CN111272717A - One-step hydrothermal synthesis based on novel ionic liquid fluorescent carbon dots and application of one-step hydrothermal synthesis to detection of sulfathiazole - Google Patents
One-step hydrothermal synthesis based on novel ionic liquid fluorescent carbon dots and application of one-step hydrothermal synthesis to detection of sulfathiazole Download PDFInfo
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- JNMRHUJNCSQMMB-UHFFFAOYSA-N sulfathiazole Chemical compound C1=CC(N)=CC=C1S(=O)(=O)NC1=NC=CS1 JNMRHUJNCSQMMB-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229960001544 sulfathiazole Drugs 0.000 title claims abstract description 38
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 29
- 238000001514 detection method Methods 0.000 title claims abstract description 24
- 239000002608 ionic liquid Substances 0.000 title claims abstract description 17
- 230000035945 sensitivity Effects 0.000 claims abstract description 8
- 239000007850 fluorescent dye Substances 0.000 claims abstract description 6
- 230000007613 environmental effect Effects 0.000 claims abstract description 4
- 239000000523 sample Substances 0.000 claims abstract description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 25
- 229910052799 carbon Inorganic materials 0.000 claims description 25
- 239000000047 product Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000012528 membrane Substances 0.000 claims description 13
- 230000000171 quenching effect Effects 0.000 claims description 10
- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 claims description 10
- 229940124530 sulfonamide Drugs 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- FZWLAAWBMGSTSO-UHFFFAOYSA-N Thiazole Chemical compound C1=CSC=N1 FZWLAAWBMGSTSO-UHFFFAOYSA-N 0.000 claims description 7
- -1 tetrafluoroborate Chemical compound 0.000 claims description 7
- 238000007865 diluting Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- 230000005284 excitation Effects 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 6
- 238000010791 quenching Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 229910021392 nanocarbon Inorganic materials 0.000 description 3
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 229940088710 antibiotic agent Drugs 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 241000194017 Streptococcus Species 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000005251 capillar electrophoresis Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000029142 excretion Effects 0.000 description 1
- 230000003394 haemopoietic effect Effects 0.000 description 1
- 230000002949 hemolytic effect Effects 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 238000003018 immunoassay Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229960000282 metronidazole Drugs 0.000 description 1
- VAOCPAMSLUNLGC-UHFFFAOYSA-N metronidazole Chemical compound CC1=NC=C([N+]([O-])=O)N1CCO VAOCPAMSLUNLGC-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000175 potential carcinogenicity Toxicity 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 150000003456 sulfonamides Chemical class 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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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
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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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- 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
Abstract
The invention discloses one-step hydrothermal synthesis based on novel ionic liquid fluorescent carbon dots and detection application of the novel ionic liquid fluorescent carbon dots to sulfathiazole. The novel sulfathiazole fluorescent probe synthesized by the invention has the advantages of simple preparation process, low cost and high selectivity, has high sensitivity and accuracy for detecting trace amount of sulfathiazole remained in an environmental sample, and has wide application prospect in the field of analysis and detection of sulfathiazole.
Description
Technical Field
The invention belongs to the technical field of synthesis of fluorescent carbon dot nano materials and detection and identification of sulfonamides antibiotics, and particularly relates to one-step hydrothermal synthesis based on novel ionic liquid fluorescent carbon dots and detection application of the one-step hydrothermal synthesis to sulfathiazole.
Background
The sulfathiazole is a sulfanilamide antibiotic with a sulfanilamide structure, is widely applied to livestock and poultry production, and is mainly used for preventing and treating infection of pathogenic bacteria such as meningococcus, hemolytic streptococcus, pneumococcus and the like. Because the sulfathiazole is difficult to metabolize in organisms and can enter the environment through biological excretion and other modes, the sulfathiazole is detected in surface water, soil and other environment media. Researches show that the sulfathiazole can harm the immune system of a human body, influence the hematopoietic function and have potential carcinogenicity, so that the development of a simple and efficient method capable of quickly detecting the trace amount of the sulfathiazole remained in the environment is very important.
At present, the commonly used detection methods such as immunoassay, liquid chromatography, capillary electrophoresis, liquid chromatography-mass spectrometry and the like have the defects of complex operation, high detection cost, long detection time consumption, poor sensitivity and specific identification and the like, and are difficult to directly carry out on-site real-time rapid detection on the sulfathiazole remained in the environment. The fluorescent carbon dots serving as a novel fluorescent carbon nano material have high stability, good biocompatibility and environmental friendliness, can be used as a high-performance nano fluorescent probe, quickly realize high-sensitivity detection and analysis on a target object, and can accurately detect the residual sulfathiazole in the environment.
However, some of the existing nano fluorescent probes have the problems of complex synthesis process, high synthesis cost, low selectivity and sensitivity, and the like, and how to realize the preparation of the high-performance fluorescent probe by a simple synthesis method has become a hot point of research.
Disclosure of Invention
The invention solves the technical problem of providing a method for preparing nano fluorescent carbon dots by a one-step hydrothermal method by taking ionic liquid as a carbon source, which is simple in synthesis and low in cost, wherein the optimal excitation/emission wavelengths of the prepared fluorescent carbon dots are 284nm and 385 nm respectively, the stability is good, the detection rate is high, the sensitivity is high, and the performance of high-selectivity identification on sulfathiazole is realized.
The invention adopts the following technical scheme for solving the technical problems, and is based on one-step hydrothermal synthesis of novel ionic liquid fluorescent carbon dots and detection application of the fluorescent carbon dots to sulfathiazole, and the method is characterized by comprising the following specific processes: the novel fluorescent carbon dots are synthesized by one-step hydrothermal reaction at 140-220 ℃ by taking 1-allyl-3-vinylimidazole tetrafluoroborate as a carbon source, malonic acid as a passivating agent and water as a solvent, have the effect of specifically identifying the sulfathiazole as a fluorescent probe, and can be used for identifying the trace sulfathiazole in an environmental sample with high sensitivity.
The invention relates to one-step hydrothermal synthesis based on novel ionic liquid fluorescent carbon dots and detection application of the novel ionic liquid fluorescent carbon dots to sulphathiazole, which are characterized by comprising the following specific steps of: respectively adding 1-allyl-3-vinyl imidazole tetrafluoroborate, malonic acid and water into a high-temperature reaction kettle, reacting at 140-220 ℃ for 3-12 h, separating and purifying the obtained product by a 0.22 mu m filter membrane, and collecting supernatant to be stored in a brown bottle at low temperature of 4 ℃.
Further preferably, the feeding molar ratio of the 1-allyl-3-vinyl imidazole tetrafluoroborate to the malonic acid is 0.2-1.8: 0.5-3.
The invention relates to one-step hydrothermal synthesis based on novel ionic liquid fluorescent carbon dots and detection application of the novel ionic liquid fluorescent carbon dots to sulphathiazole, which are characterized by comprising the following specific steps of: respectively adding 1.6650 g of 1-allyl-3-vinylimidazole tetrafluoroborate, 0.7805 g of malonic acid and 10 mL of pure water into a high-temperature reaction kettle, carrying out hydrothermal reaction for 12 h at 220 ℃, separating and purifying the obtained product by a 0.22 mu m filter membrane, diluting the product by 50 times to obtain fluorescent carbon dots for later use, placing 80 mu L of fluorescent carbon dots and sulfanilamide thiazole aqueous solution with different concentration gradients in a centrifuge tube, diluting the fluorescent carbon dots and the sulfanilamide thiazole aqueous solution to 2 mL, mixing and reacting for 2min at room temperature, placing the mixed solution in a fluorescence spectrophotometer, measuring the fluorescence intensity of the mixed solution under the condition of an excitation wavelength of 284nm, calculating the corresponding fluorescence intensity, and then calculating the correspondingQuenching effect, and obtaining the linear range of 0.008-10 mg L-1And 10-45 mg L-1Detection limit of 5 μ g L-1。
Compared with the prior art, the invention has the following advantages:
1. the invention firstly provides one-step hydrothermal synthesis based on novel ionic liquid fluorescent carbon dots and detection application thereof to sulfathiazole, and the preparation process is simple, the cost is low and the operation is convenient;
2. the prepared fluorescent carbon dots have good stability, high detection rate and high sensitivity, and have high selective identification performance on sulfathiazole;
3. the method adopts 1-allyl-3-vinyl imidazole tetrafluoroborate as a carbon source to prepare the fluorescent carbon dots, and can be used for detecting and analyzing trace sulfathiazole in an actual environment sample.
Drawings
FIG. 1 is a graph of fluorescence intensity of fluorescent carbon dots prepared in example 1 at different pH;
FIG. 2 is a graph showing the fluorescence quenching effect of the carbon fluorescent dots prepared in example 1 on sulfathiazole at different pH values;
FIG. 3 is a linear curve of the fluorescence response of the fluorescent carbon dots prepared in example 1 to sulfathiazole at room temperature;
FIG. 4 is a selective recognition test chart of the fluorescent carbon dots prepared in example 1 for sulfathiazole in sulfanilamide antibiotics.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
1.11 g of 1-allyl-3-vinyl imidazole tetrafluoroborate, 0.2602 g of malonic acid and 10 mL of pure water are respectively added into a high-temperature reaction kettle, the mixture undergoes a hydrothermal reaction at 220 ℃ for 12 hours, and the obtained product is separated and purified by a 0.22 mu m filter membrane and then diluted by 50 times for later use.
Example 2
1.11 g of 1-allyl-3-vinyl imidazole tetrafluoroborate, 0.5215 g of malonic acid and 10 mL of pure water are respectively added into a high-temperature reaction kettle, the hydrothermal reaction is carried out for 12 hours at the high temperature of 180 ℃, and the obtained product is separated and purified by a filter membrane of 0.22 mu m and then diluted by 50 times for standby.
Example 3
1.6650 g of 1-allyl-3-vinylimidazole tetrafluoroborate, 0.7805 g of malonic acid and 10 mL of pure water are respectively added into a high-temperature reaction kettle, the hydrothermal reaction is carried out for 3 hours at the high temperature of 220 ℃, and the obtained product is separated and purified by a 0.22 mu m filter membrane and then diluted by 50 times for later use.
Example 4
1.11 g of 1-allyl-3-vinyl imidazole tetrafluoroborate, 1.0406 g of malonic acid and 20 mL of pure water are respectively added into a high-temperature reaction kettle, the hydrothermal reaction is carried out for 12 hours at the high temperature of 220 ℃, and the obtained product is separated and purified by a filter membrane of 0.22 mu m and then diluted by 50 times for standby.
Example 5
1.11 g of 1-allyl-3-vinyl imidazole tetrafluoroborate, 0.5215 g of malonic acid and 10 mL of pure water are respectively added into a high-temperature reaction kettle, the hydrothermal reaction is carried out for 12 hours at the high temperature of 220 ℃, and the obtained product is separated and purified by a filter membrane of 0.22 mu m and then diluted by 50 times for standby.
Example 6
0.2220 g of 1-allyl-3-vinylimidazole tetrafluoroborate, 0.7805 g of malonic acid and 10 mL of pure water are respectively added into a high-temperature reaction kettle, the hydrothermal reaction is carried out for 12 hours at the high temperature of 220 ℃, and the obtained product is separated and purified by a 0.22 mu m filter membrane and then diluted by 50 times for later use.
Example 7
1.6650 g of 1-allyl-3-vinylimidazole tetrafluoroborate, 0.7805 g of malonic acid and 10 mL of pure water are respectively added into a high-temperature reaction kettle, the hydrothermal reaction is carried out for 12 hours at the high temperature of 220 ℃, and the obtained product is separated and purified by a 0.22 mu m filter membrane and then diluted by 50 times for later use.
Example 8
1.11 g of 1-allyl-3-vinyl imidazole tetrafluoroborate, 0.5215 g of malonic acid and 10 mL of pure water are respectively added into a high-temperature reaction kettle, the hydrothermal reaction is carried out for 12 hours at the high temperature of 140 ℃, and the obtained product is separated and purified by a 0.22 mu m filter membrane and then diluted by 50 times for standby.
Example 9
1.6650 g of 1-allyl-3-vinylimidazole tetrafluoroborate, 0.7805 g of malonic acid and 10 mL of pure water are respectively added into a high-temperature reaction kettle, the hydrothermal reaction is carried out for 6 hours at the high temperature of 220 ℃, and the obtained product is separated and purified by a 0.22 mu m filter membrane and then diluted by 50 times for later use.
Example 10
80 μ L of each of the fluorescent carbon dot materials prepared in examples 1 to 9 was added to 60 μ L of 100 mg L molar concentration-1Mixing the sulfathiazole aqueous solution at room temperature, reacting for 2min, 5min, 10 min, 20 min, and 30min, measuring fluorescence intensity with fluorescence spectrophotometer, and calculating fluorescence quenching rate (F)0-F)/F (wherein F0Carbon spot initial fluorescence intensity, F carbon spot fluorescence intensity after adding sulfathiazole). Fluorescence quenching rate of nanocarbon points to sulfathiazole prepared in examples 1 to 9 (F)0-F)/F are each: 0.420, 0.384, 0.393, 0.406, 0.409, 0.410, 0.460, 0.358 and 0.398, and the analysis result shows that the fluorescent carbon dots prepared in example 7 have high sensitivity and accuracy on the identification and detection of the sulfathiazole.
Example 11
80 μ L of the fluorescent carbon dot material prepared in example 7 was added to an aqueous solution having a pH of 1 to 14, mixed and reacted at room temperature for 2min, and measured by a fluorescence spectrophotometer. As shown in FIG. 1, the fluorescence intensity of the carbon spot remained substantially constant between pH 3 and pH 11, indicating that the carbon spot has a certain acid-base resistance.
Example 12
80 mu L of the fluorescent carbon dot material prepared in the example 1 is taken and then respectively added into the sulfathiazole aqueous solution with the pH value of 3-11, and the mixture is fully mixed and reacted for 2min at room temperature and is measured by a fluorescence spectrophotometer. As shown in FIG. 2, the quenching rate of the carbon dot on the sulfathiazole fluorescence remains unchanged between pH 3 and pH 11, and the carbon dot has better stability.
Example 13
80 μ L of the fluorescent carbon dot material prepared in example 1 was taken and added to 0.008 mg L of the fluorescent carbon dot material-1、0.01 mg L-1、0.05 mg L-1、0.1 mg L-1、0.5 mg L-1、1 mg L-1、3 mg L-1、5 mg L-1、10 mg L-1、12.5 mg L-1、15 mg L-1、20 mg L-1、25 mg L-1、30 mg L-1、35 mg L-1、40 mg L-1、45 mg L-1The sulfathiazole aqueous solution is fully mixed and reacted for 2min at room temperature, and the reaction is measured by a fluorescence spectrophotometer. As a result, as shown in FIG. 3, the quenching rate (F) of the carbon spot fluorescence0the-F)/F becomes larger with the increase of the concentration of the sulfathiazole.
Example 14
80 μ L of the fluorescent carbon dot material prepared in example 1 was taken, and then added to the fluorescent carbon dot material at a concentration of 0.01 mg L-1Sulphathiazole, 0.03 mg L-1Sulfadiazine, 0.05 mg L-1Sulfapyridine, 0.03 mg L-1Sulfadimidine, 0.03 mg L-1Sulfamonomethoxine, 0.05 mg L-1Sulfamethoxazole and 0.05 mg L-1Mixing the aqueous solution of metronidazole at room temperature for 2min, measuring fluorescence intensity with fluorescence spectrophotometer, and calculating fluorescence quenching rate (F)0-F)/F. The result shows that the fluorescence quenching rate of the nano carbon dot material to the sulfathiazole is 0.027, but the nano carbon dot material has no obvious quenching effect to other structural analogues, and the result is shown in fig. 4, which shows that the prepared fluorescent carbon dot material has strong specific recognition capability.
The foregoing embodiments illustrate the principles, principal features and advantages of the invention, and it will be understood by those skilled in the art that the invention is not limited to the foregoing embodiments, which are merely illustrative of the principles of the invention, and that various changes and modifications may be made therein without departing from the scope of the principles of the invention.
Claims (4)
1. One-step hydrothermal synthesis based on novel ionic liquid fluorescent carbon dots and detection application of the ionic liquid fluorescent carbon dots to sulfathiazole are characterized by comprising the following specific steps: the novel fluorescent carbon dots are synthesized by one-step hydrothermal reaction at 140-220 ℃ by taking 1-allyl-3-vinylimidazole tetrafluoroborate as a carbon source, malonic acid as a passivating agent and water as a solvent, have the specific identification effect on the sulfathiazole by taking the novel fluorescent carbon dots as a fluorescent probe, and can be used for identifying the trace sulfathiazole in an environmental sample with high sensitivity.
2. The one-step hydrothermal synthesis and detection application of sulfanilamide thiazole based on the novel ionic liquid fluorescent carbon dot as claimed in claim 1, which is characterized by comprising the following specific steps: respectively adding 1-allyl-3-vinyl imidazole tetrafluoroborate, malonic acid and water into a high-temperature reaction kettle, reacting at 140-220 ℃ for 3-12 h, separating and purifying the obtained product by a 0.22 mu m filter membrane, and collecting supernatant to be stored in a brown bottle at low temperature of 4 ℃.
3. The one-step hydrothermal synthesis and detection application of sulfanilamide thiazole based on the ionic liquid novel fluorescent carbon dot as claimed in claim 1 or 2, characterized in that: the feeding molar ratio of the 1-allyl-3-vinyl imidazole tetrafluoroborate to the malonic acid is 0.2-1.8: 0.5-3.
4. The one-step hydrothermal synthesis and detection application of sulfanilamide thiazole based on the novel ionic liquid fluorescent carbon dot as claimed in claim 1 or 2, which is characterized by comprising the following specific steps: respectively adding 1.6650 g of 1-allyl-3-vinyl imidazole tetrafluoroborate, 0.7805 g of malonic acid and 10 mL of pure water into a high-temperature reaction kettle, carrying out a high-temperature hydrothermal reaction for 12 h at 220 ℃, separating and purifying the obtained product by a 0.22 mu m filter membrane, diluting the product by 50 times to obtain fluorescent carbon dots for later use, placing 80 mu L of the fluorescent carbon dots and sulfanilamide thiazole aqueous solution with different concentration gradients in a centrifuge tube, diluting the fluorescent carbon dots and the sulfanilamide thiazole aqueous solution to 2 mL, mixing and reacting for 2min at room temperature, placing the mixed solution in a fluorescence spectrophotometer, measuring the fluorescence intensity of the mixed solution under the condition of an excitation wavelength of 284nm, calculating the corresponding fluorescence quenching effect, and obtaining the linear range of the fluorescence quenching effect which is 0.008-1And 10-45 mg L-1Detection limit of 5 μ g L-1。
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CN115228459A (en) * | 2022-06-14 | 2022-10-25 | 珠海科技学院 | Preparation method and application of imidazole-based ionic liquid carbonized polymer dot gel spheres |
CN116515481A (en) * | 2023-05-06 | 2023-08-01 | 河南工学院 | Ratio fluorescent probe based on carbon point, construction and application of ratio fluorescent probe to detection of quercetin |
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