CN116376544B - Fluorescent carbon dot, preparation method thereof and application thereof in detection of 5-hydroxymethylfurfural - Google Patents
Fluorescent carbon dot, preparation method thereof and application thereof in detection of 5-hydroxymethylfurfural Download PDFInfo
- Publication number
- CN116376544B CN116376544B CN202310358714.9A CN202310358714A CN116376544B CN 116376544 B CN116376544 B CN 116376544B CN 202310358714 A CN202310358714 A CN 202310358714A CN 116376544 B CN116376544 B CN 116376544B
- Authority
- CN
- China
- Prior art keywords
- fluorescent carbon
- hydroxymethylfurfural
- carbon dots
- reaction
- application
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- NOEGNKMFWQHSLB-UHFFFAOYSA-N 5-hydroxymethylfurfural Chemical compound OCC1=CC=C(C=O)O1 NOEGNKMFWQHSLB-UHFFFAOYSA-N 0.000 title claims abstract description 44
- RJGBSYZFOCAGQY-UHFFFAOYSA-N hydroxymethylfurfural Natural products COC1=CC=C(C=O)O1 RJGBSYZFOCAGQY-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 26
- 229910052799 carbon Inorganic materials 0.000 title abstract description 26
- 238000001514 detection method Methods 0.000 title description 15
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 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
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000000502 dialysis Methods 0.000 claims description 14
- 238000005119 centrifugation Methods 0.000 claims description 5
- 244000118350 Andrographis paniculata Species 0.000 claims description 3
- 239000000243 solution Substances 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 12
- 239000007864 aqueous solution Substances 0.000 description 8
- 230000008859 change Effects 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- 238000007605 air drying Methods 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 230000005284 excitation Effects 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 235000012907 honey Nutrition 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 241000746375 Andrographis Species 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 238000000695 excitation spectrum Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- 229930091371 Fructose Natural products 0.000 description 1
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 1
- 239000005715 Fructose Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical group C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000003172 aldehyde group Chemical group 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 125000004029 hydroxymethyl group Chemical group [H]OC([H])([H])* 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
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012797 qualification Methods 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
-
- 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
-
- 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
-
- 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
-
- 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"
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Immunology (AREA)
- Optics & Photonics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Biophysics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The application relates to a fluorescent carbon dot, a preparation method thereof and application thereof in detecting 5-hydroxymethylfurfural, wherein the preparation method of the fluorescent carbon dot comprises the following steps: s1: cutting herba Andrographitis leaves, adding mixed solution of isopropanol and water, and stirring; s2: transferring the mixture obtained in the step S1 into a reaction kettle, and reacting for 6-12h at 140-220 ℃; 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 fluorescent carbon dots prepared by the method have stable properties, good water solubility and dispersibility, and good selectivity to 5-hydroxymethylfurfural, and the fluorescent carbon dots are obviously quenched by adding 5-hydroxymethylfurfural into the solution of the fluorescent carbon dots, so that the fluorescent carbon dots can be used for detecting 5-hydroxymethylfurfural.
Description
Technical Field
The application relates to detection of fluorescent carbon points and 5-hydroxymethylfurfural, in particular to a fluorescent carbon point and a preparation method thereof, and application of the fluorescent carbon point in detection of 5-hydroxymethylfurfural.
Background
The 5-hydroxymethylfurfural is a chemical substance generated by dehydrating glucose or fructose, the molecular structure of the 5-hydroxymethylfurfural contains a furan ring, an aldehyde group and a hydroxymethyl, the chemical property is relatively active, and various derivatives can be prepared through oxidation, hydrogenation, condensation and other reactions, so that the 5-hydroxymethylfurfural is an important fine chemical raw material. At the same time, the 5-hydroxymethyl furfural also has sensitizationExcess 5-hydroxymethylfurfural is harmful to human body. In honey processing, heating is typically required to reduce viscosity and prevent crystallization or fermentation, whereas when the heating temperature is higher, 5-hydroxymethylfurfural is produced. The standard of honey industry in China (GH/T18796-2012) prescribes that the qualification standard of the 5-hydroxymethylfurfural content in honey is below 40 mg/kg. Therefore, it is of great importance to provide a method capable of detecting 5-hydroxymethylfurfural. For example, chinese patent CN111363542A provides a method for utilizing CaF 2 A method for detecting 5-hydroxymethylfurfural.
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 detection of 5-hydroxymethylfurfural 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 detection of 5-hydroxymethylfurfural.
In a first aspect of the present application, a method for preparing fluorescent carbon dots is provided, comprising the steps of:
s1: cutting herba Andrographitis leaves, adding mixed solution of isopropanol and water, and stirring;
s2: transferring the mixture obtained in the step S1 into a reaction kettle, and reacting for 6-12h at 140-220 ℃;
s3: and naturally cooling after the reaction is finished, centrifuging, filtering, dialyzing and freeze-drying the reaction product to obtain the fluorescent carbon dots.
Further, in the step S1, the dosage of the mixed solution of the isopropyl alcohol and the water is 10-20mL, and the dosage of the water is 130-140mL based on the dosage of the common andrographis herb of 10-15 g.
Further, in the step S2, the reaction temperature is 175-185 ℃ and the reaction time is 7-9h.
Further, in the step S3, the centrifugation method is to centrifuge for 5-20min at 7000-10000 r/m.
Further, in the step S3, the filtering method is to filter with a 0.2-0.3 μm filter membrane.
Further, in the step S3, the dialysis method is that the dialysis treatment is carried out for 48-72 hours through a dialysis bag of 500-1000 Da.
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 an application of a fluorescent carbon dot in detecting 5-hydroxymethylfurfural, wherein the fluorescent carbon dot is the fluorescent carbon dot of the second aspect.
According to the application, the fluorescent carbon dots are prepared by a specific preparation method, and the prepared fluorescent carbon dots are stable in property, have good water solubility and dispersibility, and show good selectivity to 5-hydroxymethylfurfural, and when 5-hydroxymethylfurfural is added into the solution of the fluorescent carbon dots, the fluorescence of the fluorescent carbon dots is obviously quenched, so that the fluorescent carbon dots can be used for detecting the 5-hydroxymethylfurfural.
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 carbon dots prepared in example 1;
FIG. 3 is a fluorescence emission spectrum of fluorescent carbon dots after reaction with 5-hydroxymethylfurfural of different concentrations;
FIG. 4 is a graph of the linear response of fluorescent carbon dots to 5-hydroxymethylfurfural described in example 1.
Detailed Description
The following describes a fluorescent carbon dot, a preparation method thereof and application thereof in detecting 5-hydroxymethylfurfural 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", 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 the indicated technical features. Moreover, "first," "second," "third," etc. are for non-exhaustive list description purposes only, and it should be understood that no closed limitation on the number is made.
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: cutting herba Andrographitis leaves, adding mixed solution of isopropanol and water, and stirring;
s2: transferring the mixture obtained in the step S1 into a reaction kettle, and reacting for 6-12h at 140-220 ℃;
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 preparation method, the andrographis paniculata leaves are used as raw materials, fluorescent carbon dots are obtained through a one-step hydrothermal method, the prepared fluorescent carbon dots are stable in property, have good water solubility and dispersibility, and show good selectivity to 5-hydroxymethylfurfural, and when 5-hydroxymethylfurfural is added into a solution of the fluorescent carbon dots, fluorescence of the fluorescent carbon dots is obviously quenched, so that the preparation method can be used for detecting the 5-hydroxymethylfurfural. In some specific examples, the detection linear range is 0.1-10. Mu.M and the detection limit is 0.047. Mu.M.
Meanwhile, the preparation method has the advantages of easily available raw materials, simple steps and mild reaction conditions.
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 the mixed solution of the isopropyl alcohol and the water is 10-20mL, and the amount of the water is 130-140mL, based on the amount of the common andrographis herb of 10-15 g. In particular, isopropanol dosages include, but are not limited to: 10mL, 12mL, 14mL, 16mL, 18mL, 20mL; the amount of water includes, but is not limited to: 130mL, 132mL, 134mL, 136mL, 138mL, 140mL.
Further, in the step S2, the reaction temperature is 175-185 ℃ and the reaction time is 7-9h. 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: 7h, 7.5h, 8h, 8.5h, 9h. Further, the reaction temperature was 180℃and the reaction time was 8 hours.
Further, in the step S3, the centrifugation method is to centrifuge for 5-20min at 7000-10000 r/m. Specifically, rotational speeds include, but are not limited to: 7000r/m, 7500r/m, 7800r/m, 8000r/m, 8200r/m, 8500r/m, 9000r/m, 9500r/m, 10000r/m; centrifugation times include, but are not limited to: 5min, 8min, 10min, 12min, 15min, 18min, and 20min. Further, in the step S3, the centrifugation is performed at 8000r/m for 10min.
Further, in the step S3, the filtering method is to filter with a 0.2-0.3 μm filter membrane. 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 48-72 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, 60h, 65h, 72h.
In other examples of the present application, there is also provided a fluorescent carbon dot prepared by the preparation method described above.
In further examples of the application, there is also provided the use of fluorescent carbon dots as above in the detection of 5-hydroxymethylfurfural.
Without limitation, the method for detecting 5-hydroxymethylfurfural comprises the steps of:
(1) 3mL of an aqueous solution of the fluorescent carbon dots with the concentration of 0.2mg/mL is prepared;
(2) Gradually dropwise adding 20 mu L of aqueous solutions (the concentration is changed from 0 to 12 mu M) of 5-hydroxymethylfurfural with different concentrations into the aqueous solution of the fluorescent carbon point, so that the fluorescence of the fluorescent carbon point is gradually quenched;
(3) And measuring the fluorescence intensity before and after the reaction of the aqueous solution of the fluorescent carbon point, calculating a relative fluorescence intensity change value, and establishing a standard curve of the 5-hydroxymethylfurfural according to the relation between the concentration of the aqueous solution of the 5-hydroxymethylfurfural and the relative fluorescence intensity change value.
(4) Quantitative detection: and (3) adding a sample to be detected into the aqueous solution of the fluorescent carbon dots, recording the fluorescent intensity of the solution of the fluorescent carbon dots before and after the reaction, and calculating the content of 5-hydroxymethylfurfural by referring to the standard curve obtained in the step (3).
Example 1:
the embodiment is a preparation method of fluorescent carbon dots, comprising the following steps:
s1: cutting 10g of herba Andrographitis leaves (picked from Guangdong university of Industrial science), adding 10mL of mixed solution of isopropanol and 140mL of water, and stirring thoroughly;
s2: transferring the mixture into a polytetrafluoroethylene reaction kettle, and reacting for 8 hours at 180 ℃ in a forced air drying box;
s3: and (3) naturally cooling after the reaction is finished, centrifuging the reaction product at 8000r/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 48h, 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 2.38±0.4nm. FIG. 2 is a graph of fluorescence excitation and emission spectra of the fluorescent carbon dots, showing that under excitation at 340nm, the fluorescent carbon dots emit blue light with a peak at 452 nm.
Example 2:
the embodiment is a preparation method of fluorescent carbon dots, comprising the following steps:
s1: cutting 12g of herba Andrographitis leaves (picked from Guangdong university of Industrial science), adding 15mL of mixed solution of isopropanol and 135mL of water, and stirring thoroughly;
s2: transferring the mixture into a polytetrafluoroethylene reaction kettle, and reacting for 8 hours at 220 ℃ in a forced air drying box;
s3: and (3) naturally cooling after the reaction is finished, centrifuging the reaction product at 10000r/m for 15min, filtering the solution by using a 0.22 mu m filter membrane, dialyzing the obtained filtrate by using a 500Da dialysis bag for 72h, 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: cutting 15g of andrographis paniculata leaves, adding a mixed solution of 20mL of isopropanol and 130mL of water, and fully and uniformly stirring;
s2: transferring the mixture into a polytetrafluoroethylene reaction kettle, and reacting for 10 hours at 220 ℃ in a forced air drying box;
s3: and (3) naturally cooling after the reaction is finished, centrifuging the reaction product at 10000r/m for 20min, filtering the solution by using a 0.22 mu m filter membrane, dialyzing the obtained filtrate by using a 500Da dialysis bag for 72h, and freeze-drying to obtain the fluorescent carbon dots.
Example 4:
the embodiment is the application of fluorescent carbon dots in detecting 5-hydroxymethylfurfural, and the steps of detecting 5-hydroxymethylfurfural are as follows:
(1) Redispersing the fluorescent carbon dots prepared in example 1 in deionized water to prepare a carbon dot solution with a concentration of 0.2 mg/mL;
(2) Respectively taking 3mL of carbon dot solution, gradually dropwise adding 20 mu L of 5-hydroxymethylfurfural solution (0-12 mu M) with different concentrations into the carbon dot solution, and quenching fluorescence of fluorescent carbon dots to different degrees along with the addition of the 5-hydroxymethylfurfural solution;
(3) And measuring the fluorescence intensity before and after the reaction of the aqueous solution of the fluorescent carbon point, calculating the relative fluorescence intensity change value, calculating the detection range and the detection limit of the fluorescent carbon point to the 5-hydroxymethylfurfural according to the relation between the concentration of the 5-hydroxymethylfurfural and the relative fluorescence intensity change value, wherein the fluorescence emission spectra of the fluorescent carbon point after the reaction of the 5-hydroxymethylfurfural with different concentrations are shown in the figure 3. The linear detection range is 0.1-10 mu M, the detection limit is 0.047 mu M, and the linear regression equation after fitting is shown in FIG. 4 and can be expressed as follows:
Y＝0.089X+0.0233。
(4) And taking a sample to be detected into the aqueous solution of the fluorescent carbon dots, 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 the 5-hydroxymethylfurfural in the sample to be detected.
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 (6)
1. An application of fluorescent carbon dots in detecting 5-hydroxymethylfurfural, wherein the preparation method of the fluorescent carbon dots comprises the following steps:
s1: cutting herba Andrographitis leaves, adding mixed solution of isopropanol and water, and stirring;
s2: transferring the mixture obtained in the step S1 into a reaction kettle, and reacting for 6-12h at 140-220 ℃;
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 use according to claim 1, wherein in step S1, the amount of isopropanol and the amount of water are 10-20mL and 130-140mL respectively, based on the amount of andrographis paniculata used as 10-15 g.
3. The use according to claim 1, wherein in step S2 the reaction is carried out at a temperature of 175-185 ℃ for a time of 7-9 hours.
4. Use according to any one of claims 1 to 3, wherein in step S3, the centrifugation is carried out at a speed of 7000-10000r/m for 5-20min.
5. The use according to any one of claims 1 to 3, wherein in step S3, the filtration is carried out using a 0.2-0.3 μm filter.
6. Use according to any one of claims 1 to 3, wherein in step S3 the dialysis is performed by dialysis in a dialysis bag of 500-1000Da for 48-72 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310358714.9A CN116376544B (en) | 2023-04-06 | 2023-04-06 | Fluorescent carbon dot, preparation method thereof and application thereof in detection of 5-hydroxymethylfurfural |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310358714.9A CN116376544B (en) | 2023-04-06 | 2023-04-06 | Fluorescent carbon dot, preparation method thereof and application thereof in detection of 5-hydroxymethylfurfural |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116376544A CN116376544A (en) | 2023-07-04 |
| CN116376544B true CN116376544B (en) | 2023-09-08 |
Family
ID=86978335
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310358714.9A Active CN116376544B (en) | 2023-04-06 | 2023-04-06 | Fluorescent carbon dot, preparation method thereof and application thereof in detection of 5-hydroxymethylfurfural |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116376544B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107523295A (en) * | 2017-08-29 | 2017-12-29 | 湖南农业大学 | A kind of fluorescent carbon point for the method and its preparation for preparing fluorescent carbon point as raw material using common flos traditional Chinese medicine material |
| KR20190001349A (en) * | 2017-06-27 | 2019-01-04 | 경희대학교 산학협력단 | Preparation method of Carbon Quantum-dot |
| CN109749738A (en) * | 2017-11-01 | 2019-05-14 | 浙江糖能科技有限公司 | Sulfonation carbon quantum dot, preparation method and the application in 5 hydroxymethyl furfural is being prepared as catalyst |
| WO2019211809A1 (en) * | 2018-05-04 | 2019-11-07 | Universidade Do Porto | Chemiluminescent imidazopyrazinone-based photosensitizers with available singlet and triplet excited states |
| CN111439742A (en) * | 2020-04-16 | 2020-07-24 | 河南理工大学 | Preparation method of white light carbon dots |
| CN112033941A (en) * | 2020-06-30 | 2020-12-04 | 中南民族大学 | Method for rapidly detecting resveratrol in food |
| CN113042004A (en) * | 2021-04-13 | 2021-06-29 | 昆明理工大学 | Preparation method and application of modified carbon-based material |
| CN114408896A (en) * | 2020-12-30 | 2022-04-29 | 宁德师范学院 | Method for synthesizing fluorescent carbon dots by using tea leaves as carbon source through one-step method and application of method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170050851A1 (en) * | 2015-08-18 | 2017-02-23 | Transfert Plus, Société En Commandite | Method for manufacturing carbon quantum dots |
| US20200205415A1 (en) * | 2017-07-26 | 2020-07-02 | Merck Patent Gmbh | Composition |
-
2023
- 2023-04-06 CN CN202310358714.9A patent/CN116376544B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190001349A (en) * | 2017-06-27 | 2019-01-04 | 경희대학교 산학협력단 | Preparation method of Carbon Quantum-dot |
| CN107523295A (en) * | 2017-08-29 | 2017-12-29 | 湖南农业大学 | A kind of fluorescent carbon point for the method and its preparation for preparing fluorescent carbon point as raw material using common flos traditional Chinese medicine material |
| CN109749738A (en) * | 2017-11-01 | 2019-05-14 | 浙江糖能科技有限公司 | Sulfonation carbon quantum dot, preparation method and the application in 5 hydroxymethyl furfural is being prepared as catalyst |
| WO2019211809A1 (en) * | 2018-05-04 | 2019-11-07 | Universidade Do Porto | Chemiluminescent imidazopyrazinone-based photosensitizers with available singlet and triplet excited states |
| CN111439742A (en) * | 2020-04-16 | 2020-07-24 | 河南理工大学 | Preparation method of white light carbon dots |
| CN112033941A (en) * | 2020-06-30 | 2020-12-04 | 中南民族大学 | Method for rapidly detecting resveratrol in food |
| CN114408896A (en) * | 2020-12-30 | 2022-04-29 | 宁德师范学院 | Method for synthesizing fluorescent carbon dots by using tea leaves as carbon source through one-step method and application of method |
| CN113042004A (en) * | 2021-04-13 | 2021-06-29 | 昆明理工大学 | Preparation method and application of modified carbon-based material |
Non-Patent Citations (1)
| Title |
|---|
| Red-to-blue colorimetric probe based on biomass carbon dots for smartphone-integrated optosensing of Cu(II) and L-cysteine;Dianwei Zhang等;《Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy》;第290卷;第122285-1-122285-10页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116376544A (en) | 2023-07-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108929672B (en) | Carbon quantum dot using shrimp shell as carbon source, preparation method thereof and application thereof in ascorbic acid detection | |
| CN111530437B (en) | Sulfonic acid functionalized covalent organic framework magnetic composite material with mixed action mode and preparation method and application thereof | |
| CN115138369B (en) | Molybdenum trioxide composite material and preparation method and application thereof | |
| CN116376544B (en) | Fluorescent carbon dot, preparation method thereof and application thereof in detection of 5-hydroxymethylfurfural | |
| CN111413311A (en) | Water content detection reagent and method for detecting water content in liquid | |
| MJ Alshamri et al. | Removal of toxic textile dyes from aqueous solution through adsorption onto coconut husk waste: Thermodynamic and isotherm studies | |
| WO2017125246A1 (en) | Method for elemental analysis | |
| CN112033941B (en) | Method for rapidly detecting resveratrol in food | |
| CN110964349A (en) | Oxidation modified carbon black and preparation method thereof | |
| CN116640571B (en) | Fluorescent carbon dot, preparation method thereof and application thereof in detection of Dimethoate | |
| CN109603893A (en) | A kind of preparation method of Cu, Sr doping SBA-16 mesopore molecular sieve | |
| Ahmad et al. | Studies on Tannins from Barks of Pinus roxbughii | |
| CN111847426A (en) | Preparation method of carbon quantum dots and application of carbon quantum dots in element detection | |
| CN108827896B (en) | Lead ion detection method | |
| EP0210333A2 (en) | Active carbon and process for its manufacture | |
| CN113817801A (en) | Method for determining activity of formate dehydrogenase in plant leaves and evaluating formate dehydrogenase in plant leaves | |
| Su et al. | A novel Ln-MOF-based cataluminescence sensor for detection of propionaldehyde | |
| CN110095574A (en) | Acetylacetone,2,4-pentanedione gas sensitive material and the preparation method and application thereof | |
| CN115672275B (en) | Magnetic nano biological carbonaceous material and preparation method and application thereof | |
| CN116891739B (en) | Method for preparing phosphorus-doped carbon quantum dots by taking calcium gluconate as raw material and application of phosphorus-doped carbon quantum dots in hexavalent chromium ion detection | |
| DE19728873C2 (en) | Chemical analysis with activated carbon adsorbent | |
| CN114891232B (en) | Cerium-terephthalic acid metal organic framework material and preparation method and application thereof | |
| CN112516981B (en) | Preparation method of low-titanium-load titanium-silicon material for diesel desulfurization and method for testing number of surface catalytic active sites of low-titanium-load titanium-silicon material | |
| CN111060498B (en) | Method for testing coating sequence of titanium dioxide film layer | |
| CN116990354A (en) | Composite gas-sensitive material, preparation method thereof and propane gas-sensitive sensor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |