule, free radical, temperature and pH detection due to its excellent selectivity and sensitivity. The traditional fluorescence sensing generally adopts organic molecules, metal organic framework materials, metal nanoclusters, semiconductor metal quantum dots and the like, but the application fields of the materials are greatly limited due to poor water solubility and high toxicity. In order to overcome the defects of the above materials, carbon quantum dots have been widely studied and successfully used for fluorescence detection as an emerging luminescent carbon material. However, most of the existing fluorescence sensing based on carbon quantum dots are single detection modes, and the excitation and emission wavelengths of the carbon dots are relatively short, so that the application range of the carbon dots is limited to some extent.
On the other hand, iron, an essential element in the living body, is closely related to many physiological processes of the living body, such as enzyme metabolism, oxygen transfer and transport, and immune regulation. However, abnormal iron content can cause disturbance of metabolism of organisms and even cause a large number of diseases such as Alzheimer's disease, cardiopulmonary disease, cancer and the like, so that the realization of iron ion detection by using materials with good biocompatibility has important significance.
Disclosure of Invention
In view of this, the invention provides a carbon quantum dot emitting yellow fluorescence, and a preparation method and an application thereof.
The invention specifically provides the following technical scheme:
1. a preparation method of a carbon quantum dot emitting yellow fluorescence comprises the following steps:
4) adding amino acid and aminobenzenesulfonic acid into water and uniformly mixing;
5) carrying out hydrothermal reaction in a hydrothermal reaction kettle at the reaction temperature of 100-240 ℃ for 2-10 h;
6) and after the reaction is finished, centrifuging the obtained product, taking supernate, dialyzing and drying to obtain the carbon quantum dots emitting yellow fluorescence.
Further, the amino acid is one of L-aspartic acid, D-aspartic acid, L-glutamic acid or D-glutamic acid.
Further, the amino acid is L-aspartic acid.
Furthermore, the aminobenzenesulfonic acid is one of o-, m-, and p-diaminobenzenesulfonic acid.
Further, the aminobenzenesulfonic acid is 2, 5-diaminobenzenesulfonic acid.
Furthermore, the molar ratio of the amino acid to the aminobenzenesulfonic acid is 1: 2-2: 1.
Furthermore, the molar ratio of the amino acid to the aminobenzenesulfonic acid is 2: 1.
Further, the reaction temperature in the step 2) is 180 ℃, and the reaction time is 8 h.
2. The carbon quantum dot emitting yellow fluorescence is prepared according to the preparation method.
3. The carbon quantum dot capable of emitting yellow fluorescence detects Fe in a fluorescent mode and a colorimetric mode3+The application of (1).
The invention has the beneficial effects that: the invention successfully prepares a series of carbon quantum dots which have different amino acid and aminobenzenesulfonic acid contents and emit yellow fluorescence through hydrothermal reaction, selects the carbon quantum dots with higher luminous intensity by testing fluorescence performance on a fluorescence spectrophotometer, and applies the carbon quantum dots to Fe3+And detection can realize better fluorescence and colorimetric dual-mode detection.
Drawings
In order to make the purpose, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings:
FIG. 1 is a schematic diagram of the preparation and application of a carbon quantum dot emitting yellow fluorescence;
FIG. 2 is a powder X-ray diffraction pattern of carbon quantum dots emitting yellow fluorescence;
FIG. 3 is the result of an excitation-dependent emission spectrum test of a carbon quantum dot emitting yellow fluorescence;
FIG. 4 is a result of the emission intensity of a carbon quantum dot emitting yellow fluorescence;
FIG. 5 shows the detection of Fe by the fluorescent method using carbon quantum dots emitting yellow fluorescence3+The experimental results of (1);
FIG. 6 is a colorimetric method for detecting Fe using carbon quantum dots emitting yellow fluorescence3+The experimental results of (1).
Detailed Description
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1 preparation of yellow fluorescent-emitting carbon quanta
FIG. 1 is a schematic diagram of the preparation and application of a carbon quantum dot emitting yellow fluorescence, and the preparation of the carbon quantum dot emitting yellow fluorescence comprises the following steps:
mixing amino acid, aminobenzenesulfonic acid and water under stirring. Wherein the amino acid is L-aspartic acid (Asp, recorded as A), the aminobenzenesulfonic acid is 2, 5-diaminobenzenesulfonic acid (DABSA, recorded as D), and the total amount of the two substances is 0.6 mmol. By varying the initial charge ratios of Asp and DABSA, the resulting yellow-emitting carbon quantum dots were designed to contain different amino acid and aminobenzenesulfonic acid contents. Wherein when the initial charge ratio of Asp to DABSA was 2:1 (i.e., A:0.4mmol, D:0.2mmol), the resulting carbon quantum dot emitting yellow fluorescence was designated as CDs-A2D1(ii) a When the initial charge ratio of Asp to DABSA was 1:1 (i.e., A:0.3mmol, DABSA:0.3mmol), the resulting carbon quantum dot emitting yellow fluorescence was designated as CDs-A1D1(ii) a When the initial charge ratio of Asp to DABSA was 1:2 (i.e., A:0.2mmol, D:0.4mmol), the resulting carbon quantum dot emitting yellow fluorescence was designated as CDs-A1D2. And then adding water into the three groups of reactions with different charge ratios respectively, uniformly mixing the three groups of reactions in a hydrothermal reaction kettle, and reacting for 8 hours at 180 ℃ under a hydrothermal condition to obtain the carbon quantum dots which have different charge ratios and emit yellow fluorescence. The amount of solvent water used was 10 mL. After the reaction is finished, the obtained product is firstly centrifuged (10000rpm,5min), then the supernatant is taken and put into a dialysis bag (MWCO is 200Da), the dialysis is carried out for 2h, and finally the mixture is frozen and dried to obtain carbon quantum dots which have different feeding ratios and emit yellow fluorescence and are respectively named as CDs-A2D1、CDs-A1D1And CDs-A1D2Where 1 and 2 represent the original charge ratio of L-aspartic acid (Asp, denoted by A) and 2, 5-diaminobenzenesulphonic acid (DABSA, denoted by D).
Example 2 powder X-ray diffraction (XRD) characterization of yellow fluorescent-emitting carbon quanta
The yellow fluorescent carbon quantum dots CDs-A synthesized in example 12D1Freeze drying, grinding in mortar, adding into sample tank, pressing sample, and scanning in X-ray diffractometer. FIG. 2 shows carbon quantum dots CDs-A synthesized in example 12D1As can be seen from fig. 2, the synthesized carbon quantum dot has a characteristic diffraction peak at about 25 ° 2 θ, and the occurrence of the peak proves that the carbon quantum dot has an amorphous structure. As can be demonstrated from fig. 2, the carbon quantum dots emitting yellow fluorescence have been successfully synthesized.
Example 3 excitation-dependent emission Spectroscopy test results
The yellow fluorescent carbon quantum dots CDs-A synthesized in example 12D1Freeze-drying, preparing carbon quantum dot solution (concentration is 0.25mg/mL), adding 2mL into a fluorescence cuvette, placing into a fluorescence spectrophotometer, performing fluorescence test, changing the excitation wavelength of the carbon quantum dots at intervals of 20nm, and scanning to obtain emission spectra under different excitation wavelengths, as shown in FIG. 3. Wherein the slit width of the fluorescence spectrophotometer is set as 3nm, and the spectrum scanning speed is set as 600 nm/min. As can be seen from the third graph, the emission spectrum of the carbon quantum dot is gradually red-shifted with the increase of the excitation wavelength, and the typical excitation-dependent emission phenomenon of the carbon quantum dot is shown, further proving that the carbon quantum dot emitting yellow fluorescence has been successfully synthesized.
Example 4 fluorescence intensity test results
The three carbon quantum dots obtained in example 1 were dispersed in water under ultrasonic conditions, respectively, to prepare carbon quantum dot solutions with a concentration of 0.25mg/mL, 2mL of each solution was added to a fluorescence cuvette, and then placed in a fluorescence spectrophotometer, respectively, for fluorescence testing. Wherein the slit width of the fluorescence spectrophotometer is set to 3nm, and the spectrum scanning speed is set to 600nm/min. Three carbon quantum dots CDs-A obtained by testing2D1、CDs-A1D1And CDs-A1D2The fluorescence intensity of (A), (Asp) and (D) (DABSA) is shown in FIG. 4. As can be seen from FIG. 4, when the initial charge ratio of A (Asp) to D (DABSA) is 2:1, the fluorescence intensity of the obtained carbon quantum dot is the maximum, so that the carbon quantum dots CDs-A emitting yellow fluorescence synthesized at the initial charge ratio of A: D ═ 2:1 are used in the following examples2D1And (6) carrying out testing.
Example 5 fluorescence detection of Fe3+
The carbon quantum dots CDs-A prepared in example 12D1Dispersing the mixture into water to prepare a carbon quantum dot solution with the concentration of 200 mug/mL. Then preparing Fe with different molar concentrations3+The solution was then mixed with 0.25mL of carbon quantum dot solution and 0.25mL of Fe3+The solutions were added to 2mL of ultrapure water in sequence, mixed well and left for 2 minutes before being placed in a fluorescence spectrophotometer for spectral measurement. Wherein the slit width of the fluorescence spectrophotometer is set as 3nm, and the spectrum scanning speed is set as 600 nm/min. For different molar concentrations of Fe3+The detection of the solution adopts the same operation steps and test methods. Fluorescence spectrum with Fe3+The change in concentration is shown in FIG. 5, in which the fluorescence spectrum obtained by adding 0.25mL of the carbon quantum dot solution to 2.5mL of ultrapure water is recorded as Fe3+The concentration was 0. mu.M. As can be seen from FIG. 5, with Fe3+The intensity of the fluorescence spectrum gradually decreases, proving that Fe3+The fluorescence intensity of the carbon quantum dots can be effectively quenched, so that the method is used for fluorescence detection.
EXAMPLE 6 colorimetric detection of Fe3+
The carbon quantum dots CDs-A prepared in example 12D1Dispersing the mixture into water to prepare a carbon quantum dot solution with the concentration of 200 mug/mL. Then preparing Fe with different molar concentrations3+The solution was then mixed with 0.25mL of carbon quantum dot solution and 0.25mL of Fe3+The solution is added into 2mL of ultrapure water in sequence, mixed evenly and stood for 2 minutes, and the photo of the mixed solution is directly taken under the sunlight, and for Fe with different molar concentrations3+The detection of the solution is carried out by the same methodThe operation steps and the photographing method. As shown in fig. 6, it is understood from fig. 6 that the color of the carbon quantum dot solution gradually changes from colorless to red as the iron ion concentration increases. Because the surface of the synthesized carbon quantum dot contains a large number of functional groups such as amino, carboxyl, sulfonic acid groups and the like, the synthesized carbon quantum dot can form a stable ground state compound with iron ions, and the formation of the compound can cause the ultraviolet-visible absorption spectrum of the carbon quantum dot solution to generate red shift, so that the color of the solution gradually turns red, and the synthesized carbon quantum dot solution can be well used for colorimetric detection of Fe3+。
In conclusion, the carbon quantum dots emitting yellow fluorescence can be used for detecting Fe in a fluorescent and colorimetric dual mode3+Therefore, the method has potential application value in the diagnosis of diseases related to iron ions and has important significance in the field of biomedicine.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of a carbon quantum dot emitting yellow fluorescence is characterized by comprising the following steps:
1) adding amino acid and aminobenzenesulfonic acid into water and uniformly mixing;
2) carrying out hydrothermal reaction in a hydrothermal reaction kettle at the reaction temperature of 100-240 ℃ for 2-10 h;
3) and after the reaction is finished, centrifuging the obtained product, taking supernate, dialyzing and drying to obtain the carbon quantum dots emitting yellow fluorescence.
2. The method of claim 1, wherein the amino acid is one of L-aspartic acid, D-aspartic acid, L-glutamic acid, or D-glutamic acid.
3. The method of claim 1, wherein the amino acid is L-aspartic acid.
4. The method of claim 1, wherein the aminobenzenesulfonic acid is one of o-, m-, and p-diaminobenzenesulfonic acid.
5. The method of claim 1, wherein the aminobenzenesulfonic acid is 2, 5-diaminobenzenesulfonic acid.
6. The method for preparing a carbon quantum dot emitting yellow fluorescence according to claim 1, wherein the molar ratio of the amino acid to the aminobenzenesulfonic acid is 1:2 to 2: 1.
7. The method of claim 1, wherein the molar ratio of the amino acid to the aminobenzenesulfonic acid is 2: 1.
8. The method for preparing a carbon quantum dot emitting yellow fluorescence according to claim 1, wherein the reaction temperature in the step 2) is 180 ℃ and the reaction time is 8 hours.
9. A carbon quantum dot emitting yellow fluorescence, which is produced by the production method according to any one of claims 1 to 8.
10. The method of claim 9 for detecting Fe in a fluorescent and colorimetric dual mode by using a yellow fluorescent carbon quantum dot3+The application of (1).
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| CN113046074A (en) * | 2021-03-25 | 2021-06-29 | 中国科学技术大学 | Method for synthesizing high-brightness fluorescent carbon quantum dots and application |
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| CN109504372A (en) * | 2018-11-07 | 2019-03-22 | 中国农业大学 | A kind of fluorescent carbon quantum dot solution and its preparation method and application |
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| CN104804734A (en) * | 2015-04-01 | 2015-07-29 | 河南师范大学 | Synthesis method for sulfur-nitrogen-doped fluorescent carbon dots according to one-step microwave method |
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| CN109504372A (en) * | 2018-11-07 | 2019-03-22 | 中国农业大学 | A kind of fluorescent carbon quantum dot solution and its preparation method and application |
| CN109321240A (en) * | 2018-11-23 | 2019-02-12 | 江南大学 | A kind of fluorescent orange carbon dots and preparation method thereof |
| CN110172344A (en) * | 2019-04-28 | 2019-08-27 | 山西大学 | For monitoring the fluorescent carbon quantum dot and its preparation method and application of acidic environment pH |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113046074A (en) * | 2021-03-25 | 2021-06-29 | 中国科学技术大学 | Method for synthesizing high-brightness fluorescent carbon quantum dots and application |
| CN113046074B (en) * | 2021-03-25 | 2022-05-17 | 中国科学技术大学 | Method for synthesizing high-brightness fluorescent carbon quantum dots and application |
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