CN114181696B - Double-color near-infrared emission carbon nano dot fluorescent nano material and synthesis method and application thereof - Google Patents
Double-color near-infrared emission carbon nano dot fluorescent nano material and synthesis method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of carbon-based fluorescent nano materials, in particular to a bicolor near-infrared emission carbon nano point (DNIECNDs) fluorescent nano material, and a synthesis method and application thereof. The nano material is of an amorphous structure, has the particle size of 7-10 nm, contains C, N, B and O elements, has the optimal excitation wavelength of 650nm and the emission wavelength of 700nm and 730nm. The preparation method is that o-phenylenediamine is used as a nitrogen source, boric acid is used as a boron source, a hydrothermal method is adopted for preparation, and the nano material is used for fluorescence detection of piroxicam drugs. The invention is DNIECNDs with double-color near infrared fluorescence emission characteristic and stable fluorescence, and uses the DNIECNDs as a fluorescent probe to construct a fluorescent nano sensor for detecting piroxicam with high sensitivity and high selectivity, has better specificity on the piroxicam, can realize high-sensitivity and high-selectivity fluorescent quantitative analysis of the piroxicam without fluorescent labeling, and has simple, quick and wide linear detection range.
Description
Technical Field
The invention relates to the technical field of carbon-based fluorescent nanomaterials, in particular to a bicolor near-infrared emission carbon nano dot fluorescent nanomaterial, a synthesis method and application thereof.
Background
Compared with other analysis methods, the fluorescence analysis method has the advantages of high sensitivity, strong selectivity, accuracy, rapidness, relatively simple instrument operation and the like, and is widely focused by analysis workers, and is widely applied to various fields such as medicine analysis, environmental protection, food inspection and the like. Fluorescent probes are widely used in various detection and labeling applications, such as pesticide residue determination, metal ion determination, biomolecule content determination, biomolecule labeling, macromolecule labeling, cell and subcellular structure determination, and the like.
In recent years, the good optical properties of carbon-based nanomaterials have made them of great potential in the preparation of fluorescent probes. Compared with the traditional organic dye and semiconductor quantum dot, the carbon-based nanomaterial has the advantages of good water solubility, chemical inertness, simple synthesis, adjustable surface property, low toxicity, photo-bleaching resistance and the like, and has been widely applied to various research fields. The doped fluorescent carbon-based nanomaterial is used as a derivative material of the fluorescent carbon-based nanomaterial, and has unique optical properties, environmental friendliness and high quantum yield, so that the doped fluorescent carbon-based nanomaterial is of interest to more and more researchers.
Research shows that hetero atoms with the atomic radius and bond energy similar to those of carbon atoms are doped in the molecular frame of the fluorescent carbon-based nano material, and the regulation and control of certain photoelectric properties or physical and chemical properties (such as fluorescent luminous groups, surface activity, chemical active sites, electronic properties and the like) of the fluorescent carbon-based nano material can be realized, so that the fluorescent carbon-based nano material shows optical properties different from those of traditional fluorescent carbon points. In general, the emission wavelength of the doped fluorescent carbon-based nanomaterial will show a certain difference according to the different types and contents of the hetero atoms, so that the adjustment and control of the probe sites or wave bands can be realized by searching for a proper carbon source or synthesis condition of the doped atoms. Meanwhile, the fluorescent spectrum band of the doped fluorescent carbon-based nanomaterial is relatively narrow, the half-peak width is generally between 30nm and 50nm, the fluorescent intensity is stable, bleaching resistance and quantum yield are high, so that the fluorescent carbon-based nanomaterial gradually replaces the traditional fluorescent carbon dots to be applied to the field of fluorescent analysis and detection, the possibility is provided for developing and constructing a novel multifunctional fluorescent probe, and the application range of the carbon-based nanomaterial is widened.
Disclosure of Invention
Aiming at the defects existing in the prior art, the novel N, B doped carbon-based nanomaterial with double-color near infrared emission is designed and synthesized in view of the fact that the doped carbon-based nanomaterial can change the electronic property of the traditional fluorescent carbon point and provide more active sites, so that the fluorescent carbon point has excellent fluorescent property, and meanwhile, nitrogen (N) and boron (B) atoms are equivalent to carbon atoms in size, so that uniform doping and uniform intrinsic defects can be formed, and the fluorescent sensor is constructed based on the N, B doped carbon-based nanomaterial and applied to the rapid and effective detection of piroxicam.
The technical scheme adopted by the invention for achieving the purpose is as follows: a dual-color near-infrared emission carbon nano dot fluorescent nano material is of an amorphous structure, has a particle size of 7-10 nm, contains C, N, B and O elements, has an optimal excitation wavelength of 650nm and an emission wavelength of 700nm and 730nm.
A preparation method of a double-color near-infrared emission carbon nano dot fluorescent nano material takes o-phenylenediamine as a nitrogen source and boric acid as a boron source, and adopts a hydrothermal method to prepare the material, wherein the preparation steps comprise:
(1) O-phenylenediamine and boric acid are dissolved in deionized water, and uniform suspension is formed under the ultrasonic action at room temperature;
(2) Transferring the obtained solution into a polytetrafluoroethylene high-temperature reaction kettle, reacting for 18 hours at 180 ℃, naturally cooling to room temperature, placing the obtained solution in a refrigerator for 5-10 days, and standing to remove the large-size fluorescent carbon-based nanomaterial;
(3) And (3) centrifugally cleaning the collected red solution, and preserving the supernatant at 4 ℃ to obtain the product.
Further, the method comprises the steps of,
the resistivity of the deionized water is 18MΩ & cm -1 。
Further, the method comprises the steps of,
the molar concentration ratio of the o-phenylenediamine to the boric acid is 1:1-1.5, and is preferably 1:1.31.
An application of a double-color near-infrared emission carbon nano dot fluorescent nanomaterial for fluorescence detection of piroxicam drugs.
Further, the detecting step includes:
(1) 10.0 mu L of nano material stock solution is measured and placed in a 1.5mL centrifuge tube, 50 mu L of phosphate buffer solution and 50mM of phosphate buffer solution are sequentially added, and then the mixture is separatedAdding 1.0mM piroxicam standard solution with different volumes and sample to be tested containing unknown concentration of piroxicam respectively, mixing the mixed solution at room temperature, incubating for 5-10 min, incubating with 18MΩ cm -1 The deionized water is fixed to 500 mu L and is kept stand for reaction for 20min;
(2) Measuring the change of fluorescence intensity of the obtained reaction solution under the conditions that the excitation wavelength is 650nm and the widths of excitation and emission slits are 5nm, and taking the concentration of piroxicam added into the reaction system as an abscissa, and changing the fluorescence intensity of the solution [ (FL) 0 -FL)/FL 0 ]Drawing a standard curve with the ordinate;
(3) Detecting the piroxicam concentration of the standard solution according to the fluorescence quenching degree [ (FL) of the sample to be detected by referring to the step (1) 0 -FL)/FL 0 ]And (3) comparing the standard curve with the standard curve, and calculating the piroxicam concentration in the sample.
Further, the method comprises the steps of,
the pH value of the phosphate buffer solution is 6.0-8.0.
Further, the method comprises the steps of,
the concentration of the piroxicam standard solution is 0.05-200 mu M.
Further, the method comprises the steps of,
the fluorescence intensity changes were recorded as peak changes at emission wavelengths 700nm and 730nm.
Further, the method comprises the steps of,
the phosphate buffer pH was 7.0.
The double-color near-infrared emission carbon nano dot fluorescent nano material and the synthetic method and application thereof have the beneficial effects that: the invention synthesizes the bicolor near-infrared emission carbon nano dots (DNIECNDs) with good water solubility, uniform dispersion, bicolor near-infrared emission fluorescence and stable fluorescence by adopting a simple and rapid hydrothermal method, and constructs the fluorescent nano sensor for detecting the piroxicam with high sensitivity and high selectivity by taking the DNIECNDs as a fluorescent probe. The test result shows that the DNIECNDs prepared by the invention have better specificity on the piroxicam, can realize high-sensitivity and high-selectivity fluorescence quantitative analysis of the piroxicam without fluorescent labeling, and have simple and quick method and wide linear detection range. In addition, the product prepared by the invention not only provides an effective way for efficiently detecting the piroxicam, has potential application value, but also is beneficial to expanding the application range of the carbon-based fluorescent material in drug detection.
Drawings
FIG. 1A is a Transmission Electron Microscope (TEM) of DNIECNDs of an embodiment of the present invention;
b is electron diffraction Structures (SAED) of DNIECNDs of embodiments of the invention;
c is the X-ray energy spectrum analysis (EDS) of DNIECNDs of the embodiment of the invention;
FIG. 2 is a graph of ultraviolet spectra of DNIECNDs and emission spectra of DNIECDNs at 650nm excitation wavelength according to an embodiment of the invention;
FIG. 3 is an optimized plot of excitation wavelengths for DNIECNDs in accordance with an embodiment of the present invention;
fig. 4 is a diagram showing a feasibility analysis of detecting piroxicam by dnieclcds according to the embodiment of the present invention;
FIG. 5 is a graph showing the effect of pH on DNIECNDs fluorescence intensity according to an embodiment of the present invention;
FIG. 6A is a fluorescence spectrum of DNIECNDs of the invention at different concentrations of piroxicam (0-200 μm);
b is the relative fluorescence intensity [ (FL) of DNIECNDs according to the embodiment of the invention 0 -FL)/FL 0 ]A standard curve graph for quantitatively detecting piroxicam along with the change of the concentration of the piroxicam;
FIG. 7 is a graph showing the selectivity results of the detection of piroxicam by DNIECNDs according to the embodiment of the present invention.
Detailed Description
The invention is described in further detail below with reference to the attached drawings and detailed description:
example 1:
a dual-color near-infrared emission carbon nano dot fluorescent nano material is of an amorphous structure, has a particle size of 7-10 nm, contains C, N, B and O elements, has an optimal excitation wavelength of 650nm and an emission wavelength of 700nm and 730nm.
A preparation method of a double-color near-infrared emission carbon nano dot fluorescent nano material takes o-phenylenediamine as a nitrogen source and boric acid as a boron source, and adopts a hydrothermal method to prepare the material, wherein the preparation steps comprise:
(1) O-phenylenediamine and boric acid (molar concentration ratio is 1:1-1.31) are dissolved in 18MΩ cm -1 . In deionized water, forming uniform suspension under the ultrasonic action at room temperature;
(2) Transferring the obtained solution into a polytetrafluoroethylene high-temperature reaction kettle, reacting for 18 hours at 180 ℃, naturally cooling to room temperature, placing the obtained solution in a refrigerator for 5-10 days, and standing to remove the large-size fluorescent carbon-based nanomaterial;
(3) And (3) centrifugally cleaning the collected red solution, and preserving the supernatant at 4 ℃ to obtain the product.
The preparation principle of the nano material is as follows: in view of the heteroatom with the radius and bond energy similar to those of carbon atoms, the photoelectric property or physical and chemical properties of the fluorescent carbon-based nanomaterial can be regulated and controlled, and the N, B atoms are equivalent to the carbon atoms in size and can form uniform doping and uniform intrinsic defects.
An application of a double-color near-infrared emission carbon nano dot fluorescent nanomaterial for fluorescence detection of piroxicam drugs.
The detection step comprises the following steps:
(1) Weighing 10.0 mu L of nano material stock solution, placing the nano material stock solution into a 1.5mL centrifuge tube, sequentially adding 50 mu L of 50mM phosphate buffer solution with pH of 6.0-8.0, then respectively adding different volumes of 1.0mM piroxicam standard solution and a sample to be detected containing piroxicam with unknown concentration, fully mixing the mixed solution at room temperature, incubating for 5-10 minutes, and then using 18MΩ cm -1 The deionized water of (2) is fixed to 500 mu L (the concentration of the piroxicam standard solution is 0.05-200 mu M), and the mixture is left to stand for reaction for 20min;
(2) The change in fluorescence intensity of the reaction solution obtained above was measured under the conditions of an excitation wavelength of 650nm and excitation and emission slit widths of 5nm, and the change in fluorescence intensity was recorded as peak changes at emission wavelengths of 700nm and 730nm.And the concentration of piroxicam added into the reaction system is taken as the abscissa, and the fluorescence intensity of the solution is changed [ (FL) 0 -FL)/FL 0 ]Drawing a standard curve with the ordinate;
(3) Detecting the piroxicam concentration of the standard solution according to the fluorescence quenching degree [ (FL) of the sample to be detected by referring to the step (1) 0 -FL)/FL 0 ]And (3) comparing the standard curve with the standard curve, and calculating the piroxicam concentration in the sample.
Drawing the standard curve and calculating the piroxicam content in the sample to be measured by adopting a standard addition method.
Example 2:
a double-color near-infrared emission carbon nano dot fluorescent nano material,
preparing a carbon nano dot fluorescent nano material DNIECNDs by a hydrothermal method:
(1) 0.2g of o-phenylenediamine and 0.15g of boric acid were dissolved in 8mL of 18 M.OMEGA.cm -1 In deionized water, a uniform suspension is formed under the ultrasonic action at room temperature.
(2) Transferring the obtained solution into a polytetrafluoroethylene high-temperature reaction kettle, reacting for 18 hours at 180 ℃, naturally cooling to room temperature, placing the obtained solution in a refrigerator for 5 days, and standing to remove the large-size fluorescent carbon-based nanomaterial;
(3) And (3) carrying out centrifugal cleaning on the collected red solution, wherein the centrifugal cleaning rotating speed is 10,000rpm, the centrifugal time is 20min, and the supernatant is preserved at 4 ℃ to obtain DNIECNDs with excellent fluorescence performance.
Characterization of materials: in order to study the surface morphology and the element composition of the synthesized DNIECNDs, the invention firstly carries out a series of characterization on the DNIECNDs, and the characterization results are shown in figures 1, 2, 3 and 4.
FIG. 1 is a Transmission Electron Microscope (TEM), electron diffraction Structure (SAED) and X-ray spectroscopy (EDS) of DNIECNDs, and it can be seen from FIG. 1A that DNIECNDs are monodispersed spherical particles having a relatively uniform particle diameter of about 7-10 nm, SAED analysis of FIG. 1B shows that DNIECNDs prepared by the method are amorphous structures, and FIG. 1C demonstrates that the prepared DNIECNDs mainly contain C, N, B and O three elements.
In FIG. 2, a is an ultraviolet spectrum of DNIECNDs, and b is a fluorescence spectrum of DNIECNDs at an excitation wavelength of 650 nm. The prepared dniecncds were characterized by uv-vis absorption and fluorescence emission spectra. FIG. 2 is a graph of the ultraviolet-visible absorption spectrum of an aqueous dispersion of DNIECNDs. As shown in figure a, the ultraviolet-visible spectrum of DNIECNDs shows three absorption peaks at 235nm, 285nm and 424nm, respectively. As shown in panel b, DNIECNDs exhibit distinct fluorescence emission peaks at 700nm and 730nm when the excitation wavelength is 650 nm.
FIG. 3 is a graph of fluorescence spectra of DNIECNDs at different excitation wavelengths. As shown in the figure, when the excitation wavelength is increased from 610nm to 680nm, the fluorescence peak intensities of DNIECNDs at both 700nm and 730nm are gradually increased with the increase of the excitation wavelength, and then gradually decreased with the increase of the excitation wavelength. It can be seen from FIG. 3 that the maximum excitation wavelength of DNIECNDs synthesized in this example is at 650 nm.
Fig. 4 is a feasibility analysis of DNIECNDs for detecting piroxicam. In order to verify that DNIECNDs can realize effective detection of drugs, the embodiment verifies the feasibility of DNIECNDs to detect piroxicam. As shown in FIG. 4, a is that DNIECNDs have stronger fluorescence intensity when piroxicam is not added into DNIECNDs solution, and b is that when piroxicam (100 mu M) with a certain concentration is added into DNIECNDs solution, the emission peak intensities of DNIECNDs at 700nm and 730nm generate quenching behaviors, which indicates that the DNIECNDs generate obvious fluorescence quenching phenomenon under the condition of the presence of the piroxicam. Therefore, DNIECNDs can be used as a simple and effective fluorescent probe for fluorescence detection of piroxicam.
Example 3:
in this embodiment, the method for detecting piroxicam by using DNIECNDs as a label-free fluorescent probe includes the steps of:
weighing 5 parts of 10.0 mu L of DNIECNDs stock solution prepared by the method, placing into a 1.5mL centrifuge tube, sequentially adding 50 mu L of 50mM phosphate buffer solution with pH of 6.0,6.5,7.0,7.5,8.0, and then adding 1.0mM piroxicam with the same volume respectivelyStandard solution, after the mixed solution is fully mixed at room temperature, incubating for 10min, and then incubating with 18M omega cm -1 The deionized water is fixed to 500 mu L and is kept stand for 20min for reaction; finally, the change of the maximum fluorescence intensity of the obtained reaction solution is measured under the conditions that the excitation wavelength is 650nm and the excitation and emission slit widths are 5 nm.
As can be seen from FIG. 5, the optimal pH of the PBS buffer solution in the detection system was pH 7.0.
Example 4:
responsivity of fluorescence sensor to piroxicam:
in this example, a series of different concentrations of piroxicam were measured in 50mm buffer solution in PBS at ph=7.0 according to the procedure of example 1, and the results are shown in fig. 6, and fig. 6A shows the change in fluorescence intensity of dniecncds over a concentration range of 0 to 200 μm for piroxicam. As can be seen from fig. 6A, with increasing piroxicam concentration, as can be seen from fig. 6B, the fluorescence intensity of DNIECNDs at 700nM and 730nM is continuously reduced, and the fluorescence intensity change in this embodiment records the peak change at the emission wavelength of 730nM, and piroxicam shows a good linear relationship in the concentration range of 0.05-10 μm, and the detection limit is 15.7nM. The above results fully demonstrate that the fluorescence sensor designed by the invention has good fluorescence response to piroxicam.
Example 5:
selective detection of piroxicam by DNIECNDs fluorescent probes:
weighing 14 parts of the DNIECNDs stock solution prepared by the method, placing into a 1.5mL centrifuge tube, sequentially adding 50 mu L of 50mM phosphate buffer solution with pH of 7.0, respectively adding standard solutions of 1.0mM piroxicam, glucose, lactose, sucrose, fructose, cysteine, glutathione, dopamine, doxorubicin, heparin, captopril, meloxicam, acyclovir and chloramphenicol with the same volume, fully mixing the mixed solutions at room temperature, incubating for 10min, incubating for 18M omega cm -1 The deionized water is fixed to 500 mu L and is kept stand for 20min for reaction; finally, under the conditions of 650nm excitation wavelength and 5nm excitation and emission slit width, the maximum fluorescence intensity of the obtained reaction solution is measuredAnd (3) degree change.
Fig. 7 is a view of the selectivity of the present invention for the fluorescence sensor constructed with piroxicam in a PBS buffer solution with ph=7.0, mainly for the interference substances including glucose, lactose, sucrose, fructose, cysteine, glutathione, dopamine, doxorubicin, heparin, captopril, meloxicam, acyclovir, chloramphenicol which may be present in complex actual samples, and as a result, the present invention shows that DNIECNDs have good selectivity for detecting piroxicam as a fluorescent probe and are relatively less affected by other potential interference species, indicating that DNIECNDs have specific and stable interactions and fluorescent responses for piroxicam, which has a very important significance for selectively detecting piroxicam in actual samples.
Example 6:
and (3) detecting an actual sample:
(1) Weighing 10.0 mu L of nano material stock solution, placing the nano material stock solution into a 1.5mL centrifuge tube, sequentially adding 50 mu L of 50mM phosphate buffer solution with pH of 7.0, then respectively adding different volumes of 1.0mM piroxicam standard solution and the same volumes of 1.0 mu M, 50.0 mu M and 150.0 mu M commercial tablet piroxicam sample to be tested, fully mixing the mixed solution at room temperature, incubating for 5-10 minutes, and then incubating with 18M omega cm -1 The deionized water of (2) is fixed to 500 mu L (the concentration of the piroxicam standard solution is 0.05-200 mu M), and the mixture is left to stand for reaction for 20min;
(2) The change in fluorescence intensity of the reaction solution obtained above was measured under the conditions of an excitation wavelength of 650nm and excitation and emission slit widths of 5nm, and the change in fluorescence intensity was recorded as peak changes at emission wavelengths of 700nm and 730nm. And the concentration of piroxicam added into the reaction system is taken as the abscissa, and the fluorescence intensity of the solution is changed [ (FL) 0 -FL)/FL 0 ]Drawing a standard curve with the ordinate;
(3) Detecting the piroxicam concentration of the standard solution according to the fluorescence quenching degree [ (FL) of the sample to be detected by referring to the step (1) 0 -FL)/FL 0 ]And (3) comparing the piroxicam concentration with the standard curve, calculating the concentration of the piroxicam in the sample, and calculating the recovery rate.
Table 1 shows the practical applicability of the fluorescence sensor designed by the present invention in the analysis and detection of actual samples, by taking piroxicam in commercial tablets measured by standard addition method. The results are shown in Table 1, the recovery rate of piroxicam is between 98.31% and 100.4%, and the relative standard deviation is less than 4.83%, which shows that the method of the embodiment of the invention has better reliability.
The result shows that the novel piroxicam fluorescence detection method based on DNIECNDs can effectively realize high-sensitivity and high-selectivity detection of piroxicam in commercial tablets, is simple, quick and wide in linear detection range, provides an effective way for efficiently detecting the piroxicam in an actual sample, and has potential application value.
Table 1 results of piroxicam detection in commercial tablets
The invention synthesizes DNIECDNs with good water solubility, uniform dispersion, fluorescence characteristic and stable fluorescence by adopting a simple and rapid hydrothermal method, and constructs the fluorescent nanosensor for detecting piroxicam with high sensitivity and high selectivity by taking the DNIECNDs as fluorescent probes. The test result shows that the DNIECNDs prepared by the invention have better specificity on the piroxicam, can realize high-sensitivity and high-selectivity fluorescence quantitative analysis of the piroxicam without fluorescent labeling, and have simple, quick and linear detection range. The product prepared by the invention not only provides an effective way for efficiently detecting the piroxicam, but also is beneficial to expanding the application range of the carbon-based fluorescent material in drug detection.
In the preparation method of the invention, the addition sequence and specific reaction steps of various materials can be adjusted by a person skilled in the art, so that the preparation method is suitable for small-scale preparation in a laboratory and industrial mass production in a chemical plant. In industrial mass production, specific reaction parameters can be determined experimentally by those skilled in the art.
Unless otherwise specified, the experimental methods used in the following examples are all conventional methods.
Reagents, materials, and the like used in the examples described below were obtained commercially or synthesized from commercially available starting materials unless otherwise specified.
The above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the essence of the present invention are intended to be included within the scope of the present invention.
Claims (7)
1. A synthesis method of a bicolor near-infrared emission carbon nano dot fluorescent nano material is characterized by comprising the following steps: the nano material is of an amorphous structure, has the particle size of 7-10 nm, contains C, N, B and O elements, has the optimal excitation wavelength of 650nm and the emission wavelength of 700nm and 730 nm;
the preparation method comprises the following steps of:
(1) O-phenylenediamine and boric acid are dissolved in deionized water, and uniform suspension is formed under the ultrasonic action at room temperature;
(2) Transferring the obtained solution into a polytetrafluoroethylene high-temperature reaction kettle, reacting at 180 ℃ for 18-h, naturally cooling to room temperature, placing the obtained solution in a refrigerator for 5-10 days, and standing to remove the large-size fluorescent carbon-based nanomaterial;
(3) Centrifugally cleaning the collected red solution, and preserving supernatant at 4 ℃ to obtain a product;
the resistivity of the deionized water is 18M ohm cm -1 ；
The molar concentration ratio of the o-phenylenediamine to the boric acid is 1:1-1.5.
2. The method for synthesizing the bicolor near-infrared emission carbon nano dot fluorescent nanomaterial according to claim 1, wherein the method is characterized in that: the molar concentration ratio of the o-phenylenediamine to the boric acid is 1:1.31.
3. An application of the bicolor near-infrared emission carbon nano dot fluorescent nanomaterial prepared by the synthesis method of claim 1, which is characterized in that: the nano material is used for fluorescence detection of piroxicam drugs;
(1) Measuring 10.0 mu L of nano material stock solution, placing the nano material stock solution into a centrifuge tube with the concentration of 1.5mL, sequentially adding 50 mu L of phosphate buffer solution with the concentration of 50mM, then respectively adding 1.0mM piroxicam standard solution with different volumes and a sample to be detected containing piroxicam with unknown concentration, fully mixing the mixed solution at room temperature, incubating for 5-10 minutes, and then using 18M omega cm -1 The deionized water is fixed to 500 mu L and is kept stand for reaction for 20min;
(2) Measuring the change of fluorescence intensity of the obtained reaction solution under the conditions that the excitation wavelength is 650nm and the widths of excitation and emission slits are 5nm, and taking the concentration of piroxicam added into the reaction system as an abscissa, and the change of the fluorescence intensity of the solution [ (FL) 0 -FL)/FL 0 ]Drawing a standard curve with the ordinate;
(3) Detecting the piroxicam concentration of the standard solution according to the fluorescence quenching degree [ (FL) of the sample to be detected by referring to the step (1) 0 -FL)/FL 0 ]And (3) comparing the standard curve with the standard curve, and calculating the piroxicam concentration in the sample.
4. The application of the bicolor near-infrared emission carbon nano dot fluorescent nanomaterial prepared by the synthesis method of claim 3, which is characterized in that:
the pH value of the phosphate buffer solution is 6.0-8.0.
5. The application of the bicolor near-infrared emission carbon nano dot fluorescent nanomaterial prepared by the synthesis method of claim 3, which is characterized in that: the concentration of the piroxicam standard solution is 0.05-200 mu M.
6. The application of the bicolor near-infrared emission carbon nano dot fluorescent nanomaterial prepared by the synthesis method of claim 3, which is characterized in that: the fluorescence intensity changes were recorded as peak changes at emission wavelengths 700nm and 730nm.
7. The application of the bicolor near-infrared emission carbon nano dot fluorescent nanomaterial prepared by the synthesis method of claim 4, which is characterized in that:
the phosphate buffer pH was 7.0.
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