CN111690405A - Fluorescent carbon dot, preparation method thereof and application thereof in copper ion detection - Google Patents
Fluorescent carbon dot, preparation method thereof and application thereof in copper ion detection Download PDFInfo
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- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000001514 detection method Methods 0.000 title claims abstract description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 35
- 229910001431 copper ion Inorganic materials 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 73
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
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- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 claims abstract description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
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- 239000010949 copper Substances 0.000 abstract description 31
- 230000035945 sensitivity Effects 0.000 abstract description 10
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- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
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- 241000058338 Macrobrachium nipponense Species 0.000 description 1
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
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- LJAOOBNHPFKCDR-UHFFFAOYSA-K chromium(3+) trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Cr+3] LJAOOBNHPFKCDR-UHFFFAOYSA-K 0.000 description 1
- GVHCUJZTWMCYJM-UHFFFAOYSA-N chromium(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GVHCUJZTWMCYJM-UHFFFAOYSA-N 0.000 description 1
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
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- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 description 1
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- QZRHHEURPZONJU-UHFFFAOYSA-N iron(2+) dinitrate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QZRHHEURPZONJU-UHFFFAOYSA-N 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 1
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- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 1
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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Abstract
The invention provides a fluorescent carbon dot, a preparation method thereof and application thereof in copper ion detection. The preparation method of the fluorescent carbon dot comprises the following steps: dissolving humic acid and urea in water for heating reaction; and after the reaction is finished, centrifuging, filtering, dialyzing and drying the supernatant obtained by centrifuging to obtain the fluorescent carbon dots. The fluorescent carbon dot has strong fluorescence, high monodispersity, good stability, good water solubility and fluorescence quantum yield; the fluorescent carbon dots are used as fluorescent carbon dot sensors for determining Cu in water samples2+High sensitivity and stabilityGood selectivity, low detection cost and the like, aiming at Cu2+The linear detection concentration range of the sensor is 0.1-2 mu M, has certain competitiveness compared with other sensors, and has Cu in water2+The detection has good application prospect.
Description
Technical Field
The invention belongs to the technical field of carbon quantum dots, and relates to a fluorescent carbon dot, a preparation method thereof and application thereof in copper ion detection.
Background
Cu2+The biological agent poses serious threats to environmental protection, human health and animal survival, and physiological disorders, growth retardation and even death can be caused no matter the biological agent is accumulated in a human body or an animal body to a certain degree. Cu2+The long-term high-concentration exposure can affect the liver and the kidney, is easy to accumulate in human bodies, and is closely related to brain diseases such as Alzheimer disease, Parkinson disease and the like. When entering water, it has a series of influences on the growth and development of aquatic organisms and physiological metabolic processes. Such as Cu2+The effect on the in vivo feeding rate of macrobrachium nipponensis, alkaline phosphatase, pepsin and trypsin and the high toxicity to bromus. For these reasons, Cu2+Have received a great deal of attention in various fields.
In recent years, some highly effective Cu2+Detection strategies are reported. At present, colorimetric methods and electrochemical analysis methods are mainly used for ion detection. However, colorimetric methods require the dyeing of samples, and both methods introduce toxic contaminants or generate toxic products during the experimental process, which may potentially affect the environment and even harm the safety of equipment operation and maintenance personnel. Cu in water samples2+The content of (A) can be measured by atomic absorption spectrometry, atomic emission spectrometry and Differential Pulse Anodic Stripping Voltammetry (DPASV), but all of them have higher detection limit and lower sensitivity. Inductively coupled plasma mass spectrometry (ICP-MS), electrochemical biosensors, inductively coupled plasma optical emission spectroscopy (ICP-OES) have low detection limits, but they require high experimental conditions and the equipment is large, complex and expensive. The construction of a complex sensor improves sensitivity. For example, Chen et al developed a portable multichannel tip microextraction-based Field Sample Preparation (FSP) device that used polymer-based monomers as the extraction phase. The detection limit of the fluorescence spectrum combined with the atomic absorption spectrometry can reach 0.061-0.40 ngL-1. Biological methods include enzyme inhibition, immunoassays and biosensors, and compared to conventional detection techniques, biological methodsThe method has the advantages of convenience, rapidness, economy, easy operation and the like, and is theoretically suitable for Cu2+The field rapid detection. However, the environmental sample has complex elements and much interference, and Cu2+The detection of (2) is still very difficult. Compared with the method, the fluorescence sensor has the advantages of simple preparation, high sensitivity, good selectivity, fast response time, small interference effect, low cost, environmental friendliness and the like. Therefore, Cu is detected by a fluorescent sensor2+Has good application prospect.
Quantum dots are used to fabricate optical sensors due to their unique optical properties, but most conventional quantum dots are fabricated based on semiconductors containing heavy metals, such as zinc and cadmium. Thus, the toxic effects and potential environmental hazards of quantum dots severely limit their practical applications. Compared with heavy metal quantum dots, CDs have the same fluorescence characteristic as the quantum dots, and have the advantages of low toxicity, good stability, convenient preparation, environmental protection and the like, so the CDs can be used as a fluorescent material for replacing the quantum dots. In recent years, CDs have attracted attention as a material for producing fluorescent probe sensors. Currently, CDs are widely used in biomedical and chemical fields, such as bioimaging, drug delivery, gene delivery, sensing, and catalysis. But for biomedical tests the samples need to be handled in a complex way. For example, in the detection of a target substance in blood, it is necessary to separate and dilute a blood sample with physiological saline, and then to incubate and culture red blood cells and the target substance. In vitro cell imaging is more complex with respect to sample processing, requiring not only cell culture, but also seeding and staining of the cells. The chemical sensor is relatively simple to prepare, convenient to operate and wider in application prospect.
Thus, for Cu2+The development of a novel fluorescent carbon dot and a rapid, simple and sensitive detection method are needed.
Disclosure of Invention
Based on the defects in the prior art, the invention aims to provide a preparation method of fluorescent Carbon Dots (CDs), and the invention also aims to provide the fluorescent carbon dots prepared by the method; the invention also aims to provide the application of the fluorescent carbon dot as a fluorescent probe in detecting copper ions in environmental water; the invention also aims to provide a method for detecting copper ions in the environmental water body.
The purpose of the invention is realized by the following technical scheme:
in one aspect, the invention provides a method for preparing a fluorescent carbon dot, which comprises the following steps:
dissolving humic acid and urea in water for heating reaction; and after the reaction is finished, centrifuging, filtering, dialyzing and drying the supernatant obtained by centrifuging to obtain the fluorescent carbon dots.
According to the invention, humic acid and urea are used as raw materials, a hydrothermal method is adopted to synthesize the fluorescent carbon dots, the humic acid raw materials are easy to obtain, and the reaction with the urea can increase the amino groups of the carbon dots. Using the fluorescent carbon dots and Cu2+The internal filtering effect between the two realizes the Cu2+Detecting; the fluorescent carbon dot has strong fluorescence, high monodispersity, good stability, good water solubility and fluorescence quantum yield; the fluorescent carbon dots are used as fluorescent carbon dot sensors for determining Cu in water samples2+Has the advantages of high sensitivity, strong stability, good selectivity, low detection cost and the like, and aims at Cu2+The linear detection concentration range of the sensor is 0.1-2 mu M, has certain competitiveness compared with other sensors, and has Cu in water2+The detection has good application prospect.
In the above method, the molar ratio of the humic acid to the urea is preferably 1 (1 to 5).
In the above method, the heating reaction temperature is preferably 160 to 220 ℃, and the reaction time is preferably 6 to 12 hours.
In the above method, preferably, the method of filtration dialysis is:
and filtering the supernatant obtained by centrifuging through a microporous filter membrane, and dialyzing the filtrate obtained by filtering through a dialysis bag.
In the method, preferably, the pore diameter of the microporous filter membrane is 0.1-0.45 μm, the cut-off molecular weight of the dialysis bag is 600-1500 Da, and the dialysis time is 12-36 h.
On the other hand, the invention also provides the fluorescent carbon dots prepared by the method.
The average grain diameter of the fluorescent carbon dots is less than 30 nm.
In another aspect, the invention also provides an application of the fluorescent carbon dots as a fluorescent probe in detecting copper ions in an environmental water body.
In another aspect, the present invention further provides a method for detecting copper ions in an environmental water body, which comprises the following steps:
adding the fluorescent carbon dots into sodium chloride solutions containing different copper ion concentrations to perform a fluorescence quenching reaction, and establishing a standard curve according to a linear relation between the detected fluorescence intensity and the copper ion concentration;
adding the fluorescent carbon dots into a to-be-detected environmental water body containing sodium chloride to perform fluorescence quenching reaction to obtain fluorescence intensity;
and calculating the concentration of copper ions in the water body of the environment to be measured through the standard curve.
In the above method, preferably, the concentration of the fluorescent carbon dots in the reaction system is 2 to 6mg/mL during the fluorescence quenching reaction.
In the above method, preferably, the concentration of the sodium chloride in the reaction system is 200 to 600mg/L when the fluorescence quenching reaction is performed.
In the method, preferably, when the fluorescence quenching reaction is carried out, the pH value of the reaction system is 6-12; the reaction time is 0.1-20 min.
In the above method, preferably, the linear detection range of the concentration of the copper ions is 0.1 to 2 μ M when the fluorescence quenching reaction is performed.
The invention has the beneficial effects that:
the invention takes humic acid and urea as raw materials, synthesizes fluorescent carbon dots by a hydrothermal method, and utilizes the fluorescent carbon dots and Cu2+The internal filtering effect between the two realizes the Cu2+Detecting; the fluorescent carbon dot has strong fluorescence, high monodispersity, good stability, good water solubility and fluorescence quantum yield; the fluorescent carbon dots are used as fluorescent carbon dot sensors for determining Cu in water samples2+Has the advantages of high sensitivity, strong stability, good selectivity, low detection cost and the like, and aims at Cu2+The linear detection concentration range of the sensor is 0.1-2 mu M, has certain competitiveness compared with other sensors, and has Cu in water2+The detection has good application prospect.
Drawings
FIG. 1 is a TEM image of a fluorescent carbon dot of the present invention;
FIG. 2 is a Fourier transform infrared spectrum of a fluorescent carbon dot of the present invention;
FIG. 3 is a fluorescence emission spectrum of the fluorescent carbon dots of the present invention at different excitation wavelengths;
FIG. 4A shows Cu in the present invention2+A graph of the influence of the concentration of the fluorescent carbon dots on the fluorescence quenching in the detection process;
FIG. 4B shows Cu in the present invention2+A graph of the influence of the pH value of the solution to be detected on the fluorescence intensity of the fluorescent carbon dots in the detection process;
FIG. 4C shows Cu in the present invention2+A graph of the influence of the pH value of the solution to be detected on the fluorescence quenching of the fluorescent carbon dots in the detection process;
FIG. 4D shows Cu in the present invention2+A graph of the effect of reaction time on the fluorescence quenching of the fluorescent carbon dots during detection;
FIG. 5A shows Cu concentrations of different concentrations in the present invention2+A graph of the effect on the fluorescence intensity of fluorescent carbon dots;
FIG. 5B shows Cu concentrations of different concentrations in the present invention2+A linear plot of fluorescence intensity;
FIG. 6A shows Cu in the present invention2+And a fluorescence quenching contrast diagram of the interference ions added into the fluorescent carbon dot solution;
FIG. 6B is a graph showing the comparison of fluorescence quenching when NaCl of different concentrations was added to the fluorescent carbon dot solution according to the present invention.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
The reagents and materials used in the following examples of the invention were as follows:
anhydrous barium chloride, calcium nitrate and aluminum nitrate were purchased from Yili fine chemical Co., Ltd, Beijing. Humic acid (HA, C)9H9NO6) Purchased from Tianjin Guangfu chemical research institute, and anhydrous calcium chloride, manganese chloride, potassium iodide, magnesium nitrate and lead nitrate from Beijing chemical plant. Chromium (III) nitrate nonahydrate, chromium trichloride hexahydrate, urea, nickel nitrate hexahydrate are purchased from Aladdin. Iron nitrate nonahydrate was purchased from fine chemicals, Inc. of modern Orients, Beijing. Cobalt nitrate hexahydrate and zinc nitrate were purchased from Guang-Compound science and technology development Co., Tianjin. Copper nitrate trihydrate is available from beijing western chemical corporation. Ferrous sulfate was purchased from the modern eastern (Beijing) scientific and technological development, Inc. Double Distilled Water (DDW) was used throughout the experiment.
The instruments and equipment used in the experiment are mainly ultraviolet-visible spectrophotometer UV-2600(SDPTOP, Shanghai, China); a Nicolet Magna-IR 750 spectrometer (Thermo, USA); JEM-2100 Transmission Electron microscope (JEOL, Japan); f-7000 spectrofluorometer (Hitachi, Japan).
EXAMPLE 1 preparation of fluorescent Carbon Dots (CDs)
The embodiment provides a preparation method of fluorescent Carbon Dots (CDs), which specifically comprises the following steps:
0.2276g of humic acid and 0.1209g of urea were dissolved in 25mL of water, the molar ratio of humic acid to urea being 1: 2. The mixture was stirred uniformly with ultrasound for 10min to give a brown turbid solution which was transferred to a 30mL autoclave and treated at 180 ℃ for 8 h. Then poured into a 50mL centrifuge tube and centrifuged at 6500rpm for 5 min. Extracting the supernatant, and filtering with 0.22 μm filter membrane to remove larger particles; the obtained solution is purified by a dialysis bag with MWCO of 1000Da at room temperature for 24h, and the fluorescent carbon dots are obtained after drying.
The fluorescent carbon dots are prepared into an aqueous solution of the fluorescent carbon dots and stored at 4 ℃ for later use.
Example 2: method for simulating and detecting copper ions in environmental water body in laboratory
The fluorescence prepared in example 1 aboveAddition of Carbon Dot (CDs) solution to the solution containing different Cu2+Performing fluorescence quenching reaction in sodium chloride solution (sodium chloride content of 200mg/L, pH 6), and detecting fluorescence intensity change and Cu2+Establishing a standard curve according to the linear relation between concentrations;
adding the fluorescent carbon dot solution into a to-be-detected environmental water body containing sodium chloride to perform fluorescence quenching reaction to obtain fluorescence intensity change;
calculating Cu in the water body of the environment to be measured through a standard curve2+The concentration of (c).
This example investigated the different carbon spot concentrations, reaction times and pH values of the reaction system in order to obtain the characteristics of CDs and optimal detection conditions. The excitation wavelength of the fluorescent carbon dots was 275nm, and the excitation slit and emission slit widths were both selected to be 5 nm. Selects different metal ions Cd3+,Al3+,Cr3+,Fe3+,Pb2+,Na+,Ni+,Fe2+,Ba2+,Ca2+,Co2+,Mg2+,As3+,K+,Zn2 +,Hg2+The influence of the interfering ions on the fluorescence of the fluorescent carbon dots is examined as interfering ions, and the detection of Cu is realized2+The selectivity of (a) was investigated. The experimental results and analysis are as follows:
(1) characterization of fluorescent carbon dots
FIG. 1 is a transmission electron microscope image of nanoparticles of the fluorescent carbon dots of the present invention, and it can be seen from FIG. 1 that the average particle size of the fluorescent carbon dots is less than 30 nm.
FIG. 2 is an infrared spectrum of a fluorescent carbon dot of the present invention. As can be seen from fig. 2: 3415 to 3429cm-1The infrared band in the range is due to-OH vibration of phenols and carboxylic acids and stretching of amines-NH. 2028cm-1The peak at (A) indicates that the fluorescent carbon spot contains C.ident.C with the unsaturated bond C.ident.C, 1600cm-1The peak at (a) is-NH stretching vibration. In addition, 1385cm-1Indicates the presence of C-O. These data indicate that the synthesized CDs contain-OH, -NH, and C-O groups, and these characteristic functional groups of CDs confirm that CDs have good water solubility.
FIG. 3 shows the change in excitation-dependent emission spectra of the synthesized CDs when the excitation wavelength is enhanced in the range of 250-290 nm. The fluorescence intensity gradually increases from 250 to 275nm along with the excitation wavelength and then decreases along with the increase of the excitation wavelength from 275 to 290nm, so that 275nm is selected as the optimal excitation wavelength. When the emission wavelength is 300-435 nm, the fluorescence intensity gradually increases to the highest point. This may be due to the different sizes of CDs, or to the different surface states and distributions of functional groups, and may be due to the presence of different surface energy traps on CDs.
(2)Cu2+Influence of fluorescent carbon dot concentration on fluorescence quenching in detection process
In a reaction system to be detected, the concentration of CDs in a solution is related to the initial fluorescence intensity, and the fluorescence intensity determines the linear range of the fluorescence sensor and is a key parameter of the fluorescence sensor. When the concentration of CDs is too low, the quenching effect is not good, and if the concentration is too high, absorption occurs, which affects the analysis result. As shown in FIG. 4A, the fluorescence quenching (F) increased rapidly with increasing CDs concentration before 4mg/L, and then decreased, with 4mg/L being the highest fluorescence quenching. Thus, CDs detect Cu2+The optimal concentration of (B) is 4 mg/L.
(3)Cu2+Influence of pH value of solution to be detected on fluorescence intensity and fluorescence quenching of fluorescent carbon dots in detection process
As shown in FIG. 4C, when the pH value of the solution is changed between 4 and 10, CDs are added to Cu2+The quenching efficiency of (a) increases first and then decreases. The quenching efficiency increased when the pH was between 4 and 6, probably due to the increase in fluorescence of CDs with increasing pH (FIG. 4B). When the pH is between 6 and 10, the quenching efficiency is reduced, probably due to Cu2+Cu not suitable for dissociation under neutral and basic conditions and therefore capable of reacting with CDs2+Lower concentrations result in reduced fluorescence quenching efficiency. The experimental results show that the quenching efficiency reaches a maximum at pH 6. Thus, pH has a significant effect on the fluorescence and quenching of CDs, and pH 6 is the optimal reaction condition for this experiment.
(4)Cu2+Influence of reaction time on fluorescence quenching of fluorescent carbon dots in detection process
The longer time can cause the chemical sensor to lose the original advantages, the shorter time can cause incomplete reaction, the fluorescence quenching is reduced, the linear range is narrow, and the sensitivity is low. Optimizing the reaction time within 0-10 min, and adding Cu2+Thereafter, the fluorescence values were substantially stable with no significant change (FIG. 4D). This illustrates CDs and Cu2+The reaction speed is high, and the sensor has timeliness. According to the experimental results, 2min is fast and stable as the optimal reaction time.
(5) Fluorescent carbon dot fluorescence detection of Cu of example 12+Sensitivity test of
Experiments confirm that the method is applicable to Cu2+The results are shown in fig. 5A and 5B. As can be seen in fig. 5A: with Cu2+The increase in concentration increases the fluorescence quenching efficiency of the CDs. As can be seen from fig. 5B: when Cu2+When the concentration of (A) is 0.1-2 mu M, the two show good linear relation, and the correlation coefficient can reach 0.99871. (F0-F)/F0 shows the efficiency of fluorescence quenching, the abscissa shows the concentration of the control group, and the linear range is 0.1 to 2. mu.M. The method of the invention was compared to the methods reported in the prior art, as shown in table 1.
Table 1:
as can be seen from table 1: compared with the similar carbon dot sensor, the fluorescent carbon dot has a wide linear range and a lower detection limit as the sensor, but the detection limit of the fluorescent carbon dot is higher than that of other sensors, such as a voltammetric sensor based on an electrosynthesis imprinted polymer film, but the preparation of the voltammetric sensor and other sensors is very complicated. Compared with other sensors, has certain competitiveness to Cu in water2+The detection has good application prospect.
(6) Fluorescent carbon dot fluorescence detection of Cu of example 12+Selective experiment of
As shown in fig. 6A, except for Cu2+Comparison and research of Cd3+,Al3+,Cr3+,Fe3+,Pb2+,Na+,Ni+,Fe2+,Ba2+,Ca2+,Co2+,Mg2+,As3+,K+,Zn2+And Hg2+Etc. on CDs.
In this comparative experiment, Cu was added separately2+And other ions, in the reaction system, Cu2+The concentration is 0.6 mu M, and the concentrations of other ions are Cu2+The selectivity was measured by comparing the fluorescence quenching concentration values of 10 times the concentration. On the other hand, other ions and Cu are added simultaneously2+Make up a mixed solution (in the mixed solution, Cu)2+The concentration is 0.6 mu M, and the concentrations of other ions are Cu 2+10 times the concentration) for detecting Cu as another ion pair2+Except for Hg2+Detection of Cu on carbon spots2+There was a slight effect, most cations had no effect. In this experiment, Hg was utilized by adding NaCl solution2+With Cl-To mask Hg2+Impact on the experiment. As shown in FIG. 6B, when the concentration of the salt ion in the reaction system reaches 200mg/L, effective Hg shielding can be achieved2+. Therefore, 200mg/L of salt concentration is selected in the experiment to detect Cu in real water sample2+To reduce interference of other ions.
Example 3 detection of Cu in actual Water sample by fluorescent carbon spots2+Study (2) on
In order to further verify the reliability and feasibility of the method in practical application and also to verify the applicability of the sensor, the present embodiment collects 4 water samples to test Cu2+. These samples were taken from four water samples from Beijing, China and the blank and spiked samples were analyzed with chemical sensors. The experimental conditions of the actually measured water sample are that the pH is 6, the concentration of CDs in the water sample is 4mg/L, and the concentration of NaCl in the water sample is 200 mg/L. The standard concentration is set to be 0-1 mu M, and the experimental results of blank and standard water samples are shown in Table 2.
Table 2:
as can be seen from table 2: CDs as chemical sensor for Cu2+Has higher sensitivity, has certain competitiveness, and can be used for detecting Cu2+The tool of (1).
In conclusion, humic acid and urea are used as raw materials, the fluorescent carbon dots are synthesized by a hydrothermal method, and the fluorescent carbon dots and Cu are utilized2+The internal filtering effect between the two realizes the Cu2+Detecting; the fluorescent carbon dot has strong fluorescence, high monodispersity, good stability, good water solubility and fluorescence quantum yield; the fluorescent carbon dots are used as fluorescent carbon dot sensors for determining Cu in water samples2+Has the advantages of high sensitivity, strong stability, good selectivity, low detection cost and the like, and aims at Cu2+The linear detection concentration range of the sensor is 0.1-2 mu M, has certain competitiveness compared with other sensors, and has Cu in water2+The detection has good application prospect.
Claims (10)
1. A preparation method of a fluorescent carbon dot comprises the following steps:
dissolving humic acid and urea in water for heating reaction; and after the reaction is finished, centrifuging, filtering, dialyzing and drying the supernatant obtained by centrifuging to obtain the fluorescent carbon dots.
2. The method of claim 1, wherein the molar ratio of humic acid to urea is 1: (1-5).
3. The method according to claim 1, wherein the heating reaction temperature is 160-220 ℃ and the reaction time is 6-12 h.
4. The method of claim 1, wherein the method of filtration dialysis is:
filtering the supernatant obtained by centrifuging through a microporous filter membrane, and dialyzing the filtrate obtained by filtering through a dialysis bag;
preferably, the aperture of the microporous filter membrane is 0.1-0.45 μm, the cut-off molecular weight of the dialysis bag is 600-1500 Da, and the dialysis time is 12-36 h.
5. Fluorescent carbon dots prepared by the method of any one of claims 1 to 4;
preferably, the average particle size of the fluorescent carbon dots is less than 30 nm.
6. The use of the fluorescent carbon dot of claim 5 as a fluorescent probe for detecting copper ions in an environmental water body.
7. A method for detecting copper ions in environmental water comprises the following steps:
adding the fluorescent carbon dots of claim 5 into sodium chloride solutions containing different copper ion concentrations to perform a fluorescence quenching reaction, and establishing a standard curve according to a linear relation between the detected fluorescence intensity and the copper ion concentration;
adding the fluorescent carbon dots into a to-be-detected environmental water body containing sodium chloride to perform fluorescence quenching reaction to obtain fluorescence intensity;
and calculating the concentration of copper ions in the water body of the environment to be measured through the standard curve.
8. The method according to claim 7, wherein when the fluorescence quenching reaction is carried out, the concentration of the fluorescent carbon dots in the reaction system is 2-6 mg/mL;
preferably, the concentration of the sodium chloride in the reaction system is 200-600 mg/L during the fluorescence quenching reaction.
9. The method according to claim 7, wherein when the fluorescence quenching reaction is carried out, the pH value of the reaction system is 6-12; the reaction time is 0.1-20 min.
10. The method according to claim 7, wherein the linear detection range of the concentration of the copper ion is 0.1 to 2 μ M when the fluorescence quenching reaction is performed.
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