AU2020103861A4 - Preparation of chicken feather nitrogen-doped carbon quantum dots based fluorescent probes and paraquat detection method - Google Patents
Preparation of chicken feather nitrogen-doped carbon quantum dots based fluorescent probes and paraquat detection method Download PDFInfo
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Abstract
Provided are preparation of chicken feather nitrogen-doped carbon quantum dots
based fluorescent probes and a paraquat detection method. The method for preparing
chicken feather nitrogen-doped carbon quantum dots comprises: mixing chicken
feather material and deionized water uniformly in a mass-to-volume ratio of 0.2g
1.5g: 60mL, and then adding to the solution 0.2mL-3mL of a nitrogen-containing
solution as a dopant, and ultrasonically dispersing the solution for 2min-10min, thus
obtaining a solution to be reacted; placing the solution to be reacted in an airtight
reaction kettle and reacting at a temperature between 100°C and 300°C for 1.5h to
48h to obtain a hydrothermal reaction product solution, naturally cooling the
hydrothermal reaction product solution, and taking the solution out; and centrifuging
the hydrothermal reaction product solution, taking the supernatant of the centrifuged
brown liquid, and filtering the supernatant, thus obtaining a chicken feather nitrogen
doped carbon quantum dot solution. A corresponding fluorescent probe is obtained
through the chicken feather nitrogen-doped carbon quantum dot solution; through the
exploration on the excitation wavelength and emission wavelength, the linear
regression equation is fitted with a standard solution, and the equation is used to
complete the detection. With environmentally friendly waste biomass material as raw
material, the biomass atom-doped fluorescent carbon quantum dots are prepared by a
one-step hydrothermal method, and the provided "on-off N-CQDs/Hg fluorescent
probe solution can be used for detecting the content of paraquat.
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Description
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Technical Field
The present invention relates to a pesticide residue detection technology, and in particular to a method for preparing a chicken feather nitrogen-doped carbon quantum dot solution and a method for preparing a fluorescent probe solution and a method for detecting paraquat.
Background
As a non-selective, quick-acting herbicide, paraquat has been widely used in more than 130 countries. Due to its high toxicity, paraquat is easily absorbed by the digestive tract, respiratory tract and skin, causing organ injury and even death and posing a serious risk to human health and the environment.
At present, many methods of PQ detection have been reported, such as spectrophotometry, liquid chromatography, thin layer chromatography and mass spectrometry, but they have not been better and more widely used due to their limitations such as time-consuming operation, high cost of instrument materials, and difficult pre-processing.
Since carbon quantum dots have unique photoluminescence properties, good biocompatibility, high stability, easy synthesis and functionalization, adjustable excitation/emission wavelengths and can effectively overcome the defect of high toxicity of traditional semiconductor quantum dots, they can be considered as ideal materials, and the fluorescent probe detection method by synthetic carbon dots has attracted the attention of more researchers. However, the existing preparation methods of carbon quantum dots and the detection methods used for paraquat are not ideal. On the one hand, there are problems such as environment unfriendliness and potential safety hazards. On the other hand, they are not conducive to sustainable and convenient large-scale industrial production, and thus it is necessary to improve them.
Summary of the Invention
In order to solve the defects of the prior art, the present invention provides a method for preparing chicken feather nitrogen-doped carbon quantum dots, a method for preparing fluorescent probes, and a method for detecting paraquat. With environmentally friendly waste biomass material as raw material, the biomass atom doped fluorescent carbon quantum dots are prepared by a simple one-step hydrothermal method, and the provided "on-off' N-CQDs/Hg2+ fluorescent probe solution can be used for detecting the content of paraquat in actual samples.
In order to achieve the object of the present invention, the following solution is provided:
A method for preparing chicken feather nitrogen-doped carbon quantum dots, including:
mixing chicken feather material and deionized water uniformly in a mass-to volume ratio of 0.2g-1.5g: 60mL, and then adding to the solution 0.2mL-3mL of a nitrogen-containing solution as a dopant, and ultrasonically dispersing the solution for 2min-Omin, thus obtaining a uniformly dispersed solution to be reacted;
placing the solution to be reacted in an airtight reaction kettle and reacting at a temperature between 100°C and 300°C for 1.5h to 48h to obtain a hydrothermal reaction product solution, naturally cooling the hydrothermal reaction product solution, and taking the solution out; and
centrifuging the hydrothermal reaction product solution, taking the supernatant of the centrifuged brown liquid, and filtering the supernatant with a microporous water-based filter membrane to remove large-particle impurities, thus obtaining a chicken feather nitrogen-doped carbon quantum dot solution. The preferred microporous water-based filter membrane is a 0.22tm microporous water-based filter membrane.
Further, the chicken feather material is destemmed fluff of chicken feathers.
Further, the dopant is one or more of ammonia water, ethylenediamine, aspartic acid, lysine, and glycine.
Further, the centrifugation is carried out at a rotating speed between 5000rpm and 10000rpm for 10min-30min.
The present invention further provides a method for preparing a chicken feather nitrogen-doped carbon quantum dot fluorescent probe, including:
taking the same volume of chicken feather nitrogen-doped carbon quantum dot solution and respectively adjusting with a sodium hydroxide-hydrochloric acid buffer solution with pH of 5.5-11; and
respectively adding mercury ion standard solutions with different concentrations to form a series of fluorescent carbon quantum dot-mercury ion mixed solutions with different concentrations, thus obtaining "on-off' N-CQDs/Hg2+ fluorescent probe solutions, i.e., the chicken feather nitrogen-doped carbon quantum dot fluorescent probes, wherein the mercury ion concentration here is between 30 mol/L and 150[imol/L.
The present invention further provides an application of the chicken feather nitrogen-doped carbon quantum dot solution in the detection of paraquat, and particularly a paraquat detection method based on the chicken feather nitrogen-doped carbon quantum dot solution, including:
taking the same volume of chicken feather nitrogen-doped carbon quantum dot solutions and respectively adjusting with a sodium hydroxide-hydrochloric acid buffer solution with pH of 5.5-11;
respectively adding mercury ion standard solutions with different concentrations to form a series of fluorescent carbon quantum dot-mercury ion mixed solutions with different concentrations, thus obtaining an "on-off' N-CQDs/Hg2+ fluorescent probe solution;
adding different concentrations of paraquat standard solutions to the "on-off' N CQDs/Hg fluorescent probe solution respectively;
respectively measuring the intensity of fluorescence emitted within a range from 380nm to 410nm under each fluorescence excitation at an excitation wavelength between 31Onm and 330nm to obtain the fluorescence intensity of a series of different concentrations of paraquat-N-CQDs/Hg2+ fluorescent probe solutions, making a plot and performing linear fitting to obtain a linear regression equation; and detecting the content of paraquat in river water or tap water by the linear regression equation.
Furthermore, the mercury ion concentration here is between 30tmol/L and 150jmol/L.
Furthermore, the concentration of the paraquat standard solution is between 0.01 pg/mL and 20 g/mL.
Preferably, the fluorescence spectrum is scanned at an excitation wavelength of 320nm, the fluorescence intensity of a series of paraquat-N-CQDs/Hg2+ fluorescent probe solutions with different concentrations is measured respectively at an emission wavelength of 386nm, a plot is then made, and linear fitting is carried out to obtain a linear regression equation, wherein the degree of fitting of the linear fitting is greater than 0.99; the linear regression equation is y=92.41x+123.31, where x is the concentration of paraquat in [g/mL; y is F-F0, where FO represents the fluorescence intensity of an N-CQD detection system at 386 nm in the absence of paraquat, and F represents the fluorescence intensity of the N-CQD detection system at 386 nm in the presence of paraquat; the linear range of the linear regression equation is between 0 and 1 g/mL.
Furthermore, the detection limit of paraquat concentration is 16 g/L.
The present invention has the following beneficial effects:
1. The present invention uses waste biomass materials as raw materials, and prepares a carbon quantum dot solution through a one-step hydrothermal method, which realizes the recycling and reuse of waste biomass chicken feathers. The present invention is environmentally friendly and sustainable, low-cost, uses widely available materials, and can be put into industrial production easily; moreover, the present invention is environmentally friendly and easy to operate and prepares biomass-based carbon quantum dots with good fluorescence performance, strong anti-bleaching ability and good stability.
2. The biomass-based carbon quantum dots prepared by the present invention do not contain heavy metal elements such as cadmium and lead and are safe to use and non-toxic.
3. As a paraquat fluorescent probe, the carbon quantum dots prepared by the present invention have extremely high sensitivity, selectivity and anti-interference, can accurately detect the content of paraquat in a solution, and have a correlation coefficient of 0.99 relative to the concentration; in the detection of paraquat, the detection limit can be as low as 16 g/L.
4. At present, the global livestock product processing industry generates more than 8.6 million tons of keratin-containing livestock and poultry processing waste each year. The promotion of the present invention realizes the recycling and reuse of waste biomass chicken feathers and will play a positive role in promoting in-depth research on the efficient use of keratin waste and sustainable technology, especially on the use of atom-doped carbon quantum dots and fluorescent probes synthesized from waste biomass materials and their application in the detection of paraquat, thus providing more scientific basis for rapid pesticide detection.
Brief Description of the Drawings
The drawings described herein are only to illustrate selected embodiments, rather than all possible implementations, and are not intended to limit the scope of the present invention.
Fig. 1 shows a transmission electron microscopy image and a particle size distribution diagram of the carbon quantum dots prepared in Example 1 of the present invention.
Fig. 2 shows the emission spectrum of the carbon quantum dots prepared in Example 1 of the present invention under different excitation wavelengths.
Fig. 3 shows the quenching spectrum of different paraquat concentrations over the fluorescence intensity in Application Example 1 of the present invention.
Fig. 4 shows the linear relationship between different paraquat concentrations and F-FO in Application Example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clear, the present invention will be described in further detail below with reference to the accompanying drawings. The following embodiments are merely exemplary and are not intended to limit the present invention. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the scope of the present invention.
Specific embodiments of the present invention will now be described below. It should be noted that embodiments in the present invention and the features in the embodiments may be combined with each other without conflict.
Example 1
A method for preparing chicken feather nitrogen-doped carbon quantum dots, including:
(1) mixing destemmed fluff of chicken feathers and deionized water uniformly in a mass-to-volume ratio of 0.2g: 60mL, and then adding to the solution 0.2mL of ammonia water as a dopant, and ultrasonically dispersing the solution for 2min, thus obtaining a uniformly dispersed solution to be reacted;
(2) placing the solution to be reacted, obtained in step (1), in an airtight reaction kettle and reacting at 100°C for 48h to obtain a hydrothermal reaction product solution, naturally cooling the hydrothermal reaction product solution, and taking the solution out; and
(3) centrifuging the hydrothermal reaction product solution, obtained in step (2), at a rotating speed of 10000 rpm for 10min, taking the supernatant of the centrifuged brown liquid, and filtering the supernatant with a 0.22 m microporous water-based filter membrane to remove large-particle impurities, thus obtaining a fluorescent carbon quantum dot solution, i.e., a chicken feather nitrogen-doped carbon quantum dot solution.
Example 2
A method for preparing chicken feather nitrogen-doped carbon quantum dots, including:
(1) mixing destemmed fluff of chicken feathers and deionized water uniformly in a mass-to-volume ratio of 1.0g: 60mL, and then adding to the solution 1.5mL of ethylenediamine solution as a dopant, and ultrasonically dispersing the solution for min, thus obtaining a uniformly dispersed solution to be reacted;
(2) placing the solution to be reacted, obtained in step (1), in an airtight reaction kettle and reacting at 150°C for 24h to obtain a hydrothermal reaction product
solution, naturally cooling the hydrothermal reaction product solution, and taking the solution out; and
(3) centrifuging the hydrothermal reaction product solution, obtained in step (2), at a rotating speed of 8000 rpm for 20 min, taking the supernatant of the centrifuged brown liquid, and filtering the supernatant with a 0.22 m microporous water-based filter membrane to remove large-particle impurities, thus obtaining a fluorescent carbon quantum dot solution, i.e., a chicken feather nitrogen-doped carbon quantum dot solution.
Example 3
A method for preparing chicken feather nitrogen-doped carbon quantum dots, including:
(1) mixing destemmed fluff of chicken feathers and deionized water uniformly in a mass-to-volume ratio of 1.5g: 60mL, and then adding to the solution 3mL of lysine solution as a dopant, and ultrasonically dispersing the solution for 10min, thus obtaining a uniformly dispersed solution to be reacted;
(2) placing the solution to be reacted, obtained in step (1), in an airtight reaction kettle and reacting at 300°C for 1.5h to obtain a hydrothermal reaction product
solution, naturally cooling the hydrothermal reaction product solution, and taking the solution out; and
(3) centrifuging the hydrothermal reaction product solution, obtained in step (2), at a rotating speed of 5000 rpm for 30 min, taking the supernatant of the centrifuged brown liquid, and filtering the supernatant with a 0.22 m microporous water-based filter membrane to remove large-particle impurities, thus obtaining a fluorescent carbon quantum dot solution, i.e., a chicken feather nitrogen-doped carbon quantum dot solution.
Related tests/detections were performed on the results of Examples 1 to 3, and the related test/detection results of Example 1 are shown in Figs. 1 and 2.
The position of the maximum emission wavelength under the maximum excitation wavelength is marked in Fig. 2, and the red shift phenomenon of the carbon dot emission can be illustrated in the upper right corner of Fig. 2.
Carbon dots have fluorescence tunability and red shift effect; therefore, when used in detection methods, they need to be searched in a wide range from violet to red, that is, it is required to explore the maximum excitation wavelength and maximum emission wavelength of the corresponding carbon dots in the range of excitation wavelength from 200nm to 500nm and emission wavelength from 260nm to 700nm. The measurement wavelength spacing is measured by the instrument, the exploration time for the maximum excitation wavelength can be set to 10nm, and the emission wavelength slit is set to 2nm.
Application Example 1
Provided is the application of the above-mentioned chicken feather nitrogen doped carbon quantum dot solution in detecting the content of paraquat in the presence of mercury ions. The method applied to paraquat detection includes the following steps:
1. First, preparing chicken feather nitrogen-doped carbon quantum dot fluorescent probes:
(1) taking the same volume of fluorescent carbon quantum dot solutions prepared in Examples 1 to 3 and adjusting with a sodium hydroxide-hydrochloric acid buffer solution with pH 8; for example, the amount of the buffer solution added per 500 L of quantum dot system may be 200 L; and
(2) respectively adding a 30umol/L mercury ion standard solution to form fluorescent carbon quantum dot-mercury ion mixed solutions, thus obtaining "on-off' N-CQDs/Hg fluorescent probe solutions, i.e., the chicken feather nitrogen-doped carbon quantum dot fluorescent probes.
2. Adding paraquat standard solutions with concentrations of 0.05, 0.1., 0.2, 0.4, 0.6, 0.8, 1, 1.8, 2, 2.5, 5, 10, and 20 g/mL to the "on-off"'N-CQDs/Hg2+ fluorescent probe solutions, respectively.
3. Scanning the fluorescence spectrum with the excitation wavelength of 320nm, measuring the fluorescence intensity of a series of paraquat-N-CQDs/Hg2+ fluorescent probe solutions with different concentrations at the emission wavelength of 386nm, making a plot and respectively performing linear fitting to obtain a linear regression equation.
4. Detecting the content of paraquat in river water or tap water. It is used to test the practical applicability of the N-CQDs system method in PQ. Samples are collected, the pH of the water samples is adjusted to neutral with a sulfuric acid solution, the sample solutions are filtered with a 0.22 pm microporous filter membrane, and then placed in volumetric flasks at 4C for later use. The contents of
paraquat in the samples are calculated according to a linear regression equation. The linear range of the linear regression equation is from 0 to 1 g/mL.
The quenching spectrum of different paraquat concentrations over the fluorescence intensity in Application Example 1 is shown in Fig. 3.
The linear relationship between different paraquat concentrations and F-FO in Application Example 1 is shown in Fig. 4.
Application Example 2
Provided is the application of the above-mentioned chicken feather nitrogen doped carbon quantum dot solution in detecting the content of paraquat in the presence of mercury ions. The method applied to paraquat detection includes the following steps:
1. First, preparing chicken feather nitrogen-doped carbon quantum dot fluorescent probes:
(1) taking the same volume of fluorescent carbon quantum dot solutions prepared in Examples 1 to 3 and adjusting with a sodium hydroxide-hydrochloric acid buffer solution with pH 10; for example, the amount of the buffer solution added per 500L of quantum dot system may be 200L; and
(2) respectively adding a 150tmol/L mercury ion standard solution to form fluorescent carbon quantum dot-mercury ion mixed solutions, thus obtaining "on-off' N-CQDs/Hg fluorescent probe solutions, i.e., the chicken feather nitrogen-doped carbon quantum dot fluorescent probes.
2. Adding paraquat standard solutions with concentrations of 0.05, 0.1., 0.2, 0.4, 0.6, 0.8, 1, 1.8, 2, 2.5, 5, 10, and 20[g/mL to the "on-offN-CQDs/Hg2+ fluorescent probe solutions, respectively.
3. Scanning the fluorescence spectrum with the excitation wavelength of 31Onm, measuring the fluorescence intensity of a series of paraquat-N-CQDs/Hg2+ fluorescent probe solutions with different concentrations at the emission wavelength of 380nm, making a plot, and performing linear fitting to obtain a linear regression equation.
4. Detecting the content of paraquat in river water or tap water. it is used to test the practical applicability of the N-CQDs system method in PQ. Samples are collected, the pH of the water samples is adjusted to neutral with a sulfuric acid solution, the sample solutions are filtered with a 0.22 pm microporous filter membrane, and then placed in volumetric flasks at 4C for later use. The contents of
paraquat in the samples are calculated according to a linear regression equation. The linear range of the linear regression equation is from 0 to1 g/mL.
Application Example 3
Provided is the application of the above-mentioned chicken feather nitrogen doped carbon quantum dot solution in detecting the content of paraquat in the presence of mercury ions. The method applied to paraquat detection includes the following steps:
1. First, preparing chicken feather nitrogen-doped carbon quantum dot fluorescent probes:
(1) taking the same volume of fluorescent carbon quantum dot solutions prepared in Examples 1 to 3 and adjusting with a sodium hydroxide-hydrochloric acid buffer solution with pH 10; for example, the amount of the buffer solution added per 500L of quantum dot system may be 200L; and
(2) respectively adding a 150tmol/L mercury ion standard solution to form fluorescent carbon quantum dot-mercury ion mixed solutions, thus obtaining "on-off' N-CQDs/Hg fluorescent probe solutions, i.e., the chicken feather nitrogen-doped carbon quantum dot fluorescent probes.
2. Adding paraquat standard solutions with concentrations of 0.05, 0.1., 0.2, 0.4, 0.6, 0.8, 1, 1.8, 2, 2.5, 5, 10, and 20[g/mL to the "on-off"N-CQDs/Hg2+ fluorescent probe solutions, respectively.
3. Scanning the fluorescence spectrum with the excitation wavelength of 330nm, measuring the fluorescence intensity of a series of paraquat-N-CQDs/Hg2+ fluorescent probe solutions with different concentrations at the emission wavelength of 380nm, making a plot, and performing linear fitting to obtain a linear regression equation.
4. Detecting the content of paraquat in river water or tap water. It is used to test the practical applicability of the N-CQDs system method in PQ. Samples are collected, the pH of the water samples is adjusted to neutral with a sulfuric acid solution, the sample solutions are filtered with a 0.22 pm microporous filter membrane, and then placed in volumetric flasks at 5C for later use. The contents of
paraquat in the samples are calculated according to a linear regression equation. The linear range of the linear regression equation is from 0 to1 g/mL.
In the present invention, through the investigation on the preparation method and doping conditions of the chicken feather nitrogen-doped carbon quantum dots, in the presence of mercury ions, the fluorescence of the nitrogen-doped carbon quantum dot solution is quenched (off), and after addition of paraquat, the quenched fluorescence is restored (on), and then the fluorescence intensity of the mixed solution is measured with a microplate reader to obtain the concentration information in the samples of the paraquat solution to be tested, thereby realizing the fluorescence detection of the actual samples. It not only makes full use of waste biological materials, but also obtains a probe that can accurately detect the content of paraquat in the solution, and in combination with a specific detection method, the correlation coefficient for the concentration reaches 0.99; in the paraquat detection, the detection limit can be as low as 16[g/L.
The fluorescent carbon quantum dots prepared by the present invention have excellent fluorescence performance, preferably have an excitation wavelength of 320 nm during the fluorescence test process, and have a selective recognition ability for paraquat.
The above embodiments are only preferred embodiments of the present invention, and are not meant to be the only embodiments or limiting the present invention. Those skilled in the art should understand that various changes or equivalent substitutions made to the present invention without departing from the scope of the present invention fall within the protection scope of the present invention.
Claims (5)
1. A method for preparing chicken feather nitrogen-doped carbon quantum dots, comprising:
mixing chicken feather material and deionized water uniformly in a mass-to volume ratio of 0.2g-1.5g: 60mL, and then adding to the solution 0.2mL-3mL of a nitrogen-containing solution as a dopant, and ultrasonically dispersing the solution for 2min-l0min, thus obtaining a uniformly dispersed solution to be reacted;
placing the solution to be reacted in an airtight reaction kettle and reacting at a temperature between 100°C and 300°C for 1.5h to 48h to obtain a hydrothermal reaction product solution, naturally cooling the hydrothermal reaction product solution, and taking the solution out; and
centrifuging the hydrothermal reaction product solution, taking the supernatant of the centrifuged brown liquid, and filtering the supernatant, thus obtaining a chicken feather nitrogen-doped carbon quantum dot solution;
wherein the dopant is one or more of ammonia water, ethylenediamine, aspartic acid, lysine, and glycine;
wherein the centrifugation is carried out at a rotating speed between 5000rpm and 10000rpm for 10min-30min;
wherein the chicken feather material is destemmed fluff of chicken feathers.
2. A method for preparing chicken feather nitrogen-doped carbon quantum dot fluorescent probes, comprising:
taking the same volume of chicken feather nitrogen-doped carbon quantum dot solutions obtained by the method for preparing chicken feather nitrogen-doped carbon quantum dots according to claims 1-4, and respectively adjusting with a sodium hydroxide-hydrochloric acid buffer solution with pH of 5.5-11; and
respectively adding mercury ion standard solutions with different concentrations to form a series of fluorescent carbon quantum dot-mercury ion mixed solutions with different concentrations, thus obtaining "on-off'N-CQDs/Hg2+ fluorescent probe solutions, i.e., the chicken feather nitrogen-doped carbon quantum dot fluorescent probes; wherein the mercury ion concentration is between 30tmol/L and 150tmol/L.
3. A paraquat detection method, comprising:
respectively adding mercury ion standard solutions with different concentrations to form a series of fluorescent carbon quantum dot-mercury ion mixed solutions with different concentrations, thus obtaining "on-off'N-CQDs/Hg2+ fluorescent probe solutions;
adding different concentrations of paraquat standard solutions to the "on-off'N CQDs/Hg fluorescent probe solutions respectively;
respectively measuring the intensity of fluorescence emitted within a range from 380nm to 410nm under each fluorescence excitation at an excitation wavelength between 31Onm and 330nm to obtain the fluorescence intensity of a series of different concentrations of paraquat-N-CQDs/Hg2+ fluorescent probe solutions, making a plot and performing linear fitting to obtain a linear regression equation; and
detecting the content of paraquat in river water or tap water by the linear regression equation;
wherein the mercury ion concentration is between 30tmol/L and 150tmol/L.
4. The paraquat detection method according to claim 3, wherein the concentration of the paraquat standard solution is between 0.01 g/mL and 20 [g/mL.
5. The paraquat detection method according to claim 3,wherein,
the fluorescence spectrum is scanned at an excitation wavelength of 320nm, the fluorescence intensity of a series of paraquat-N-CQDs/Hg2+ fluorescent probe solutions with different concentrations is measured respectively at an emission wavelength of 386nm, a plot is then made, and linear fitting is carried out to obtain a linear regression equation;
the degree of fitting of the linear fitting is greater than 0.99; the linear regression equation is y=92.41x+123.31, where x is the concentration of paraquat in [g/mL; y is F-FO, where FO represents the fluorescence intensity of an N-CQD detection system at 386 nm in the absence of paraquat, and F represents the fluorescence intensity of the N-CQD detection system at 386 nm in the presence of paraquat; the linear range of the linear regression equation is between 0 and1 g/mL.
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| CN202010423652.1A CN111573652B (en) | 2020-05-19 | 2020-05-19 | Preparation of chicken feather nitrogen-doped carbon quantum dot and fluorescent probe and paraquat detection method |
| CNCN202010423652.1 | 2020-05-19 |
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| CN113462377A (en) * | 2021-06-23 | 2021-10-01 | 青岛农业大学 | Preparation method of silicon dioxide coated carbon quantum dot composite material and application of silicon dioxide coated carbon quantum dot composite material in detection of different veterinary drug residues |
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| CN111573652B (en) | 2021-10-22 |
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