CN113549450A - Potassium-nitrogen co-doped carbon dots based on flint pericarp and preparation method and application thereof - Google Patents
Potassium-nitrogen co-doped carbon dots based on flint pericarp and preparation method and application thereof Download PDFInfo
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- 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"
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- 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"
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Abstract
The invention provides a potassium-nitrogen co-doped carbon dot based on flint pericarp and a preparation method and application thereof. The preparation method takes the flint peel and ethylenediamine as precursors and secondary water as a solvent, and prepares the potassium-nitrogen co-doped carbon dots through one-step hydrothermal reaction. The method for preparing the carbon quantum dots is simple, low in cost and easy in obtaining of raw materials. The waste steamship peel is used as a raw material to synthesize the potassium-nitrogen co-doped carbon dots, so that the biomass waste can be reasonably utilized, the energy is saved, and the environment is protected. The prepared carbon quantum dots have excellent optical properties, and can realize the identification and selective detection of tetracycline antibiotics based on different detection mechanisms of fluorescence enhancement, fluorescence ratio and fluorescence quenching. The carbon quantum dot can be used for detecting the contents of chlortetracycline hydrochloride, tetracycline and oxytetracycline in milk, honey, fish and pork.
Description
Technology neighborhood
The invention relates to a luminescent nano material, in particular to a potassium-nitrogen co-doped carbon dot based on flint pericarp and a preparation method and application thereof.
Background
The synthesis, properties and applications of CDs have advanced greatly over the past few decades. Researchers have synthesized a large number of carbon dots using small organic molecules, macromolecules, biomass, and the like as carbon sources. Compared with other carbon sources, the biomass carbon source is an eco-friendly natural product, and has many advantages in the preparation of carbon dots, including low price, readily available raw materials, greenness and abundance. In addition, carbon dots produced from natural biomass can convert low value biomass waste into valuable nanomaterials. Therefore, the method not only saves energy, but also is beneficial to environmental protection, and plays a significant role in realizing the development mode of circular economy and social sustainable development in China. In recent years, various biomasses have been used as raw materials for producing carbon dots, for example, walnut shells, egg shells, rice hulls, lychee seeds, hair, crab shells, bee pollen. Carbon dots prepared using biomass have been widely used as bio-imaging markers, sensors, drug delivery and other applications.
Tetracycline antibiotics (TCs), a versatile broad spectrum antibiotic, are widely used as animal feed additives, as well as sterilization and therapeutic agents for infectious diseases in humans due to their high efficacy and low cost. However, abuse and recalcitrance of TCs can produce residues in animal products, aqueous environments and soils, posing a threat to food safety, environmental protection and human health. Therefore, it is of great importance to develop a simple and effective method for selectively and sensitively detecting the residual TC in food, environment and drugs. Patent publication No. CN 111154485A discloses that a sulfur-nitrogen double-doped carbon quantum dot detects tetracycline antibiotics (tetracycline, aureomycin and oxytetracycline) in a fluorescence quenching mode, but cannot realize selective identification and detection of the three tetracycline antibiotics when two or three of the three antibiotics exist at the same time. Therefore, it is necessary to develop a fluorescence sensor that discriminates and selectively detects TCs by different changes in the signal of fluorescence.
Disclosure of Invention
The invention aims to provide a potassium-nitrogen co-doped carbon dot based on turkey pericarp and a preparation method and application thereof. The prepared carbon quantum dot has excellent optical properties, can realize the identification and selective detection of tetracycline antibiotics based on different fluorescence detection mechanisms, and can be used for detecting the contents of aureomycin hydrochloride (CTC), Tetracycline (TC) and Oxytetracycline (OTC) in actual samples such as milk, honey, fish and pork.
The invention provides a potassium-nitrogen co-doped carbon dot based on flint pericarp and a preparation method thereof, which are characterized by comprising the following steps:
1) putting the steamship peel in a beaker, adding ultrapure water, adding ethylenediamine into the solution, and performing ultrasonic treatment to obtain a mixed solution; the mass ratio of the flint peel, the ethylenediamine and the ultrapure water is 0.2-1:2.88-14.4: 16;
2) placing the mixed solution in a high-pressure reaction kettle, carrying out hydrothermal reaction for 2-4h at the temperature of 140-160 ℃, then naturally cooling the reaction kettle to room temperature, and filtering with filter paper to remove large particles in the reacted solution; then, further filtering the dark brown filtrate by a cylindrical filter membrane filter (0.22 mu m) to obtain a potassium-nitrogen co-doped carbon dot aqueous solution prepared from the turkey pericarp;
3) and (3) placing the carbon quantum dot aqueous solution in a refrigerator at 4 ℃.
The mass ratio of the flint peel, the ethylenediamine and the ultrapure water in the step 1) is preferably 1:14.4: 16.
The hydrothermal reaction temperature in the step 2) is preferably 150 ℃, and the reaction time is preferably 3 h.
The potassium-nitrogen co-doped carbon dots prepared by the method can be used for identifying and detecting aureomycin hydrochloride, tetracycline and oxytetracycline, and are based on three different detection mechanisms of fluorescence enhancement, fluorescence ratio type and fluorescence quenching form.
The potassium-nitrogen co-doped carbon dots are used for identifying and detecting aureomycin hydrochloride and oxytetracycline, and are based on fluorescence enhancement and fluorescence quenching mechanisms, namely aureomycin hydrochloride and oxytetracycline are respectively and gradually dripped into a potassium-nitrogen doped carbon dot solution, the fluorescence intensity of the potassium-nitrogen co-doped carbon dots is respectively enhanced and reduced for identification, a working curve is made according to the change of the fluorescence intensity, and the aureomycin hydrochloride and the oxytetracycline are further respectively and quantitatively detected.
The potassium-nitrogen co-doped carbon dots are used for identifying and detecting tetracycline and are based on a fluorescence ratio type mechanism, namely, a mixed solution of europium nitrate or europium fluoride or europium chloride hexahydrate or europium nitrate hexahydrate and sodium citrate is added into a potassium-nitrogen doped carbon dot solution, tetracycline is identified by adding tetracycline after the fluorescence intensity changes in a ratio type manner, a working curve is prepared according to the change of the fluorescence intensity, and the tetracycline is further quantitatively detected.
The potassium-nitrogen co-doped carbon dots can also be used as a sensor for detecting the content of chlortetracycline hydrochloride, tetracycline and oxytetracycline in actual samples such as milk, honey, fish and pork.
Compared with the prior art, the invention has the beneficial effects that:
the invention synthesizes a potassium-nitrogen co-doped carbon dot by using waste steamship peel as a carbon source and ethylenediamine as a nitrogen source through a one-step hydrothermal method.
The waste steamship peel is used as biomass waste, so that waste is changed into valuable, energy is saved, and the method is green and environment-friendly. The firer pericarp surface contains a large amount of potassium elements, the ethylenediamine is used as a common reagent, the source is wide, and the firer pericarp surface contains a large amount of-NH-functional groups, so that the carbon dot surface contains rich potassium nitrogen functional groups.
The quantum yield of the potassium-nitrogen-codoped carbon dots is high, and the relative quantum yield of the obtained potassium-nitrogen-codoped carbon dots is generally between 8 and 15 percent by taking quinine sulfate (the quantum yield is 54 percent).
The potassium-nitrogen co-doped carbon dots prepared by the method can be used for detecting the contents of chlortetracycline hydrochloride, tetracycline and oxytetracycline in actual samples of milk, honey, fish and pork.
In a word, the method has the advantages of simple operation process, easily obtained raw materials, environmental protection, low requirement on preparation conditions, stable optical property and high fluorescence quantum yield of the obtained potassium-nitrogen co-doped carbon dots, and the carbon dots are used as fluorescence sensors to detect tetracycline antibiotics, have different sensing mechanisms and different fluorescence signals, and realize the identification and detection of the tetracycline antibiotics. And can be used for detecting the content of chlortetracycline hydrochloride, tetracycline and oxytetracycline hydrochloride in actual samples such as milk, honey, fish and pork.
Drawings
FIG. 1 is a chart of the UV absorption spectrum and fluorescence excitation and emission spectrum of potassium-nitrogen co-doped carbon dots based on turkey pericarp prepared in example 1
FIG. 2 is a graph showing the dependence of fluorescence excitation wavelength of K-N co-doped carbon dots based on Pyrolusitum pericarp prepared in example 1
FIG. 3 is a general spectrum of XPS spectra of K-N co-doped carbon dots based on Pyrola pericarp prepared in example 1
FIG. 4 is a fluorescence spectrum titration chart and working curve chart of oxytetracycline for potassium-nitrogen co-doped carbon dot detection based on turkey pericarp prepared in example 1
FIG. 5 is a fluorescence spectrum titration chart and working curve chart of chlortetracycline hydrochloride detected by potassium-nitrogen co-doped carbon dots based on turkey pericarp prepared in example 1
Detailed Description
The present invention will be described in detail with reference to the following examples and the accompanying drawings, wherein the examples show detailed embodiments and specific operation procedures, but the scope of the present invention is not limited to the following examples.
Example 1
1) Placing 0.5g of waste steamship peel in a beaker, adding 8mL of ultrapure water, adding 8mL of ethylenediamine into the solution, and performing ultrasonic treatment to obtain a mixed solution;
2) putting the mixed solution into a high-pressure reaction kettle, and carrying out hydrothermal reaction for 3h at 150 ℃;
3) after the reaction is stopped, naturally cooling the reaction kettle to room temperature, and filtering with filter paper to remove large particles in the reacted solution; then, further filtering the dark brown filtrate by a cylindrical filter membrane filter (0.22 mu m) to obtain a potassium-nitrogen co-doped carbon dot aqueous solution prepared from the turkey pericarp;
4) the carbon quantum dot aqueous solution is stored in a refrigerator at 4 ℃ for standby, and the relative quantum yield (based on quinine sulfate) is 15%.
The characteristics and the application of the potassium-nitrogen co-doped carbon dots are shown in figures 1-5.
Example 2
1) Placing 0.5g of waste steamship peel in a beaker, adding 8mL of ultrapure water, adding 8mL of ethylenediamine into the solution, and performing ultrasonic treatment to obtain a mixed solution;
2) putting the mixed solution into a high-pressure reaction kettle, and carrying out hydrothermal reaction for 2h at 150 ℃;
3) after the reaction is stopped, naturally cooling the reaction kettle to room temperature, and filtering with filter paper to remove large particles in the reacted solution; then, further filtering the dark brown filtrate by a cylindrical filter membrane filter (0.22 mu m) to obtain a potassium-nitrogen co-doped carbon dot aqueous solution prepared from the turkey pericarp;
4) the carbon quantum dot aqueous solution is stored in a refrigerator at 4 ℃ for standby, and the relative quantum yield (based on quinine sulfate) is 12.6%.
Example 3
1) Placing 0.5g of waste steamship peel in a beaker, adding 8mL of ultrapure water, adding 8mL of ethylenediamine into the solution, and performing ultrasonic treatment to obtain a mixed solution;
2) putting the mixed solution into a high-pressure reaction kettle, and carrying out hydrothermal reaction for 4h at 150 ℃;
3) after the reaction is stopped, naturally cooling the reaction kettle to room temperature, and filtering with filter paper to remove large particles in the reacted solution; then, further filtering the dark brown filtrate by a cylindrical filter membrane filter (0.22 mu m) to obtain a potassium-nitrogen co-doped carbon dot aqueous solution prepared from the turkey pericarp;
4) the carbon quantum dot aqueous solution is stored in a refrigerator at 4 ℃ for standby, and the relative quantum yield (based on quinine sulfate) is 13%.
Example 4
1) Placing 0.5g of waste steamship peel in a beaker, adding 8mL of ultrapure water, adding 8mL of ethylenediamine into the solution, and performing ultrasonic treatment to obtain a mixed solution;
2) putting the mixed solution into a high-pressure reaction kettle, and carrying out hydrothermal reaction for 3h at 180 ℃;
3) after the reaction is stopped, naturally cooling the reaction kettle to room temperature, and filtering with filter paper to remove large particles in the reacted solution; then, further filtering the dark brown filtrate by a cylindrical filter membrane filter (0.22 mu m) to obtain a potassium-nitrogen co-doped carbon dot aqueous solution prepared from the turkey pericarp;
4) the carbon quantum dot aqueous solution is stored in a refrigerator at 4 ℃ for standby, and the relative quantum yield (based on quinine sulfate) is 13.2%.
Example 5
1) Placing 0.5g of waste steamship peel in a beaker, adding 8mL of ultrapure water, adding 8mL of ethylenediamine into the solution, and performing ultrasonic treatment to obtain a mixed solution;
2) putting the mixed solution into a high-pressure reaction kettle, and carrying out hydrothermal reaction for 3h at 120 ℃;
3) after the reaction is stopped, naturally cooling the reaction kettle to room temperature, and filtering with filter paper to remove large particles in the reacted solution; then, further filtering the dark brown filtrate by a cylindrical filter membrane filter (0.22 mu m) to obtain a potassium-nitrogen co-doped carbon dot aqueous solution prepared from the turkey pericarp;
4) the carbon quantum dot aqueous solution is stored in a refrigerator at 4 ℃ for standby, and the relative quantum yield (based on quinine sulfate) is 10.5%.
Example 6
1) Placing 0.5g of waste steamship peel in a beaker, adding 8mL of ultrapure water, adding 1.6mL of ethylenediamine into the solution, and performing ultrasonic treatment to obtain a mixed solution;
2) putting the mixed solution into a high-pressure reaction kettle, and carrying out hydrothermal reaction for 3h at 150 ℃;
3) after the reaction is stopped, naturally cooling the reaction kettle to room temperature, and filtering with filter paper to remove large particles in the reacted solution; then, further filtering the dark brown filtrate by a cylindrical filter membrane filter (0.22 mu m) to obtain a potassium-nitrogen co-doped carbon dot aqueous solution prepared from the turkey pericarp;
4) the carbon quantum dot aqueous solution is stored in a refrigerator at 4 ℃ for standby, and the relative quantum yield (based on quinine sulfate) is 8%.
Example 7
1) Placing 0.1g of waste steamship peel in a beaker, adding 8mL of ultrapure water, adding 5mL of ethylenediamine into the solution, and performing ultrasonic treatment to obtain a mixed solution;
2) putting the mixed solution into a high-pressure reaction kettle, and carrying out hydrothermal reaction for 3h at 150 ℃;
3) after the reaction is stopped, naturally cooling the reaction kettle to room temperature, and filtering with filter paper to remove large particles in the reacted solution; then, further filtering the dark brown filtrate by a cylindrical filter membrane filter (0.22 mu m) to obtain a potassium-nitrogen co-doped carbon dot aqueous solution prepared from the turkey pericarp;
4) the carbon quantum dot aqueous solution is stored in a refrigerator at 4 ℃ for standby, and the relative quantum yield (based on quinine sulfate) is 11%.
Example 8
The potassium-nitrogen co-doped carbon dots based on the turkey pericarp prepared in example 1 was used for detecting oxytetracycline, and as shown in fig. 4, an oxytetracycline solution was gradually added dropwise to the potassium-nitrogen co-doped carbon dot solution, and the intensity of the fluorescence peak at 456nm gradually decreased as the oxytetracycline concentration increased from (0-100 μ M).
Example 9
The potassium-nitrogen co-doped carbon dots based on the pericarp of turkey prepared in example 1 were used for detecting aureomycin hydrochloride, and as shown in fig. 5, a aureomycin hydrochloride solution was gradually added dropwise to the potassium-nitrogen co-doped carbon dot solution, and the intensity of the fluorescence peak at 456nm gradually increased as the concentration of aureomycin hydrochloride increased from (0-200 μ M).
Example 10
The potassium-nitrogen co-doped carbon dots based on the turkey pericarp prepared in example 1 is used for detecting tetracycline, europium nitrate/europium fluoride/europium chloride hexahydrate/europium nitrate hexahydrate aqueous solution and sodium citrate solution are added into the potassium-nitrogen co-doped carbon dot solution and mixed uniformly, the tetracycline solution is gradually added dropwise, the fluorescence peak intensity at 456nm gradually decreases and the fluorescence intensity at 618nm gradually increases with the increase of the tetracycline concentration (0-128 mu M).
Example 11
The potassium-nitrogen co-doped carbon dot aqueous solution prepared in example 1 is used for detecting contents of aureomycin hydrochloride, tetracycline and oxytetracycline in milk, honey, fish and pork, fluorescence intensity of only potassium-nitrogen co-doped carbon dots (a potassium-nitrogen co-doped carbon dot, europium nitrate and sodium citrate mixed solution) and fluorescence intensity of actual samples of milk, honey, fish and pork are respectively measured by a labeling recovery method, a certain amount of aureomycin hydrochloride, tetracycline and oxytetracycline standard solution is continuously added, fluorescence intensity of the standard solutions is measured, and original content and labeling recovery rate are calculated based on corresponding working curves.
Claims (7)
1. A potassium-nitrogen co-doped carbon dot based on flint pericarp and a preparation method thereof are characterized by comprising the following steps:
1) putting the steamship peel in a beaker, adding ultrapure water, adding ethylenediamine into the solution, and performing ultrasonic treatment to obtain a mixed solution; wherein the mass ratio of the flint peel, the ethylenediamine and the ultrapure water is 0.2-1:2.88-14.4: 16;
2) placing the mixed solution in a high-pressure reaction kettle, carrying out hydrothermal reaction for 2-4h at the temperature of 140-160 ℃, then naturally cooling the reaction kettle to room temperature, and filtering with filter paper to remove large particles in the reacted solution; then, further filtering the dark brown filtrate by a cylindrical filter membrane filter to obtain a potassium-nitrogen co-doped carbon dot aqueous solution;
3) and (3) storing the potassium-nitrogen co-doped carbon dot aqueous solution in a refrigerator at 4 ℃ for later use.
2. The preparation method of the potassium-nitrogen co-doped carbon dots based on the turkey pericarp as claimed in claim 1, wherein the mass ratio of the turkey pericarp, the ethylenediamine and the ultrapure water in the step 1) is 1:14.4: 16.
3. The preparation method of potassium-nitrogen co-doped carbon dots based on turkey pericarp as claimed in claim 1, wherein the hydrothermal reaction temperature in step 2) is 150 ℃ and the time is 3 h.
4. The potassium-nitrogen co-doped carbon dots prepared by the method of claim 1, 2 or 3.
5. The potassium-nitrogen co-doped carbon dot as claimed in claim 4 is used for identifying and detecting chlortetracycline hydrochloride, tetracycline and oxytetracycline.
6. The potassium-nitrogen co-doped carbon dot according to claim 5, which is used for identifying and detecting aureomycin hydrochloride, tetracycline and oxytetracycline, wherein the identification and detection of aureomycin hydrochloride and oxytetracycline are realized by respectively and gradually dripping aureomycin hydrochloride and oxytetracycline into a potassium-nitrogen co-doped carbon dot solution, and the fluorescence intensity of the potassium-nitrogen co-doped carbon dot is respectively enhanced and reduced, and the identification and detection of tetracycline is realized by adding europium nitrate or europium fluoride or europium chloride hexahydrate or a mixed solution of europium nitrate hexahydrate and sodium citrate into the potassium-nitrogen co-doped carbon dot solution, and then adding tetracycline and changing the fluorescence ratio.
7. The potassium-nitrogen co-doped carbon dot of claim 4 is used for detecting the contents of aureomycin hydrochloride, tetracycline and oxytetracycline in milk, honey, fish and pork.
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