CN116640571A - Fluorescent carbon dot, preparation method thereof and application thereof in detection of Dimethoate - Google Patents
Fluorescent carbon dot, preparation method thereof and application thereof in detection of Dimethoate Download PDFInfo
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- CN116640571A CN116640571A CN202310630288.XA CN202310630288A CN116640571A CN 116640571 A CN116640571 A CN 116640571A CN 202310630288 A CN202310630288 A CN 202310630288A CN 116640571 A CN116640571 A CN 116640571A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 50
- 239000005947 Dimethoate Substances 0.000 title claims abstract description 49
- MCWXGJITAZMZEV-UHFFFAOYSA-N dimethoate Chemical compound CNC(=O)CSP(=S)(OC)OC MCWXGJITAZMZEV-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000001514 detection method Methods 0.000 title abstract description 18
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 14
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000004108 freeze drying Methods 0.000 claims abstract description 7
- 238000005360 mashing Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 49
- 238000000034 method Methods 0.000 claims description 17
- 238000000502 dialysis Methods 0.000 claims description 14
- 244000118350 Andrographis paniculata Species 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000002994 raw material Substances 0.000 abstract description 6
- 241000746375 Andrographis Species 0.000 abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 230000008859 change Effects 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 5
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 2
- 238000000695 excitation spectrum Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 241000238631 Hexapoda Species 0.000 description 1
- 230000000895 acaricidal effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000000749 insecticidal effect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- 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"
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- 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"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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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"
- G01N2021/6432—Quenching
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Abstract
The application relates to a fluorescent carbon dot, a preparation method thereof and application thereof in detecting dimethoate. The preparation method of the fluorescent carbon dots comprises the following steps: s1: mashing herba Andrographitis rhizome, adding ethylenediamine and water, and stirring; s2: transferring the mixture obtained in the step S1 into a reaction kettle, and reacting for 8-12h at 160-200 ℃; s3: and naturally cooling after the reaction is finished, centrifuging, filtering, dialyzing and freeze-drying the reaction product to obtain the fluorescent carbon dots. The application takes the rhizome of common andrographis herb as the raw material, obtains the fluorescent carbon dots by a hydrothermal method, has the advantages of easily obtained raw material, simple reaction, excellent luminous performance of the obtained fluorescent carbon dots, wide detection linear range and low detection limit, and can be used for detecting Dimethoate.
Description
Technical Field
The application relates to detection of fluorescent carbon dots and Dimethoate, in particular to a fluorescent carbon dot and a preparation method thereof, and the fluorescent carbon dot is used for detecting Dimethoate.
Background
Dimethoate is a moderate toxic systemic organophosphorus insecticidal and acaricidal agent, is widely used for insect prevention of crops, and makes great contribution to agricultural development. However, the use of a large or irregular number of Dimethoate causes serious damage to the ecosystem and also presents a significant risk to human health. Therefore, it is of great importance to provide a method capable of detecting the fruits.
Fluorescent Carbon Dots (CDs) have the advantages of good water solubility, low toxicity and simple preparation method, and have been widely applied to analysis and detection of various substances, but the application of the fluorescent Carbon Dots (CDs) in Dimethoate detection has not been reported yet.
Disclosure of Invention
The application aims to provide a fluorescent carbon dot and a preparation method thereof, and the fluorescent carbon dot is applied to detecting dimethoate.
In a first aspect of the present application, a method for preparing fluorescent carbon dots is provided, comprising the steps of:
s1: mashing herba Andrographitis rhizome, adding ethylenediamine and water, and stirring;
s2: transferring the mixture obtained in the step S1 into a reaction kettle, and reacting for 8-12h at 160-200 ℃;
s3: and naturally cooling after the reaction is finished, centrifuging, filtering, dialyzing and freeze-drying the reaction product to obtain the fluorescent carbon dots.
In one embodiment, in the step S1, the amount of ethylenediamine is 5-10g and the amount of water is 100-150mL calculated by 10-20g of the rhizome of andrographis paniculata.
In one embodiment, in the step S2, the reaction temperature is 175-185 ℃ and the reaction time is 9-11h.
In one embodiment, in the step S3, the centrifugation is performed at 8000-12000r/m for 5-15 min.
In one embodiment, in the step S3, the filtering method is filtering with a 0.2-0.3 μm filter membrane.
In one embodiment, in the step S3, the dialysis is performed by dialysis treatment with a dialysis bag of 500-1000Da for 48-60 hours.
In a second aspect of the application, a fluorescent carbon dot is provided, and the fluorescent carbon dot is prepared by the preparation method in the first aspect.
In a third aspect of the application, there is provided the use of the fluorescent carbon dots of the second aspect for detecting Dimethoate.
In a fourth aspect of the present application, there is provided a method of detecting a dimethoate, comprising the steps of:
preparing the fluorescent carbon dots according to the second aspect into a fluorescent carbon dot solution;
adding Dimethoate solutions with different concentrations into the fluorescent carbon dot solution, measuring the fluorescence intensity before and after the reaction of the obtained mixed solution, and establishing a Dimethoate standard curve according to the relation between the concentration of the fluorescent carbon dot solution and the relative fluorescence intensity variation value;
and adding a sample to be detected into the fluorescent carbon dot solution, measuring the fluorescent intensity of the obtained mixed solution before and after the reaction, substituting the fluorescent intensity into the standard curve of the Dimethoate, and calculating the content of the Dimethoate in the sample to be detected.
In one embodiment, the fluorescent carbon dot solution has a concentration of 0.2-0.6mg/mL.
The application takes the rhizome of common andrographis herb as the raw material, obtains the fluorescent carbon dots by a hydrothermal method, has the advantages of easily obtained raw material, simple reaction, excellent luminous performance of the obtained fluorescent carbon dots, wide detection linear range and low detection limit, and can be used for detecting Dimethoate.
Drawings
FIG. 1 is a TEM test chart of fluorescent carbon dots prepared in example 1;
FIG. 2 is a graph showing fluorescence excitation and emission spectra of fluorescent carbon dots prepared in example 1;
FIG. 3 is a graph showing fluorescence emission spectra of fluorescent carbon dots at various concentrations of Dimethoate;
FIG. 4 is a graph showing the linear response of fluorescent carbon dots prepared in example 1 to Dimethoate;
FIG. 5 is a graph showing the fluorescence change of the fluorescent carbon dots prepared in example 1 for different types of pesticides.
Detailed Description
The following describes a fluorescent carbon dot, a preparation method thereof and application thereof in detecting Dimethoate in detail by referring to specific examples. The present application may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.
In the present application, "first aspect", "second aspect", "third aspect", "fourth aspect", etc. are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or quantity, nor as implying an importance or quantity of technical features indicated. Moreover, the terms "first," "second," "third," "fourth," and the like are used for non-exhaustive list description purposes only, and are not to be construed as limiting the number of closed forms.
In the application, the technical characteristics described in an open mode comprise a closed technical scheme composed of the listed characteristics and also comprise an open technical scheme comprising the listed characteristics.
In the present application, the numerical ranges are referred to as continuous, and include the minimum and maximum values of the ranges, and each value between the minimum and maximum values, unless otherwise specified. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range description features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to include any and all subranges subsumed therein.
The percentage content referred to in the present application refers to mass percentage for both solid-liquid mixing and solid-solid mixing and volume percentage for liquid-liquid mixing unless otherwise specified.
The percentage concentrations referred to in the present application refer to the final concentrations unless otherwise specified. The final concentration refers to the ratio of the additive component in the system after the component is added.
The temperature parameter in the present application is not particularly limited, and may be a constant temperature treatment or a treatment within a predetermined temperature range. The constant temperature process allows the temperature to fluctuate within the accuracy of the instrument control.
Some examples of the application provide a method for preparing fluorescent carbon dots, comprising the following steps:
s1: mashing herba Andrographitis rhizome, adding ethylenediamine and water, and stirring;
s2: transferring the mixture obtained in the step S1 into a reaction kettle, and reacting for 8-12h at 160-200 ℃;
s3: and naturally cooling after the reaction is finished, centrifuging, filtering, dialyzing and freeze-drying the reaction product to obtain the fluorescent carbon dots.
According to the application, the common andrographis herb rhizome is used as a raw material, the fluorescent carbon dots are obtained through a hydrothermal method, the raw material is easy to obtain, the reaction is simple, the obtained fluorescent carbon dots have excellent luminous performance, stable properties and good water solubility and dispersibility, the reaction condition is mild, and the Dimethoate solution is added into the solution of the fluorescent carbon dots, so that the fluorescence of the fluorescent carbon dots is obviously quenched, and therefore, the common andrographis herb fluorescent carbon dot can be used for detecting Dimethoate, and the detection linear range is wider and the detection limit is lower. In one example, the linear range of detection is 0.2-15 μg/mL and the limit of detection is 0.091 μg/mL.
It will be appreciated that the reaction vessel may be, for example, a polytetrafluoroethylene reaction vessel, and that the reaction may be carried out, for example, in a forced air drying oven.
It will be appreciated that in step S1, the stirring should be sufficient to mix the materials uniformly for the subsequent reaction to proceed.
Further, in the step S1, the amount of ethylenediamine is 5-10g and the amount of water is 100-150mL calculated by 10-20g of the rhizome of Andrographis paniculata. Specifically, the amount of ethylenediamine includes, but is not limited to: 5g, 6g, 7g, 8g, 9g and 10g; the amount of water includes, but is not limited to: 100mL, 110mL, 120mL, 130mL, 140mL, 150mL. Without limitation, the water is deionized water.
Further, in the step S2, the reaction temperature is 175-185 ℃ and the reaction time is 9-11h. Specifically, the reaction temperature includes, but is not limited to: 175 ℃, 177 ℃, 178 ℃, 179 ℃, 180 ℃, 181 ℃, 182 ℃, 183 ℃, 185 ℃; reaction times include, but are not limited to: 9h, 9.5h, 10h, 10.5h, 11h. Further, the reaction temperature was 180℃and the reaction time was 10 hours.
Further, in the step S3, the centrifugation method is to centrifuge for 5-15 min at the rotation speed of 8000-12000 r/m. Specifically, rotational speeds include, but are not limited to: 8000r/m, 8500r/m, 9000r/m, 9500r/m, 10000r/m, 10500r/m, 11000r/m, 11500r/m, 12000r/m; centrifugation times include, but are not limited to: 5min, 8min, 10min, 12min, 15min. Further, the centrifugation is carried out at 10000r/m for 10min.
Further, the filtration method is to use a 0.2-0.3 μm filter membrane for filtration. Further, the filtration method is filtration with a 0.22 μm filter membrane.
Further, in the step S3, the dialysis method is that the dialysis treatment is carried out for 48-60 hours through a dialysis bag of 500-1000 Da. In particular, the specifications of the dialysis bag include, but are not limited to: 500Da, 600Da, 700Da, 800Da, 900Da, 1000Da; dialysis times include, but are not limited to: 48h, 55h and 60h.
In other examples of the present application, there is also provided a fluorescent carbon dot prepared by the preparation method described above.
In still other examples of the application, there is also provided the use of fluorescent carbon dots as above in detecting dimethoate.
In still other examples of the present application, there is also provided a method of detecting a dimethoate, comprising the steps of:
preparing the fluorescent carbon dots into fluorescent carbon dot solution;
adding Dimethoate solutions with different concentrations into the fluorescent carbon dot solution, measuring the fluorescence intensity before and after the reaction of the obtained mixed solution, and establishing a Dimethoate standard curve according to the relation between the concentration of the fluorescent carbon dot solution and the relative fluorescence intensity variation value;
and adding a sample to be detected into the fluorescent carbon dot solution, measuring the fluorescent intensity of the obtained mixed solution before and after the reaction, substituting the fluorescent intensity into the standard curve of the Dimethoate, and calculating the content of the Dimethoate in the sample to be detected.
Further, the concentration of the fluorescent carbon dot solution is 0.2-0.6mg/mL.
Without limitation, the method for detecting the Dimethoate comprises the following steps:
(1) Preparing 5mL of fluorescent carbon dot solution with the concentration of 0.4mg/mL, wherein the solvent is water;
(2) Adding 100 mu L of Dimethoate solution with different concentrations (the concentration is changed from 0 to 20 mu g/mL, and the solvent is water) into the fluorescent carbon dot solution, so that the fluorescence of the fluorescent carbon dot is gradually quenched;
(3) And measuring the fluorescence intensity before and after the reaction of the fluorescent carbon dot solution, and establishing a Dimethoate standard curve according to the relation between the concentration of the fluorescent carbon dot solution and the relative fluorescence intensity change value.
(4) Quantitative detection: adding a sample to be detected into the fluorescent carbon dot solution prepared in the step (1), recording the fluorescent intensity values of the fluorescent carbon dot solution before and after the reaction, and calculating the content of the Dimethoate by referring to the standard curve of the Dimethoate obtained in the step (3).
Example 1:
the embodiment is a preparation method of fluorescent carbon dots, comprising the following steps:
s1: mashing 15g of Andrographis paniculata rhizome (picked from Guangdong university of Industrial science), adding 5g of ethylenediamine, adding 120mL of deionized water as solvent, and stirring thoroughly;
s2: transferring the solution into a polytetrafluoroethylene reaction kettle, and reacting for 10 hours at 180 ℃ in a blast drying box;
s3: and (3) naturally cooling after the reaction is finished, centrifuging the reaction product at 10000r/m for 10min, filtering the solution by using a 0.22 mu m filter membrane, dialyzing the obtained filtrate by using a 500Da dialysis bag for 60h, and freeze-drying to obtain the fluorescent carbon dots.
The fluorescent carbon dots prepared in example 1 were redispersed in deionized water for testing. Fig. 1 is a TEM test chart of the fluorescent carbon dots, and it is seen that the fluorescent carbon dots have excellent dispersibility, are uniformly spherical, and have an average particle diameter of 2.50±0.5nm. FIG. 2 is a graph of fluorescence excitation and emission spectra of the fluorescent carbon dots, which shows that under excitation at 350nm, the fluorescent carbon dots emit blue light with peak at 475 nm.
Example 2:
the embodiment is a preparation method of fluorescent carbon dots, comprising the following steps:
s1: mashing 20g of Andrographis paniculata rhizome (picked from Guangdong university of Industrial science), adding 10g of ethylenediamine, adding 150mL of deionized water as solvent, and stirring thoroughly;
s2: transferring the solution into a polytetrafluoroethylene reaction kettle, and reacting for 12 hours at 200 ℃ in a blast drying box;
s3: and (3) naturally cooling after the reaction is finished, centrifuging the reaction product at 10000r/m for 10min, filtering the solution by using a 0.22 mu m filter membrane, dialyzing the obtained filtrate by using a 500Da dialysis bag for 60h, and freeze-drying to obtain the fluorescent carbon dots.
Example 3:
the embodiment is a preparation method of fluorescent carbon dots, comprising the following steps:
s1: mashing 10g of Andrographis paniculata rhizome (picked from Guangdong university of Industrial science), adding 5g of ethylenediamine, adding 120mL of deionized water as solvent, and stirring thoroughly;
s2: transferring the solution into a polytetrafluoroethylene reaction kettle, and reacting for 8 hours at 160 ℃ in a blast drying box;
s3: and (3) naturally cooling after the reaction is finished, centrifuging the reaction product at 10000r/m for 10min, filtering the solution by using a 0.22 mu m filter membrane, dialyzing the obtained filtrate by using a 500Da dialysis bag for 60h, and freeze-drying to obtain the fluorescent carbon dots.
Example 4:
the embodiment is the application of fluorescent carbon dots in detecting dimethoate, and the steps of detecting dimethoate are as follows:
(1) Redispersing the fluorescent carbon dots prepared in the example 1 in deionized water to prepare a fluorescent carbon dot solution with the concentration of 0.4 mg/mL;
(2) Respectively taking 5mL of fluorescent carbon dot solution, gradually dropwise adding 100 mu L of Dimethoate solution (0-20 mu g/mL) with different concentrations into the solution, and quenching the fluorescence of the fluorescent carbon dot to different degrees along with the addition of the Dimethoate solution;
(3) The fluorescence intensity of the fluorescent carbon dot solution before and after the reaction is measured, the relative fluorescence intensity change value is calculated, the fluorescence emission spectrum of the fluorescent carbon dot after the reaction of the Dimethoate solution with different concentrations is shown in figure 3, and the detection range and the detection limit of the Dimethoate by the fluorescent carbon dot are calculated according to the relation between the concentration of the Dimethoate solution and the relative fluorescence intensity change value. The linear detection range is 0.2-15 mug/mL, the detection limit is 0.091 mug/mL, and the linear regression equation after fitting is shown in FIG. 4, and can be expressed as follows:
Y=0.059X+0.056。
(4) And (3) taking a sample to be detected into the fluorescent carbon dot solution, recording the change of the fluorescent intensity of the fluorescent carbon dot solution before and after the reaction, and substituting the change into the linear regression equation for calculation to obtain the content of Dimethoate in the sample to be detected.
In addition, the fluorescent carbon dot solution is mixed with an equal amount of different pesticide samples (the concentration is 50 mug/mL), wherein blank is a blank control group, namely the fluorescent carbon dot solution is mixed with an equal amount of water, and the fluorescent intensity after the reaction of the fluorescent carbon dot solution is measured, and as shown in a result of fig. 5, the fluorescent carbon dot has a better specific recognition effect on Dimethoate.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples merely illustrate a few embodiments of the present application, which are convenient for a specific and detailed understanding of the technical solutions of the present application, but should not be construed as limiting the scope of the claims. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the application, which are all within the scope of the application. It should be understood that, based on the technical solutions provided by the present application, those skilled in the art may obtain technical solutions through logical analysis, reasoning or limited experiments, which are all within the scope of protection of the appended claims. The scope of the patent is therefore intended to be covered by the appended claims, and the description and drawings may be interpreted as illustrative of the contents of the claims.
Claims (10)
1. The preparation method of the fluorescent carbon dots is characterized by comprising the following steps:
s1: mashing herba Andrographitis rhizome, adding ethylenediamine and water, and stirring;
s2: transferring the mixture obtained in the step S1 into a reaction kettle, and reacting for 8-12h at 160-200 ℃;
s3: and naturally cooling after the reaction is finished, centrifuging, filtering, dialyzing and freeze-drying the reaction product to obtain the fluorescent carbon dots.
2. The method for preparing fluorescent carbon dots according to claim 1, wherein in the step S1, the amount of ethylenediamine is 5-10g and the amount of water is 100-150mL, based on 10-20g of the rhizome of andrographis paniculata.
3. The method for preparing fluorescent carbon dots according to claim 1, wherein in the step S2, the reaction temperature is 175-185 ℃ and the reaction time is 9-11h.
4. The method for preparing a fluorescent carbon dot according to any one of claims 1 to 3, wherein in the step S3, the centrifugation is performed at 8000-12000r/m for 5-15 min.
5. The method for preparing a fluorescent carbon dot according to any one of claims 1 to 3, wherein in the step S3, the filtration is performed by using a 0.2 to 0.3 μm filter.
6. The method for preparing a fluorescent carbon dot according to any one of claims 1 to 3, wherein in the step S3, the dialysis is performed by a dialysis treatment with a dialysis bag of 500-1000Da for 48-60 hours.
7. A fluorescent carbon dot prepared by the method of any one of claims 1-6.
8. Use of the fluorescent carbon dots of claim 7 for detecting dimethoate.
9. A method of detecting a dimethoate comprising the steps of:
preparing the fluorescent carbon dots of claim 7 into a fluorescent carbon dot solution;
adding Dimethoate solutions with different concentrations into the fluorescent carbon dot solution, measuring the fluorescence intensity before and after the reaction of the obtained mixed solution, and establishing a Dimethoate standard curve according to the relation between the concentration of the fluorescent carbon dot solution and the relative fluorescence intensity variation value;
and adding a sample to be detected into the fluorescent carbon dot solution, measuring the fluorescent intensity of the obtained mixed solution before and after the reaction, substituting the fluorescent intensity into the standard curve of the Dimethoate, and calculating the content of the Dimethoate in the sample to be detected.
10. The method of detecting dimethoate as claimed in claim 9, wherein the concentration of said fluorescent carbon dot solution is 0.2-0.6mg/mL.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110412005A (en) * | 2019-08-30 | 2019-11-05 | 贵州大学 | A kind of dimethoate pesticide detection method based on aptamers regulation carbon dots fluorescence |
CN110697681A (en) * | 2019-10-12 | 2020-01-17 | 青海大学 | Method for preparing carbon dots from broad beans, carbon dots and application thereof |
CN113025322A (en) * | 2021-03-11 | 2021-06-25 | 武汉轻工大学 | High-fluorescence carbon dot powder, preparation method thereof and application thereof in nitroimidazole drug detection |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN110412005A (en) * | 2019-08-30 | 2019-11-05 | 贵州大学 | A kind of dimethoate pesticide detection method based on aptamers regulation carbon dots fluorescence |
CN110697681A (en) * | 2019-10-12 | 2020-01-17 | 青海大学 | Method for preparing carbon dots from broad beans, carbon dots and application thereof |
CN113025322A (en) * | 2021-03-11 | 2021-06-25 | 武汉轻工大学 | High-fluorescence carbon dot powder, preparation method thereof and application thereof in nitroimidazole drug detection |
Non-Patent Citations (1)
Title |
---|
DIANWEI ZHANG ET AL.: ""Red-to-blue colorimetric probe based on biomass carbon dots for smartphone-integrated optosensing of Cu(II) and L-cysteine"", SPECTROCHIMICA ACTA PART A: MOLECULAR AND BIOMOLECULAR SPECTROSCOPY, vol. 290, pages 1 - 10 * |
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