CN111704901A - Preparation method and application of boron-sulfur doped carbon quantum dots - Google Patents
Preparation method and application of boron-sulfur doped carbon quantum dots Download PDFInfo
- Publication number
- CN111704901A CN111704901A CN201910205103.4A CN201910205103A CN111704901A CN 111704901 A CN111704901 A CN 111704901A CN 201910205103 A CN201910205103 A CN 201910205103A CN 111704901 A CN111704901 A CN 111704901A
- Authority
- CN
- China
- Prior art keywords
- boron
- sulfur
- source
- carbon quantum
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Immunology (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Optics & Photonics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Materials Engineering (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention provides a preparation method and application of boron-sulfur-doped carbon quantum dots, namely a method for high-sensitivity detection of dopamine by using the boron-sulfur-doped carbon quantum dots, which comprises the following steps: after a carbon source, a boron source and a sulfur source are mixed, the carbon source, the boron source and the sulfur source are uniformly mixed in a liquid phase mixing mode, then preliminary doping of heteroatoms is realized through a microwave preliminary reaction, and then a boron-sulfur doped carbon quantum dot is directly prepared through a one-step hydrothermal microwave reaction.
Description
Technical Field
The invention relates to the technical field of fluorescent probes, in particular to a carbon quantum dot fluorescent probe, and specifically relates to a preparation method and application of the carbon quantum dot fluorescent probe for detecting dopamine.
Background
The fluorescent probe is a detection means with wide application, and generally, the fluorescence intensity of the fluorescent probe can obviously change along with the change of the concentration of an object to be detected. Therefore, it has been extensively and deeply studied in the fields of industrial and agricultural production, scientific research, environmental science, biomedicine, and the like. At present, common fluorescent probes are mainly classified into two types, namely non-carbon-based fluorescent probes and carbon-based fluorescent probes, the non-carbon-based fluorescent probes mainly comprise semiconductor quantum dots of various selenides and sulfides, and the semiconductor quantum dots have great obstacles for wide application due to potential high toxicity, instability and poor biocompatibility. Compared with a non-carbon-based fluorescent probe, the carbon-based fluorescent probe has excellent properties such as high sensitivity, good chemical stability, excellent biocompatibility, nontoxicity and the like. Therefore, the carbon-based fluorescent probe, especially the carbon quantum dot fluorescent probe, has practical application value in the fields of biological labeling, medical diagnosis, pollutant detection and the like.
In 2000, the swedish scientist Carlsson identified dopamine as the emissary of intracerebral information, a finding that led him to the current year of the nobel prize for medicine. Dopamine is a nerve-conducting substance, can transmit happy and happy information, and plays an important role in the central nervous system. If the dopamine-producing neurons die, dopamine in the body becomes abnormal, which can cause muscle stiffness and tremor, and speech ambiguity, etc., i.e., parkinson's disease. In addition, studies have shown that dopamine stimulates people's desire to purchase and produces a sweet feeling of love.
Therefore, the method has important significance for efficiently and sensitively detecting the dopamine.
Disclosure of Invention
The invention aims to provide a carbon quantum dot fluorescent probe capable of efficiently and sensitively detecting dopamine, which has the characteristics of high dopamine identification degree and sensitive reaction. Even under the condition of extremely low dopamine content, the obvious quenching phenomenon still can occur, and a good linear relation is kept between the quenching efficiency and the dopamine concentration.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of boron-sulfur doped carbon quantum dots for dopamine detection comprises the following steps:
(1) firstly, weighing a proper amount of carbon source, boron source and sulfur source, mixing and stirring the carbon source, the boron source and the sulfur source in deionized water uniformly, then centrifugally drying, and grinding and refining the obtained solid mixture in an agate mortar;
(2) putting the solid mixture obtained in the step (1) into a microwave oven for preliminary carbonization doping reaction;
(3) taking the product after the reaction in the step (2) out of the microwave oven, then grinding and refining the product by using the mortar again, and then dispersing the product in deionized water again, wherein the water-solid volume-mass ratio is 3-5: 1;
(4) transferring the mixture obtained in the step (3) to a microwave reactor, setting a temperature-raising program, raising the temperature to 160-200 ℃, and preserving the temperature for 10-30 min;
(5) after the reaction is finished, after the reaction container is naturally cooled to room temperature, centrifuging, filtering and washing the product.
Preferably, the carbon source is oxalic acid, the boron source is boric acid, and the sulfur source is thiourea.
Preferably, the mass ratio of the carbon source, the boron source and the sulfur source in the step (1) is (4-6): (2-2.5): 1.
Preferably, the stirring in step (1) is one of mechanical stirring and manual stirring.
Preferably, the microwave power in step (2) is 100-.
Preferably, filter paper is used as a reaction matrix in the step (2), and the grinding substance in the step (1) is uniformly spread on the surface.
Preferably, the preliminary reaction in the step (2) can dope part of boron and sulfur sources, and the subsequent thorough reaction is performed, so that the preparation of the high-content boron and sulfur doped carbon quantum dots is facilitated, and the step plays an important role in the final product.
Preferably, the microwave reactor in step (4) is a hydrothermal microwave reactor.
Preferably, the washing in step (5) comprises washing with deionized water and ethanol alternately.
The boron-sulfur doped carbon quantum dot prepared by the invention can be used as a fluorescent probe, especially used for detecting dopamine, and shows better fluorescence quenching performance and sensitive selectivity.
The principle of the invention is that the high-performance modification of the carbon quantum dots is realized through the doping of boron-sulfur heteroatoms, and particularly the strong promotion effect on the electron-hole separation performance of the carbon quantum dots is realized, and in the contact process with dopamine, the dopamine is converted into a dopamine quinone substance, and the transfer of electrons on the surfaces of the dopamine and the carbon quantum dots can be realized, so that the fluorescence quenching of the carbon quantum dots is finally realized, and the detection purpose of the dopamine is also achieved. The preliminary charring doping used in the present invention has an important effect on the final product performance, and the applicant has found that the detection line is only 200nM under the same parameters if the reaction is direct.
Compared with the prior art, the invention has the advantages that:
1) a high-performance fluorescent probe is prepared by introducing a preliminary carbonization reaction and combining a reaction instrument of hydrothermal microwaves;
2) boron and sulfur heteroatoms are introduced into the carbon quantum dots, and the carbon quantum dots are modified, so that the electron-hole separation efficiency of the carbon quantum dots is improved, and the high-sensitivity detection of dopamine is realized;
3) the method for preparing the boron-sulfur-carbon quantum dots is simple, does not need to use toxic and harmful substances, and meets the development requirement of green chemistry.
Drawings
Fig. 1 is a transmission electron microscope photograph of boron-sulfur doped carbon quantum dots prepared according to an embodiment of the present invention, which is a photograph at a low magnification and a photograph at a high magnification, respectively;
fig. 2 shows fluorescence intensity spectra of the boron-sulfur doped carbon quantum dots prepared by the invention at different dopamine concentrations, wherein the concentrations increase from top to bottom.
Detailed Description
In order to make the content of the present invention more apparent to those skilled in the art, the following detailed description of the technical solutions of the present invention is provided with reference to specific embodiments.
Example 1
Respectively weighing oxalic acid, boric acid and thiourea according to the mass ratio of 4:2:1, putting the oxalic acid, boric acid and thiourea into a beaker, adding deionized water, uniformly stirring by using a glass rod, centrifuging by using a 50mL centrifuge tube, drying, and grinding for 20min by using an agate mortar. Then, the abrasive is laid flat on filter paper, the power of a microwave oven is set to be 300W, the abrasive is radiated for 3min (here, because the raw materials for reaction are easy to decompose, the reaction time cannot be prolonged), and after the reaction is finished, the abrasive is taken out of the microwave oven and then collected in a mortar to be ground for 20min again. And then, completely dissolving the substances by using 30mL of deionized water, transferring the dissolved substances into a hydrothermal microwave reaction container, heating to 180 ℃ for reaction for 30min, and after the reaction is finished, naturally cooling the reaction container to room temperature, and then carrying out conventional centrifugation, filtration and washing on the product.
Example 2
Respectively weighing oxalic acid, boric acid and thiourea according to the mass ratio of 4:2:1, putting the oxalic acid, boric acid and thiourea into a beaker, adding deionized water, uniformly stirring by using a glass rod, centrifuging by using a 50mL centrifuge tube, drying, and grinding for 20min by using an agate mortar. Then, the abrasive is laid flat on filter paper, the power of a microwave oven is set to be 400W, the abrasive is radiated for 2min (here, because the raw materials for reaction are easy to decompose, the reaction time cannot be prolonged), and after the reaction is finished, the abrasive is taken out of the microwave oven and then collected in a mortar for grinding for 20min again. And then, completely dissolving the substances by using 30mL of deionized water, transferring the dissolved substances into a hydrothermal microwave reaction container, heating to 180 ℃ for reaction for 30min, and after the reaction is finished, naturally cooling the reaction container to room temperature, and then carrying out conventional centrifugation, filtration and washing on the product.
Example 3
Respectively weighing oxalic acid, boric acid and thiourea according to the mass ratio of 6:2:1, putting the oxalic acid, boric acid and thiourea into a beaker, adding deionized water, uniformly stirring by using a glass rod, centrifuging by using a 50mL centrifugal tube, drying, and grinding for 20min by using an agate mortar. Then, the abrasive is laid flat on filter paper, the power of a microwave oven is set to be 200W, the abrasive is radiated for 4min (here, because the raw materials for reaction are easy to decompose, the reaction time cannot be prolonged), and after the reaction is finished, the abrasive is taken out of the microwave oven and then collected in a mortar for grinding for 20min again. And then, completely dissolving the substances by using 40mL of deionized water, transferring the dissolved substances into a hydrothermal microwave reaction container, heating to 180 ℃ for reaction for 30min, and after the reaction is finished, naturally cooling the reaction container to room temperature, and then carrying out conventional centrifugation, filtration and washing on the product.
Example 4
Respectively weighing oxalic acid, boric acid and thiourea according to the mass ratio of 4:2:1, putting the oxalic acid, boric acid and thiourea into a beaker, adding deionized water, uniformly stirring by using a glass rod, centrifuging by using a 50mL centrifuge tube, drying, and grinding for 20min by using an agate mortar. Then, the abrasive is laid flat on filter paper, the power of a microwave oven is set to be 400W, the abrasive is radiated for 2min (here, because the raw materials for reaction are easy to decompose, the reaction time cannot be prolonged), and after the reaction is finished, the abrasive is taken out of the microwave oven and then collected in a mortar for grinding for 20min again. And then, completely dissolving the substances by using 30mL of deionized water, transferring the dissolved substances into a hydrothermal microwave reaction container, heating to 200 ℃ for reaction for 10min, and after the reaction is finished, naturally cooling the reaction container to room temperature, and then carrying out conventional centrifugation, filtration and washing on the product.
It is obvious that the above examples are only examples for clearly illustrating the present invention, and are not intended to limit the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (8)
1. A preparation method of boron-sulfur doped carbon quantum dots for dopamine detection is characterized by comprising the following steps:
(1) firstly, weighing a proper amount of a carbon source, a boron source and a sulfur source, uniformly mixing and stirring the carbon source, the boron source and the sulfur source in deionized water, then centrifugally drying, and grinding and refining the obtained solid mixture in an agate mortar, wherein the carbon source is oxalic acid, the boron source is boric acid, and the sulfur source is thiourea; the mass ratio of the oxalic acid to the boric acid to the thiourea is (4-6) to (2-2.5) to 1;
(2) putting the solid mixture obtained in the step (1) into a microwave oven for preliminary carbonization doping reaction;
(3) taking the product after the reaction in the step (2) out of the microwave oven, then grinding and refining the product by using the mortar again, and then dispersing the product in deionized water again, wherein the water-solid volume-mass ratio is 3-5: 1;
(4) transferring the mixture obtained in the step (3) to a microwave reactor, setting a temperature-raising program, raising the temperature to 160-200 ℃, and preserving the temperature for 10-30 min;
(5) after the reaction is finished, after the reaction container is naturally cooled to room temperature, centrifuging, filtering and washing the product.
2. The method for preparing boron-sulfur doped carbon quantum dots for dopamine detection according to claim 1, wherein the method comprises the following steps: the stirring in the step (1) is one of mechanical stirring or manual stirring.
3. The method for preparing boron-sulfur doped carbon quantum dots for dopamine detection according to claim 1, wherein the method comprises the following steps: the power of the microwave oven in the step (2) is 100-500W, and the initial reaction time is 1-5 min.
4. The method for preparing boron-sulfur doped carbon quantum dots for dopamine detection according to claim 1, wherein the method comprises the following steps: in the step (2), filter paper is used as a reaction substrate, and the grinding substance in the step (1) is uniformly spread on the surface.
5. The method for preparing boron-sulfur doped carbon quantum dots for dopamine detection according to claim 1, wherein the method comprises the following steps: in the step (2), the preliminary reaction is carried out, so that partial boron and sulfur sources can be doped.
6. The method for preparing boron-sulfur doped carbon quantum dots for dopamine detection according to claim 1, wherein the method comprises the following steps: the microwave reactor in the step (4) is a hydrothermal microwave reactor.
7. The boron-sulfur doped carbon quantum dot of any one of claims 1-6.
8. The boron-sulfur doped carbon quantum dot according to claim 7, which is used for a fluorescent probe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910205103.4A CN111704901A (en) | 2019-03-18 | 2019-03-18 | Preparation method and application of boron-sulfur doped carbon quantum dots |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910205103.4A CN111704901A (en) | 2019-03-18 | 2019-03-18 | Preparation method and application of boron-sulfur doped carbon quantum dots |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111704901A true CN111704901A (en) | 2020-09-25 |
Family
ID=72536310
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910205103.4A Withdrawn CN111704901A (en) | 2019-03-18 | 2019-03-18 | Preparation method and application of boron-sulfur doped carbon quantum dots |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111704901A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110105952A (en) * | 2019-05-21 | 2019-08-09 | 成晓艳 | A kind of preparation method and applications of boron sulfur doping carbon quantum dot |
| CN113247879A (en) * | 2021-04-16 | 2021-08-13 | 昆明理工大学 | Method for preparing carbonized polymer quantum dots through spray pyrolysis |
-
2019
- 2019-03-18 CN CN201910205103.4A patent/CN111704901A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110105952A (en) * | 2019-05-21 | 2019-08-09 | 成晓艳 | A kind of preparation method and applications of boron sulfur doping carbon quantum dot |
| CN113247879A (en) * | 2021-04-16 | 2021-08-13 | 昆明理工大学 | Method for preparing carbonized polymer quantum dots through spray pyrolysis |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104789217B (en) | Amphipathy carbon quantum dot and preparation method thereof | |
| CN103273079B (en) | Gold nanoflower preparing method and application of gold nanoflowers | |
| CN103588189A (en) | Egg-based method for realizing hydrothermal synthesis of carbon quantum dots | |
| CN111704901A (en) | Preparation method and application of boron-sulfur doped carbon quantum dots | |
| CN105567227A (en) | Method for extracting graphene quantum dots from coffee-ground solid waste | |
| CN107603611A (en) | One kind has Catalyzed Synthesis By Peroxidase active fluoro carbon quantum dot and preparation method thereof | |
| CN104071769A (en) | Method for preparing fluorescent carbon point by virtue of chemical oxidation method, fluorescent carbon point and application of fluorescent carbon point | |
| CN108872171A (en) | A kind of application of fluorescent carbon point and preparation method thereof and detection tetracycline | |
| CN106829920A (en) | A kind of green fluorescence carbon quantum dot material and preparation method thereof | |
| CN109437154A (en) | A method of the controllable carbon quantum dot of energy band is prepared by raw material of coal | |
| CN111154485A (en) | Preparation of sulfur-nitrogen double-doped carbon quantum dot and application of sulfur-nitrogen double-doped carbon quantum dot in tetracycline detection | |
| CN105670617A (en) | Simple efficient one-step method for batch preparation of nitrogen-doped petroleum coke-based carbon quantum dots | |
| CN106883850A (en) | A kind of carbon quantum dot fluorescence labeling material and preparation method thereof | |
| CN102502610A (en) | Simple method for preparing a large amount of graphene | |
| CN110451488A (en) | A kind of method of Passivation modified cane molasses graphene quantum dot | |
| CN103616357A (en) | Visual biosensor device and preparation method thereof | |
| CN107572505A (en) | A kind of preparation method of Ag doping graphene quantum dot | |
| CN107954478A (en) | A kind of liquid solution method for preparing molybdenum disulfide quantum dot | |
| CN103878386A (en) | Method for preparing fluorescent silver nano-clusters | |
| CN102208755A (en) | Dry etching method for preparing graphene quantum dots through using ultraviolet (UV)-light | |
| CN106517130A (en) | Method for preparing hydroxyl iron phosphate micro-nano powder material by using phosphorus-rich biomass | |
| CN104560037B (en) | Method of preparing carbon quantum dots with high quantum yield in oil phase | |
| CN108441214A (en) | A kind of preparation method of more Heteroatom doping type carbon quantum dot fluorescence probes | |
| CN117487540A (en) | Microwave-assisted synthesis method and application of nitrogen-iron-manganese co-doped carbon point | |
| CN102430387B (en) | Method for preparing novel carbon material at low temperature for processing dye waste water |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20200925 |
|
| WW01 | Invention patent application withdrawn after publication |