Glyphosate detection material as well as preparation method and application thereof

Abstract

The invention discloses a glyphosate detection material as well as a preparation method and application thereof, and solves the technical problems of high cost, complex operation and low efficiency in the prior art. The glyphosate detection material contains ZnO and Fe doped in a ZnO crystal lattice; diffraction peaks of Fe / ZnO are observed at the positions of 31.8 degrees, 34.4 degrees, 36.3 degrees, 47.6 degrees, 56.7 degrees, 62.9 degrees and 68 degrees in an XRD (X-Ray Diffraction) pattern; an FT-IR spectrum has absorption peaks at the positions of 3445 cm <-1 >, 1631 cm <-1 >, 1385 cm <-1 > and 620 cm <-1 >; an XPS (X-ray photoelectron spectroscopy) full spectrum has characteristic peaks at the positions of 288.6 eV, 530.4 eV, 723.9 eV, 710.7 eV, 1044.7 eV and 1021.6 eV. The preparation method comprises the following steps: dissolving soluble ferric salt and soluble zinc salt in an organic solvent to obtain a first reaction solution; adding terephthalic acid into the first reaction solution to obtain a second reaction solution; adding a morphology regulator into the second reaction solution to obtain a third reaction solution; performing high-pressure solvent heat treatment on the third reaction liquid to obtain a solid-liquid mixture; collecting, washing and drying precipitates in the solid-liquid mixture to obtain a precursor; and calcining the precursor in an air atmosphere to obtain the glyphosate detection material.

Description

Technical Field

[0001] The present invention relates to the technical field of glyphosate detection, and in particular to a glyphosate detection material and a preparation method and application thereof. Background Art

[0002] Glyphosate is a highly effective, broad-spectrum, non-selective herbicide that was originally considered environmentally friendly and widely produced and used for commercial purposes, making it one of the most consumed herbicides in the world. However, recent studies have pointed out that glyphosate may cause many human health risks, such as cancer and endocrine disruptors.

[0003] The accurate detection and identification of glyphosate is crucial for environmental monitoring. Currently, some analytical techniques have been developed for glyphosate detection, such as chromatography, electrochemical sensing and spectroscopy, but these methods have the disadvantages of high cost, complex operation and low efficiency. Summary of the invention

[0004] The main purpose of the present invention is to provide a glyphosate detection material and a preparation method and application thereof, so as to solve the technical problems of high cost, complex operation and low efficiency existing in the analysis technology in the prior art.

[0005] In order to achieve the above object, according to the first aspect of the present invention, a glyphosate detection material is provided, and the technical scheme is as follows:

[0006] Glyphosate detection material, containing ZnO and Fe doped in the ZnO lattice; XRD spectrum shows diffraction peaks of Fe / ZnO at 31.8°, 34.4°, 36.3°, 47.6°, 56.7°, 62.9° and 68°; FT-IR spectrum shows diffraction peaks at 3445cm -1 、1631cm -1 、1385cm -1 、620cm -1 There are absorption peaks at; the XPS full spectrum has characteristic peaks at 288.6eV, 530.4eV, 723.9eV, 710.7eV, 1044.7eV, and 1021.6eV.

[0007] As a further improvement of the above-mentioned glyphosate detection material: Zn, Fe, O and C are evenly distributed in the detection material.

[0008] As a further improvement of the above-mentioned glyphosate detection material: the high-resolution fine spectrum of Zn 2p has characteristic peaks at 1021.1eV and 1044.2eV; the high-resolution fine spectrum of Fe 2p has characteristic peaks at 710.5eV, 713.6eV, 717.3eV, 723.7eV, 726.4eV, and 730.0eV.

[0009] In order to achieve the above object, according to the second aspect of the present invention, a method for preparing the glyphosate detection material described in the first aspect is provided, and the technical scheme is as follows:

[0010] The preparation method of glyphosate detection material comprises the following steps:

[0011] dissolving a soluble iron salt and a soluble zinc salt in an organic solvent to obtain a first reaction solution;

[0012] adding terephthalic acid to the first reaction solution to obtain a second reaction solution;

[0013] adding a morphology regulator to the second reaction solution to obtain a third reaction solution;

[0014] performing high pressure solvent thermal treatment on the third reaction liquid to obtain a solid-liquid mixture;

[0015] collecting, washing, and drying the precipitate in the solid-liquid mixture to obtain a precursor;

[0016] The precursor is calcined in an air atmosphere to obtain a glyphosate detection material.

[0017] As a further improvement of the preparation method of the glyphosate detection material mentioned above: in the first reaction solution, Fe 3+ / (Zn 2+ +Fe 3+ ) has a molar percentage of 10% to 15%.

[0018] As a further improvement of the above-mentioned method for preparing the glyphosate detection material: the organic solvent comprises DMF and EtOH in a volume ratio of 2:1.

[0019] As a further improvement to the preparation method of the above-mentioned glyphosate detection material: the morphology regulator is triethylamine.

[0020] As a further improvement of the preparation method of the glyphosate detection material described above: the third reaction solution is added with 4.5 mmol of Fe per 30 mL of organic solvent. 3+ and Zn 2+ , 2mmol terephthalic acid and 5mL triethylamine.

[0021] As a further improvement of the preparation method of the above-mentioned glyphosate detection material: the calcination treatment is carried out at 450° C. for 2 hours.

[0022] In order to achieve the above object, according to the third aspect of the present invention, a method for detecting glyphosate is provided, and the technical scheme is as follows:

[0023] The method for detecting glyphosate comprises the following steps:

[0024] Adding the glyphosate detection material, oxidant, and color developer described in the first aspect to a solution to be tested containing glyphosate to obtain a mixed solution;

[0025] The absorbance of the mixed solution was tested, and then the glyphosate concentration in the test solution was converted based on the linear relationship between the absorbance and the glyphosate concentration.

[0026] The glyphosate detection material of the present invention and its preparation method and application have the beneficial effects of utilizing the high electronic conductivity and transparency of ZnO and Fe 3+ / Fe 2+ The enzyme-like activity of Fe 3+ and Fe 2+ By doping in the ZnO lattice, a detection material with adjustable specific surface area, special surface physicochemical properties and efficient catalytic activity was obtained, which can perform direct, specific and highly sensitive colorimetric detection of glyphosate. It has the advantages of low cost, simple operation and high detection efficiency. It can detect glyphosate in real water bodies and provides a simple strategy for the development of a high-performance pesticide detection platform.

[0027] The present invention is further described below in conjunction with the accompanying drawings and specific embodiments. Additional aspects and advantages of the present invention will be partially given in the following description, partially become apparent from the following description, or be learned through the practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] The drawings constituting a part of the present invention are used to assist in understanding the present invention. The contents provided in the drawings and their related descriptions in the present invention can be used to explain the present invention, but do not constitute improper limitations on the present invention. In the drawings:

[0029] Figure 1 For Fe / ZnO in Fe 3+ / (Zn 2+ +Fe 3+ ) at different molar percentages.

[0030] Figure 2 This is the relative activity diagram of Fe / ZnO at different TEA dosages.

[0031] Figure 3 This is the relative activity diagram of Fe / ZnO at different calcination temperatures.

[0032] Figure 4 This is the relative activity diagram of Fe / ZnO at different test pH.

[0033] Figure 5 This is the relative activity diagram of Fe / ZnO at different test temperatures.

[0034] Figure 6 UV-vis spectra of different chromogens oxidized by Fe / ZnO in the presence and absence of H2O2.

[0035] Figure 7 A under different test systems 652 Curve over time.

[0036] Figure 8 UV-vis spectra of Fe / ZnO / H2O2 / TMB system at different glyphosate concentrations.

[0037] Fig. 9 This is the linear relationship between the absorbance of the Fe / ZnO / H2O2 / TMB system and glyphosate concentration at different glyphosate concentrations.

[0038] Fig.10 This is the selectivity result diagram of glyphosate detection in Fe / ZnO / H2O2 / TMB system.

[0039] Fig.11 This is the anti-interference ability diagram of the Fe / ZnO / H2O2 / TMB system in detecting glyphosate.

[0040] Fig.12 SEM photos of the test materials obtained with different TEA dosages.

[0041] Fig.13 TEM images, HRTEM images and element mapping of Fe / ZnO.

[0042] Fig.14 XRD spectra of ZnO and Fe / ZnO.

[0043] Fig.15 This is a partial enlarged view of the XRD spectra of ZnO and Fe / ZnO.

[0044] Fig.16 FT-IR spectra of ZnO and Fe / ZnO.

[0045] Fig.17 This is the full XPS spectrum of Fe / ZnO.

[0046] Fig.18High-resolution fine spectrum of Zn 2p in Fe / ZnO.

[0047] Fig.19 High-resolution fine spectrum of Fe 2p in Fe / ZnO. DETAILED DESCRIPTION

[0048] The present invention is described clearly and completely below in conjunction with the accompanying drawings. A person skilled in the art will be able to implement the present invention based on these descriptions. Before describing the present invention in conjunction with the accompanying drawings, it should be particularly noted that:

[0049] The technical solutions and technical features provided in each part of the present invention, including the following description, may be combined with each other if there is no conflict.

[0050] In addition, the embodiments of the present invention involved in the following description are generally only a part of the embodiments of the present invention, rather than all the embodiments. Therefore, based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work should fall within the scope of protection of the present invention.

[0051] About the terms and units in the present invention: The terms "include", "have" and any variations thereof in the description and claims of the present invention and related parts are intended to cover non-exclusive inclusions.

[0052] The specific implementation method of the preparation method of the glyphosate detection material of the present invention comprises the following steps:

[0053] (1) Dissolving a soluble iron salt and a soluble zinc salt in an organic solvent to obtain a first reaction solution; wherein the soluble iron salt is Fe(NO)3·9H2O, and the soluble zinc salt is Zn(NO3)3·6H2O; the organic solvent is composed of DMF (N,N-dimethylformamide) and EtOH (anhydrous ethanol) in a volume ratio of 2:1, with a total volume of 30 mL; the first reaction solution is a clear light yellow solution, and Fe 3+ and Zn 2+ The total molar amount is 4.5 mmol.

[0054] (2) 2 mmol of terephthalic acid was added to the first reaction solution to obtain a second reaction solution.

[0055] (3) Triethylamine (TEA) is added dropwise to the second reaction solution, and after the addition is completed, ultrasonic treatment is performed to obtain a third reaction solution.

[0056] (4) The third reaction liquid was charged into a polytetrafluoroethylene reaction kettle and kept at 120° C. for 10 h to obtain a solid-liquid mixture.

[0057] (5) collecting, washing, and drying the precipitate in the solid-liquid mixture to obtain a precursor; wherein the precipitate is collected by centrifugal separation, the precipitate is washed three times with DMF and EtOH respectively, and then dried under vacuum at 60°C.

[0058] (6) The precursor is calcined in an air atmosphere to obtain a glyphosate detection material, which is represented by Fe / ZnO.

[0059] In the above preparation method, TEA as a morphology regulator can not only inhibit the growth of 3D structure, but also act as a proton remover to promote M n+ (Zn 2+ , Fe 3+ ) and terephthalic acid, therefore, in order to verify the beneficial effect of triethylamine, the test material obtained by the preparation process without triethylamine is represented as Fe / ZnO-w. At the same time, in order to explore the effect of Fe doping on the catalytic performance of the test material, the material without Fe(NO)3·9H2O is represented as ZnO.

[0060] The specific implementation of the method for detecting glyphosate of the present invention comprises the following steps:

[0061] (1) Add the above-mentioned Fe / ZnO, oxidant and color developer to a test solution containing glyphosate to obtain a mixed solution; wherein the oxidant is H2O2 and the color developer is TMB (3,3',5,5'-tetramethylbenzidine).

[0062] (2) The absorbance of the mixed solution is tested, and then the glyphosate concentration in the test solution is calculated based on the linear relationship between the absorbance and the glyphosate concentration.

[0063] The beneficial effects of the present invention are illustrated below by means of experimental data and characterization data.

[0064] In order to obtain the best test results for Fe / ZnO and its absorbance detection conditions, multiple parallel tests were conducted, using relative activity as an evaluation index. 3+ The relative activity refers to the absorbance of the test solution at 652 nm (expressed as A 652 ) and the percentage of the maximum absorbance value. The test solution was prepared by sequentially adding Fe / ZnO (50 μL, 1 mg / mL), H2O2 (50 μL, 10 mM), and TMB (100 μL, 10 mM) to HAc-NaAc buffer solution (pH = 3.5, 4.8 mL, 0.2 M) and incubating for 15 minutes. The absorbance was measured using a USB4000 spectrophotometer from Ocean Optics, Inc., USA.

[0065] Figure 1 For Fe / ZnO in Fe 3+ / (Zn 2+ +Fe 3+ ) at different molar percentages. Figure 2 This is the relative activity diagram of Fe / ZnO at different TEA dosages. Figure 3 This is the relative activity diagram of Fe / ZnO at different calcination temperatures. Figure 4 This is the relative activity diagram of Fe / ZnO at different test pH. Figure 5 This is the relative activity diagram of Fe / ZnO at different test temperatures.

[0066] like Figure 1 As shown, when Fe 3+ / (Zn 2+ +Fe 3+ ) molar percentage ≤10%, the catalytic activity of Fe / ZnO increases with Fe 3+ The dosage increases; when Fe 3+ / (Zn 2+ +Fe 3+ ) continued to increase to 15%, the catalytic activity of Fe / ZnO remained almost unchanged; however, 3+ / (Zn 2+ +Fe 3+ ) continued to increase, resulting in a decrease in relative activity, indicating that excessive addition of Fe 3+ This will lead to a decrease in the catalytic activity of Fe / ZnO. Figure 2 As shown in Figure 2, the Fe / ZnO obtained with 5 mL TEA showed the best activity, and excessive TEA led to a decrease in catalytic activity. Figure 3 As shown in Figure 2, Fe / ZnO exhibits the best catalytic activity at a calcination temperature of 450°C, and too high a calcination temperature will lead to a decrease in catalytic activity. Figure 4-5 As shown in Figure 2, the highest catalytic activity of Fe / ZnO was observed at pH 3.5 and 40 °C. 3+ The amount of Fe / ZnO, TEA amount, calcination temperature, test pH and test temperature all significantly affect the catalytic activity of Fe / ZnO. Therefore, when not otherwise specified, the subsequent test data and characterization data are all carried out under the optimal parameters, that is, the third reaction solution is added with 4.5 mmol of Fe / ZnO per 30 mL of organic solvent. 3+ and Zn 2+ , 2mmol terephthalic acid and 5mL triethylamine were prepared. 3+ / (Zn 2+ +Fe 3+ ) has a molar percentage of 10%.

[0067] Then the effects of the types of color developers and whether H2O2, Fe(NO)3·9H2O, and TEA were used on the absorbance of the detection material were investigated.

[0068] Figure 6 UV-vis spectra of different chromogens oxidized by Fe / ZnO in the presence and absence of H2O2. Figure 7 A under different test systems 652 Curve over time.

[0069] like Figure 6 As shown, with TMB, ABTS (2,2'-hydrazine-bis(3-ethylbenzothiazoline-6-sulfonic acid) diamine salt) and OPD (o-phenylenediamine) as chromogenic substrates, when H2O2 is present, Fe / ZnO catalyzes H2O2 to oxidize TMB, ABTS, and OPD, all of which produce characteristic absorption, but TMB is the most sensitive color developer. When H2O2 is absent, the color development of the color developer is not obvious, indicating that Fe / ZnO has excellent catalytic activity for H2O2.

[0070] like Figure 7 As shown, the catalytic activity of Fe / ZnO is 15.3 times and 7.5 times that of ZnO and Fe / ZnO-w, respectively, indicating that the doping of Fe and the use of TEA play a crucial role in the catalytic activity of Fe / ZnO.

[0071] Then, by adjusting the concentration of glyphosate, a linear relationship between the absorbance of the Fe / ZnO / H2O2 / TMB system and the glyphosate concentration was obtained. The test solution was prepared by sequentially adding Fe / ZnO (50 μL, 1 mg / mL), glyphosate (100 μL, 0-40 mg / L), H2O2 (50 μL, 10 mM), and TMB (100 μL, 10 mM) to a HAc-NaAc buffer solution (pH=3.5, 4.7 mL, 0.2 M).

[0072] Figure 8 UV-vis spectra of Fe / ZnO / H2O2 / TMB system at different glyphosate concentrations. Fig. 9 This is the linear relationship between the absorbance of the Fe / ZnO / H2O2 / TMB system and glyphosate concentration at different glyphosate concentrations.

[0073] like Figure 8 As shown, after adding glyphosate, A 652 It gradually decreases, indicating that glyphosate inhibits the catalytic activity of Fe / ZnO, and the inhibition increases proportionally with the increase of glyphosate concentration. Fig. 9 As shown, the glyphosate concentration and the inhibitory absorbance at 652 nm (expressed as ΔA 652, defined as the A before and after adding glyphosate to the Fe / ZnO / H2O2 / TMB system 652 There is a good linear relationship between the difference between the two values, and the linear regression equation obtained by fitting is y=0.062x+0.058(R 2 =0.9963), y is ΔA 652 , x is the glyphosate concentration in the test solution, and x is 0.02-10 mg / L. The calculated detection limit is 0.0156 mg / L, which is much lower than the maximum contaminant level of glyphosate in drinking water set by the U.S. Environmental Protection Agency, which is 0.7 ppm (i.e. 0.7 mg / L).

[0074] Then the selectivity and anti-interference ability of the Fe / ZnO / H2O2 / TMB system in detecting glyphosate were tested.

[0075] Fig.10 This is the selectivity result diagram of glyphosate detection in Fe / ZnO / H2O2 / TMB system. Fig.11 This is the anti-interference ability diagram of the Fe / ZnO / H2O2 / TMB system in detecting glyphosate.

[0076] like Fig.10 As shown in the figure, among glyphosate, malathion, dichlorvos, chlorpyrifos, methyl parathion, phoxim, acetamiprid, methomyl and carbendazim, the Fe / ZnO / H2O2 / TMB system can selectively recognize glyphosate. Fig.11 As shown in the figure, when the test solution contains 1mM of various interfering ions (K + , Ca 2+ 、Na + Mg 2+ 、Zn 2+ 、SO4 2- , Cl - 、HCO3 - ) and glyphosate, the ΔA of the Fe / ZnO / H2O2 / TMB system 652 No obvious changes occurred, indicating that the Fe / ZnO / H2O2 / TMB system has strong anti-interference ability in detecting glyphosate.

[0077] Then the practicality of the Fe / ZnO / H2O2 / TMB system for detecting glyphosate was tested.

[0078] The standard addition method was used to detect the glyphosate level in tap water, lake water and farmland water. After pre-treating the actual water sample with a 0.22 μm filter membrane, glyphosate with accurate concentration was added to the water sample, and the glyphosate concentration and recovery rate were calculated according to the above calibration curve. As shown in Table 1, the glyphosate measured in the water sample was in good agreement with the spiked value, and the recovery rate was 91.8-106.5%. The results show that the Fe / ZnO / H2O2 / TMB system of the present invention also has good accuracy in colorimetric detection of glyphosate concentration in actual water samples.

[0079] Table 1

[0080]

[0081] Then, ZnO, Fe / ZnO, and Fe / ZnO-w were characterized to explore the effects of Fe doping and TEA use on the microstructure of the detection materials.

[0082] Fig.12 The SEM images of the test materials obtained with different TEA dosages are shown in Figure 2. Among them, ac used no TEA (i.e., Fe / ZnO-w), df used 2 mL TEA, and gi used 5 mL TEA.

[0083] like Fig.12 As shown in the figure, without the addition of TEA, Fe / ZnO-w presents a 3D cubic structure with an average particle size of about 23μm. When the amount of TEA is 2mL, Fe / ZnO transforms from 3D cubes to hexagonal flakes with a reduced size (length L≈13μm, width W≈1.6μm). Further increasing the amount of TEA to 5mL leads to a further reduction in the size of Fe / ZnO (W≈4.7μm, L≈9.4μm). It can be seen that TEA, as a morphology regulator, can inhibit the growth of 3D structures.

[0084] Table 2 shows the specific surface area and pore volume of the test materials obtained with different TEA dosages. It can be seen from Table 2 that as the TEA dosage increases from 0 to 5 mL, the BET surface area of ​​Fe / ZnO expands to 93.1 m 2 / g.

[0085] Table 2

[0086] TEA dosage (mL) <![CDATA[Specific surface area (m 2 / g)]]> <![CDATA[Pore volume (cm 3 / g)]]> 0 44.6 0.24 2 51.0 0.25 5 93.1 0.42

[0087] Fig.13 TEM images, HRTEM images and element mapping of Fe / ZnO.

[0088] HRTEM photos ( Fig.13b) clearly shows the lattice spacing of 0.261 nm, which is consistent with the (102) plane of ZnO (PDF#05-0664). Elemental mapping ( Fig.13 df) show that Zn, Fe, O and C are uniformly distributed in Fe / ZnO, indicating that Fe is uniformly doped into the ZnO lattice.

[0089] Fig.14 XRD spectra of ZnO and Fe / ZnO. Fig.15 This is a partial enlarged view of the XRD spectra of ZnO and Fe / ZnO.

[0090] like Fig.14 As shown in Figure 2, the diffraction peaks of Fe / ZnO were observed at 2θ=31.8°, 34.4°, 36.3°, 47.6°, 56.7°, 62.9° and 68°, which matched the diffraction peak positions of ZnO and PDF#05-0664, indicating that Fe doping did not significantly change the phase structure. Compared with ZnO, the decrease in the diffraction peak intensity of Fe / ZnO may be due to the reduction in particle size. Fig.15 As shown in the figure, under the local magnification of 2θ=30°~40°, it can be seen that Fe doping causes the diffraction peak position of Fe / ZnO to shift to a higher angle, which means that Fe is effectively incorporated into the ZnO lattice. No carbon diffraction peak appears, indicating that carbon exists in an amorphous structure.

[0091] Fig.16 FT-IR spectra of ZnO and Fe / ZnO.

[0092] like Fig.16 As shown in Figure 2, Fe / ZnO and ZnO have very similar FT-IR spectra, where 3445 cm -1 The broad absorption band at 1631 cm is attributed to the stretching vibration of the OH bond and M-OH bond of water molecules adsorbed on the surface of the detection material. -1 The absorption peak at 1385 cm is attributed to the stretching vibration of the C-OH bond and C=O in the -COOH group. -1 The absorption peak at is attributed to COO - Stretching vibration, 455cm -1 The band at 620 cm corresponds to the stretching vibration of the Zn-O bond. These results indicate that the Fe / ZnO surface is rich in -COOH groups and -C=O groups, which serve as potential binding sites for H2O2 and catalytic sites for H2O2 decomposition, respectively. -1 A new broad absorption peak appears at , which can be attributed to the stretching vibration of the Fe-O bond, confirming that Fe is successfully incorporated into the structure.

[0093] Fig.17This is the full XPS spectrum of Fe / ZnO. Fig.18 High-resolution fine spectrum of Zn 2p in Fe / ZnO. Fig.19 High-resolution fine spectrum of Fe 2p in Fe / ZnO.

[0094] like Fig.17 As shown in the full XPS spectrum of Fe / ZnO, the binding energies at 288.6eV, 530.4eV, 723.9(710.7)eV and 1044.7(1021.6)eV are the characteristic peaks of C1s, O 1s, Fe 2p and Zn 2p, respectively. Fig.18 As shown, the high-resolution spectrum of Zn 2p shows that 1021.1eV (Zn 2p 3 / 2 ) and 1044.2eV(Zn 2p 1 / 2 ) binding energy; 2p 1 / 2 and 2p 3 / 2 The binding energy difference between them is 23.1 eV, indicating the presence of Zn 2+ Ions. Fig.19 As shown in the high-resolution spectrum of Fe 2p, Fe 2+ The peak value is at 710.5eV (Fe 2p 3 / 2 ) and 723.7 eV (Fe 2p 1 / 2 ), Fe 3+ The peak value is at 713.6eV (Fe 2p 3 / 2 ) and 726.4 eV (Fe 2p 1 / 2 ), indicating the presence of Fe in the Fe / ZnO catalyst; the satellite peaks I at 717.3 eV and II at 730.0 eV are attributed to Fe 3+ Species.

[0095] The equipment used for the above characterization is: field emission electron scanning microscope (JSM 7800F Prime, JEOL Ltd.), transmission electron microscope (JEOL JEM-F 200 (HR), JEOL Ltd.), X-ray diffractometer (MiniFlex600, Rigaku Corporation), X-ray photoelectron spectrometer (Thermo Scientific K-Alpha, Thermo Fisher Scientific Inc.), infrared spectrometer (Specturm 2, PerkinElmer Instrument Co., Ltd.).

[0096] The above is a description of the relevant contents of the present invention. A person skilled in the art will be able to implement the present invention based on these descriptions. Based on the above contents of the present invention, all other embodiments obtained by a person skilled in the art without creative work shall fall within the scope of protection of the present invention.

Claims

1. Glyphosate detection material, characterized in that: Contains ZnO and Fe doped in the ZnO lattice; XRD spectrum shows diffraction peaks of Fe / ZnO at 31.8°, 34.4°, 36.3°, 47.6°, 56.7°, 62.9° and 68°; FT-IR spectrum shows diffraction peaks at 3445cm -1 、1631cm -1 、1385cm -1 、620cm -1 There are absorption peaks at; the XPS full spectrum has characteristic peaks at 288.6eV, 530.4eV, 723.9eV, 710.7eV, 1044.7eV, and 1021.6eV.

2. The glyphosate detection material according to claim 1, characterized in that: Zn, Fe, O and C are evenly distributed in the test material.

3. The glyphosate detection material according to claim 1, characterized in that: The high-resolution fine spectrum of Zn 2p has characteristic peaks at 1021.1 eV and 1044.2 eV; the high-resolution fine spectrum of Fe 2p has characteristic peaks at 710.5 eV, 713.6 eV, 717.3 eV, 723.7 eV, 726.4 eV, and 730.0 eV.

4. The method for preparing the glyphosate detection material according to any one of claims 1 to 3, characterized in that: The following steps are involved: dissolving a soluble iron salt and a soluble zinc salt in an organic solvent to obtain a first reaction solution; adding terephthalic acid to the first reaction solution to obtain a second reaction solution; adding a morphology regulator to the second reaction solution to obtain a third reaction solution; performing high pressure solvent thermal treatment on the third reaction liquid to obtain a solid-liquid mixture; collecting, washing, and drying the precipitate in the solid-liquid mixture to obtain a precursor; The precursor is calcined in an air atmosphere to obtain a glyphosate detection material.

5. The method for preparing the glyphosate detection material according to claim 4, characterized in that: In the first reaction solution, Fe 3+ / (Zn 2+ +Fe 3+ ) has a molar percentage of 10% to 15%.

6. The method for preparing the glyphosate detection material according to claim 4, characterized in that: The organic solvent includes DMF and EtOH in a volume ratio of 2:

1.

7. The method for preparing the glyphosate detection material according to claim 4, characterized in that: The morphology regulator is triethylamine.

8. The method for preparing the glyphosate detection material according to claim 7, characterized in that: The third reaction solution was added with 4.5 mmol of Fe per 30 mL of organic solvent. 3+ and Zn 2+ , 2mmol terephthalic acid and 5mL triethylamine.

9. The method for preparing the glyphosate detection material according to claim 4, characterized in that: The calcination treatment is carried out at 450° C. for 2 hours.

10. A method for detecting glyphosate, characterized in that: The following steps are involved: Adding the glyphosate detection material, oxidant and developer according to any one of claims 1 to 3 into a solution to be tested containing glyphosate to obtain a mixed solution; The absorbance of the mixed solution is tested, and then the glyphosate concentration in the test solution is converted based on the linear relationship between the absorbance and the glyphosate concentration.

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