Fluorescent probe for detecting avenaceum in water as well as preparation method and application of fluorescent probe
The fluorescent probe prepared by the reaction of the dislocation of ten-melon ring and sulfur flavin T at room temperature solved the problem of difficulty in detecting oat dryness in water in the prior art, and achieved a fast, sensitive and highly selective detection effect.
Patent Information
- Application Number
- CN202411409991.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-10
- Publication Date
- 2025-03-14
AI Technical Summary
The prior art is difficult to effectively detect the residuals of oats in water, and traditional detection methods are time-consuming and require large-scale equipment.
A fluorescent probe was prepared by reacting a dislocated aqueous solution of ten-melon ring (ns-Q[10]) and sulfur flavin T (ThT) at room temperature, and the probe was used to identify oatmeal crumbs in the aqueous solution.
It realizes fast, sensitive and highly selective detection of oat crumbs in water, and has the advantages of simplicity of operation, low cost and real-time detection.
Smart Images
Figure CN119614180A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of analytical chemistry, and in particular to a fluorescent probe for detecting oat rust in water, and a preparation method and application thereof. Background Art
[0002] In order to improve the productivity of agricultural production, pesticides are widely used in agriculture, and the residues of pesticides will cause serious harm to human health and ecosystems. Among them, oat blight (DFQ) is a quaternary ammonium herbicide, which is mainly used to control wild oats in the seedling stage of wheat. Since oat blight has certain effective initial and residual activity and is very soluble in water, the pollution of soil and water bodies is a real problem. Therefore, it is very necessary to develop a portable and sensitive method for detecting oat blight in aqueous solution.
[0003] Currently, there are few reports on the detection of oat rust, and the detection methods for pesticides mainly include capillary electrophoresis, gas chromatography-mass spectrometry, etc. These methods are time-consuming and require large equipment. The fluorescent probe detection method has the advantages of high selectivity, simple operation, fast response speed and high sensitivity. Therefore, constructing a suitable fluorescent probe is of great significance for the detection of oat rust residues. Summary of the invention
[0004] In order to solve the above technical problems existing in the prior art, the present invention provides a fluorescent probe for detecting oat rust in water, and a preparation method and application thereof.
[0005] A fluorescent probe for detecting oat rust in water, the specific structural formula of which is as follows:
[0006]
[0007] The method for preparing the fluorescent probe for detecting oat rust in water is prepared by directly reacting an aqueous solution of a dislocated ten-membered cucurbitacin (ns-Q
[10] ) and an aqueous solution of thioflavin T (ThT) at room temperature.
[0008] Further, when the dislocated ten-membered cucurbitacin solution and the thioflavin T solution are mixed, the molar ratio of the dislocated ten-membered cucurbitacin to the thioflavin T in the mixture is 1:1.
[0009] Furthermore, the preparation method comprises the following steps:
[0010] 1) The concentration is 1×10 -4 mol / L dislocated ten-membered cucurbit ring solution;
[0011] 2) The concentration is 1×10 -3 mol / L Thioflavin T solution;
[0012] 3) Mix the dislocated ten-membered cucurbitacin solution and the thioflavin T solution in a molar ratio of 1:1, and then react at room temperature to prepare a 2×10 -5 mol / L probe solution.
[0013] The fluorescent probe for detecting oat rust in water is used in detecting oat rust in water.
[0014] Furthermore, the detection of oat rust in water is to identify oat rust under aqueous medium conditions.
[0015] A method for detecting oat rust in water, using the above-mentioned fluorescent probe for detection.
[0016] Furthermore, the method for detecting oat rust in water specifically comprises the following steps:
[0017] 1) Prepare the probe at a concentration of 2×10 -5 mol / L probe standard solution;
[0018] 2) adding the aqueous solution to be tested to the probe standard solution prepared in step 1), leaving it for 10-40 minutes, then measuring the fluorescence emission spectrum at a fixed excitation wavelength of 448 nm, and plotting a curve of the change in fluorescence intensity at the excited laser wavelength;
[0019] 3) According to the curve of step 2), the change value ΔI of the fluorescence emission spectrum intensity at 493 nm corresponding to the addition of the aqueous solution containing avenate blight to be tested into the fluorescent probe solution is calculated, and the avenate blight in the water can be detected.
[0020] Furthermore, in the step 3), specifically, it is observed whether there is a phenomenon of reduced fluorescence intensity at 493nm. If it occurs, it means that aastacia is contained therein; if not, it means that no aastacia is contained or the content of aastacia is lower than the detection limit; or the color of the solution in the cuvette turns light yellow and quenching occurs under ultraviolet light, which means that the test solution contains aastacia; if the above phenomenon is not observed, it means that no aastacia is contained or the content of aastacia is lower than the detection limit.
[0021] Furthermore, the detection limit is determined by drawing a standard curve.
[0022] Drawing of standard curve:
[0023] (1) Take a quartz cuvette and add 2×10 -5 mol / L fluorescent probe solution, and accurately add 1×10 -2 0.6 μL of 1 mol / L oatmeal standard solution was stirred evenly, and the fluorescence emission spectrum was determined at a fixed excitation wavelength of 448 nm.
[0024] (2) According to the above step (1), a quantitative amount of 0.6 μL of oatmeal standard solution is continuously added to the above 3 mL of probe solution, and a series of fluorescence emission curves are measured at an excitation wavelength of 448 nm until the vertical coordinate value of the fluorescence emission curve changes slowly. The titration operation can be stopped and the fluorescence intensity at the emission wavelength of 493 nm can be plotted.
[0025] (3) With the concentration of oat skewers as the horizontal axis and the difference between the fluorescence emission intensity of the probe at 493 nm and the fluorescence emission intensity of different concentrations of oat skewers added (I0-I) as the vertical axis, a standard curve can be obtained.
[0026] Compared with the prior art, the technical effects created by the present invention are embodied in:
[0027] 1. The fluorescent probe prepared by the present invention is a new type of probe that can detect oat rust in water.
[0028] 2. The detection method of the present invention has the advantages of high sensitivity, high selectivity, low detection cost, simple sample processing, convenient operation, rapid determination and real-time detection.
[0029] 3. During the experiment, it was found that among the 20 pesticides involved in the experiment, the fluorescent probe of the present invention only responded to avenate blight (see Figure 4 ), indicating that the fluorescent probe of the present invention has high selectivity. At the same time, it can quantitatively detect oat rust in the sample to be tested, which has the advantage of quantitative detection.
[0030] 4. The concentration obtained by the present invention is 2.0×10 -5 mol / L fluorescent probe standard solution containing 20 different pesticides was added for testing. The test results are as follows Figure 3 Then, different concentrations of oatmeal were added to the probe solution to obtain different curves, and the standard curve was prepared using the graph. Figure 5 The detection limit was calculated to be 2.63×10 -7 mol / L. BRIEF DESCRIPTION OF THE DRAWINGS
[0031] Figure 1 The fluorescence spectra of the misaligned ten-membered cucurbitacin and thioflavin T (ThT). Among them: a and b are a series of solutions prepared by the molar ratio method, from 0 equivalent to 2.0 equivalent, with an interval of 0.1, and the fluorescence emission spectra of ThT (λex = 448nm); c is a series of solutions prepared by the same Job method, and the fluorescence spectra were obtained by data processing using origin software;
[0032] Figure 2 The NMR experiment and inclusion pattern diagram of the misaligned ten-membered cucurbitacin and thioflavin T (ThT);
[0033] Figure 3 This is a graph showing the test results of adding 20 different pesticides to the fluorescent probe standard solution with a concentration of 2.0×10-5 mol / L prepared by the present invention for testing.
[0034] Figure 4 The fluorescence color change diagram of the probe to 20 pesticides under ultraviolet light (a) and the interference diagram of different pesticides to it in the presence of oat rust (b);
[0035] Figure 5 Fluorescence titration spectra of gradually adding different concentrations of oatmeal solution to the probe standard solution, (d) is a standard curve of the concentration of oatmeal and I0-I according to the curve in (c);
[0036] Figure 6 This is the NMR experimental mechanism diagram of detecting oat tartar with probe solution. DETAILED DESCRIPTION
[0037] The technical solution of the present invention is further defined below in conjunction with specific implementation methods, but the scope of protection required is not limited to the description.
[0038] Embodiment 1:
[0039] The preparation method of each reagent in the analytical method of the present invention is:
[0040] (1) Weigh the dislocated ten-membered melon ring and dissolve it in secondary water with pH = 7 to obtain a concentration of 1×10 -4 mol / L dislocated ten-membered cucurbitacin solution.
[0041] (2) Weigh thioflavin T (ThT) and dissolve it in water at pH 7 to obtain a concentration of 1×10 -3 mol / L Thioflavin T (ThT) solution.
[0042] (3) Mix the two solutions in a molar ratio of 1:1 and react at room temperature for a period of time to obtain a concentration of 2×10 -5 mol / L fluorescent probe standard solution;
[0043] (4) Preparation of other pesticide solutions:
[0044] Accurately weigh the analytically pure standard products of various pesticides required, dissolve them in a secondary aqueous solution of pH = 7 to obtain a concentration of 1×10 -2 mol / L other pesticide standard solutions;
[0045] Embodiment 2:
[0046] The fluorescent probe prepared in Example 1 was used to detect oat blight in water, as follows:
[0047] (1) Determination of standard curve:
[0048] Take 8 5 mL volumetric flasks and add 1.0 × 10 -4 mol / L fluorescent probe solution 1000 μL, and then 1×10 -2 0μL, 0.6μL, 1.2μL, 1.8μL, 2.4μL, 3.0μL, 3.6μL, 4.0μL of mol / L aatrate standard solution were made up to volume with a secondary aqueous solution of pH=7 and shaken evenly. After being allowed to react at room temperature for about 20 minutes, the fluorescence emission spectrum was determined at a fixed excitation wavelength of 448nm. The standard curve was drawn with the concentration of aatrate as the horizontal axis and the difference (ΔI) between the fluorescence emission intensity of the probe at 493nm (I0) and the fluorescence emission intensity (I) of different concentrations of aatrate added as the vertical axis. The detection limit of aatrate detected by the fluorescent probe was calculated based on the slope of the standard curve and the standard deviation σ of the blank values measured 11 times, according to the detection limit calculation formula (3σ / k), see Figure 5 .
[0049] (3) Sample testing:
[0050] Take an aqueous solution containing oat rust and other pesticide standard solutions, add the prepared fluorescent probe standard solution into them, and observe the phenomenon of reduced fluorescence intensity at 493nm under the excitation wavelength of 448nm. Figure 4 Only the aqueous solution containing oat rust showed a decrease in fluorescence intensity at 493 nm; other pesticide standard solutions showed no decrease in fluorescence intensity at 493 nm, indicating that the fluorescent probe of the present invention has high selectivity.
[0051] Finally, it should be pointed out that the above embodiments are only representative examples of the present invention. Obviously, the technical solution of the present invention is not limited to the above embodiments, and there are many variations. All variations that can be directly derived or associated with the content disclosed by ordinary technicians in this field should be considered as the protection scope of the present invention.
Claims
1. A fluorescent probe for detecting oat blight in water, characterized in that: Its specific structural formula is as follows:
2. The method for preparing the fluorescent probe for detecting avenacanthus in water according to claim 1, characterized in that: The method is prepared by directly reacting a dislocated ten-membered cucurbitacin aqueous solution and a thioflavin T aqueous solution at room temperature.
3. The preparation method according to claim 2, characterized in that: When the misaligned ten-membered cucurbitacin solution and the thioflavin T solution are mixed, the molar ratio of the misaligned ten-membered cucurbitacin to the thioflavin T in the mixture is 1:
1.
4. The preparation method according to claim 2, characterized in that: The following steps are involved: 1) The concentration is 1×10 -4 mol / L dislocated ten-membered cucurbit ring solution; 2) The concentration is 1×10 -3 mol / L Thioflavin T solution; 3) Mix the dislocated ten-membered cucurbitacin solution and the thioflavin T solution in a molar ratio of 1:1, and then react at room temperature to prepare a 2×10 -5 mol / L probe solution.
5. Use of the fluorescent probe for detecting oat rust in water according to claim 1 in detecting oat rust in water.
6. The use according to claim 5, characterized in that: The detection of oat rust in water is to identify oat rust under aqueous solution medium conditions.
7. A method for detecting oat rust in water, characterized in that: The fluorescent probe according to claim 1 is used for detection.
8. The method for detecting oat rust in water according to claim 1, characterized in that: The steps include: 1) Prepare the probe at a concentration of 2×10 -5 mol / L probe standard solution; 2) adding the aqueous solution to be tested to the probe standard solution prepared in step 1), leaving it for 10-40 minutes, then measuring the fluorescence emission spectrum at a fixed excitation wavelength of 448 nm, and plotting a curve of the change in fluorescence intensity at the excited laser wavelength; 3) According to the curve of step 2), the change value ΔI of the fluorescence emission spectrum intensity at 493 nm corresponding to the addition of the aqueous solution containing avenate blight to be tested into the fluorescent probe solution is calculated, and the avenate blight in the water can be detected.
9. The method for detecting oat rust in water according to claim 8, characterized in that: In the step 3), specifically, whether the fluorescence intensity at 493 nm decreases is observed. If so, it indicates that oat rust is contained therein; if not, it indicates that oat rust is not contained or the content of oat rust is below the detection limit; Or if you see with the naked eye that the color of the solution in the cuvette turns light yellow and quenches under ultraviolet light, it means that the test solution contains oat skewer. If the above phenomenon is not observed, it means that it does not contain oat skewer or the content of oat skewer is below the detection limit.
10. The method for detecting oat rust in water according to claim 9, characterized in that: The detection limit is determined by drawing a standard curve.