CN111044510A - A method for anti-etching-aggregation colorimetric detection of Fume series fungicides based on silver nano-triangles - Google Patents
A method for anti-etching-aggregation colorimetric detection of Fume series fungicides based on silver nano-triangles Download PDFInfo
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Abstract
本发明公开了一种基于银纳米三角片的抗刻蚀‑聚集比色检测福美系列杀菌剂的方法，对于一般溶液体系，检测时，将不同量的福美系列杀菌剂加入银纳米三角片溶液中，并加入卤素离子，反应一段时间，将溶液颜色与标准色板对比，得到福美系列杀菌剂的浓度；对于土壤体系，检测时，将土壤中的福美系列杀菌剂洗脱出来，除去溶液中带正电荷的分子，然后加入到银纳米三角片溶液中，并加入卤素离子，反应一段时间，将溶液颜色与标准色板进行对比，得到土壤中福美系列杀菌剂残留量。本发明不仅适用于简单溶液体系，而且能够进行土壤福美系列杀菌剂残留检测，充分扩大比色检测的范围，丰富比色检测的色彩，检测灵敏度高、检测范围广、操作简便且成本低。
The invention discloses a method for anti-etching-aggregation colorimetric detection of Fume series bactericides based on silver nano-triangular sheets. For a general solution system, different amounts of Fume series bactericides are added to the silver nano-triangle sheet solution during detection. , and add halide ions, react for a period of time, compare the color of the solution with the standard swatch, and obtain the concentration of Fume series fungicides; for soil systems, when testing, the Fume series fungicides in the soil are eluted out, and the residues in the solution are removed. Positively charged molecules are then added to the silver nano-triangle plate solution, and halide ions are added to react for a period of time, and the color of the solution is compared with the standard color plate to obtain the residual amount of Fumei series fungicides in the soil. The invention is not only suitable for a simple solution system, but also can carry out the residual detection of soil fumei series fungicides, fully expands the range of colorimetric detection, enriches the colors of colorimetric detection, has high detection sensitivity, wide detection range, simple operation and low cost.
Description
Technical Field
The invention belongs to the technical field of detection of thiram series bactericides, and particularly relates to an anti-etching-aggregation colorimetric detection method of thiram series bactericides based on silver nano triangular plates.
Background
The thiram series bactericides have serious harm to health and environment, particularly residue in soil, and the traditional method is difficult to realize quick and accurate detection due to complex soil components. With the development of nanotechnology, precious metal nanoparticles with unique Localized Surface Plasmon Resonance (LSPR) characteristics are gradually used in pesticide detection, mainly including Surface-enhanced Raman scattering (SERS) and colorimetric methods. Because the SERS method needs to depend on a large-scale detection instrument, the cost is high, the portability is poor, and the detection result is spectral data which is not visual enough, the popularization of the method in practical detection application is limited.
The colorimetric method based on the noble metal nanoparticles can realize detection through color change of a reaction solution, and the method can judge the concentration of an object to be detected only by naked eyes without any instrument. At present, some reports utilize a noble metal nanoparticle colorimetric method to detect thiram residues, but the methods can only change the shade of the solution color, so that the defects of single solution color, small change amplitude, low resolution and the like exist, and the method can only be applied to water, plant seeds and the like generally and cannot be applied to soil.
Disclosure of Invention
The invention aims to provide a method for colorimetric detection of thiram series bactericide residues, which has the advantages of high sensitivity, rich colors, wide detection range, simplicity, rapidness and low cost.
In order to achieve the purpose, the technical scheme of the invention comprises the following steps:
1. dissolving the standard thiram series bactericide by using a dissolving agent, adding the dissolved standard thiram series bactericide into a silver nano triangular plate solution, adding ultrapure water for constant volume, and preparing standard solutions of thiram series bactericides with different concentrations; wherein the dissolving agent is any one of chloroform, acetone and dimethylformamide.
2. And (3) adding a halogen ion aqueous solution into the standard solution prepared in the step (1), mixing, standing for 5-10 minutes, observing the color of the solution, and making a standard colorimetric card of the concentration and the color of the thiram series bactericide in the standard solution.
3. Adding a sample solution to be detected into a silver nano triangular plate solution, adding ultrapure water to a constant volume, then adding a halogen ion aqueous solution, mixing, standing for 5-10 minutes, observing the color of the solution, and comparing the color of the solution with a standard colorimetric card of the concentration and the color of the thiram series bactericide in a standard solution to determine the concentration of the thiram series bactericide in the sample solution to be detected.
When the sample to be detected is a soil sample, in the step 1, adding a thiram series bactericide standard into the soil sample without thiram series bactericides, adding a dissolving agent after the soil sample is naturally dried, stirring for 5-10 minutes, performing centrifugal separation, adding a charge shielding agent into the obtained supernatant, uniformly mixing, adding into a silver nano triangular plate solution, adding ultrapure water to a constant volume, and preparing into standard solutions of thiram series bactericides with different concentrations; and 3, adding the soil sample to be detected into a dissolving agent, stirring for 5-10 minutes, performing centrifugal separation, adding a charge shielding agent into the supernatant, uniformly mixing, adding the mixture into a silver nano triangular plate solution, adding ultrapure water to a constant volume, adding a halogen ion aqueous solution, mixing, standing for 5-10 minutes, observing the color of the solution, and comparing the color with a standard colorimetric card of the concentration and the color of the thiram series bactericide in the standard solution to determine the content of the thiram series bactericide in the soil sample to be detected.
In the detection method, the LSPR peak of the silver triangular nanosheet is located between 450 nm and 760 nm.
In the detection method, the thiram series bactericides comprise thiram, thiram arsenic, thiram zinc and the like.
In the detection method, the halogen ion aqueous solution is 0.1mM KBr aqueous solution or 0.1mM KI aqueous solution, and the volume ratio of the halogen ion aqueous solution to the silver nano triangular plate solution is 1: 2.
In the detection method, the charge shielding agent is sodium polyacrylate.
The invention has the following beneficial effects:
the silver nano triangular plate adopted by the invention has unique sharp corners and a sheet-shaped structure, and the change of the shape, the size and the dispersion state of the silver nano triangular plate can cause the LSPR spectrum and the solution color to be greatly changed, so that the silver nano triangular plate is very suitable for colorimetric detection. Therefore, the invention utilizes a proper amount of thiram series bactericides to promote the silver nanometer triangular plate to resist the etching of halogen ions, and realizes the anti-etching colorimetric detection; and the high-content thiram series bactericides cause the silver nano triangular plates to be aggregated, so that the aggregation colorimetric detection is realized. The invention combines the anti-etching colorimetric method and the aggregation colorimetric method by utilizing the anti-halogen ion etching effect and the aggregation effect of the Fumei series bactericide on the silver triangular nanoplatelets, so as to obtain the detection method of the Fumei series bactericide, which has the advantages of high sensitivity, rich colors, wide detection range, simplicity, convenience, rapidness and low cost. .
Drawings
FIG. 1 is a digital photograph of colorimetric detection of thiram with different concentrations by silver nano triangular plate with LSPR peak at 550 nm.
FIG. 2 is a spectrum diagram of colorimetric detection of thiram with different concentrations by silver nanometer triangular plate with LSPR peak at 550 nm.
FIG. 3 is a digital photograph of different concentrations of thiram detected by silver nanoprism with LSPR peak at 600 nm.
FIG. 4 is a spectrum diagram of silver nano triangular plate with LSPR peak at 600nm for colorimetric detection of thiram with different concentrations.
FIG. 5 is a digital photograph of different concentrations of thiram detected by silver nanoprism with LSPR peak at 650 nm.
FIG. 6 is a spectrum diagram of colorimetric detection of thiram with different concentrations by silver nano triangular plate with LSPR peak at 650 nm.
FIG. 7 is a digital photograph of colorimetric detection of thiram with different concentrations by silver nanoprisms with LSPR peak at 700 nm.
FIG. 8 is a spectrum diagram of colorimetric detection of thiram with different concentrations by silver nanometer triangular plate with LSPR peak at 700 nm.
Fig. 9 is a digital photograph of colorimetric detection of thiram residue in soil using silver nanoprisms.
FIG. 10 is a spectrum diagram of the colorimetric detection of thiram residue in soil using silver nanoprisms.
Detailed Description
The invention will be further described in detail with reference to the following figures and examples, but the scope of the invention is not limited to these examples.
The Silver nanoplatelets solutions in the following examples were prepared according to the method disclosed in the literature "Zhang CH, Zhu J, Li JJ, ethyl.small and Sharp Triangular Silver Nanoplates Synthesized using tilling tringular nucleic acid and heat Excellent SERS Activity for Selective detection of third material resource in Soil [ J ]. ACS Applied Materials & Interfaces,2017,9(20): 17387-.
Example 1
1.1 mL of silver nanopyramid solution with the LSPR peak at 550nm (the average side length of the silver nanopyramid is 29nm) is taken, thiram chloroform solution is added into the solution, the volume is adjusted to 1.5mL by ultrapure water, and thiram standard solutions with final concentrations of 0, 0.075, 0.15, 0.25, 0.5, 0.75, 0.85, 1.0, 1.1 and 1.25 MuM are respectively prepared.
2. Adding 500 mu L of 0.1mM KBr aqueous solution into the standard solution prepared in the step 1 respectively, mixing, standing for 10 minutes, observing and recording the color change of the solution, measuring the absorption spectrum of the solution after reaction, and making a standard colorimetric card of the concentration and the color of thiram in the standard solution, wherein the result is shown in figure 1. As can be seen from fig. 1, when the concentration of thiram is low, the silver nanoprisms are etched, so that the solution appears orange yellow; with the gradual increase of the concentration of thiram, the function of the thiram for promoting the silver nano triangular plate to resist the bromine ion etching is gradually enhanced, so that the etching degree is reduced, and the color of the solution is gradually deepened to be brownish red; as the concentration of thiram continues to increase, silver nano triangular plates are aggregated, and the solution is grayish white. Fig. 2 is a graph of the corresponding absorption spectrum of the sample of fig. 1, which verifies the change of the silver nanoprisms from being etched to resistant to etching to aggregation as the concentration of thiram increases.
3. And (3) adding 200 mu L of thiram sample solution to be detected into 1mL of silver nano triangular plate solution with the LSPR peak at 550nm, adding ultrapure water to a constant volume of 1.5mL, adding 500 mu L of 0.1mM KBr aqueous solution, mixing, standing for 10 minutes, observing the color of the solution, and comparing the color with the standard colorimetric card of the thiram concentration and the color in the standard solution prepared in the step (2) to determine the concentration of the thiram in the sample solution to be detected.
In this example, thiram was detected in the range of 0.15. mu.M to 1.25. mu.M.
Example 2
1.1 mL of silver nanopyramid solution with the LSPR peak positioned at 600nm (the average side length of the silver nanopyramid is 46nm) is taken, acetone solution of thiram is added into the solution, the volume is adjusted to 1.5mL by ultrapure water, and thiram standard solutions with final concentrations of 0, 0.075, 0.15, 0.25, 0.5, 0.75, 0.85, 1.0, 1.1 and 1.25 MuM are respectively prepared.
2. Adding 500 mu L of 0.1mM KBr aqueous solution into the standard solution prepared in the step 1, mixing, standing for 10 minutes, observing and recording the color change of the solution, measuring the absorption spectrum of the solution after reaction, and making a standard colorimetric card of the concentration and the color of thiram in the standard solution, wherein the result is shown in figure 3. As can be seen from fig. 3, when the concentration of thiram is low, the silver nanoprisms are etched, so that the solution appears orange-yellow; with the gradual increase of the concentration of thiram, the role of the thiram in promoting the silver nano triangular plate to resist the bromine ion etching is gradually enhanced, so that the etching degree is reduced, and the color of the solution is gradually deepened into brownish red, purple and blue; as the concentration of thiram continues to increase, silver nanoplatelets aggregate and the solution appears bluish-grey to off-white. Fig. 4 is a corresponding absorption spectrum of the sample of fig. 3, which verifies that the silver nano triangular plate changes from being etched to resisting etching to being aggregated with the increase of thiram concentration.
3. And (3) adding 200 mu L of thiram sample solution to be detected into 1mL of silver nano triangular plate solution with the LSPR peak at 550nm, adding ultrapure water to a constant volume of 1.5mL, adding 500 mu L of 0.1mM KBr aqueous solution, mixing, standing for 10 minutes, observing the color of the solution, and comparing the color with the standard colorimetric card of the thiram concentration and the color in the standard solution prepared in the step (2) to determine the concentration of the thiram in the sample solution to be detected.
In this example, thiram was detected in the range of 0.075. mu.M to 1.25. mu.M.
Example 3
1. Taking 1mL of silver nano triangular plate solution with an LSPR peak at 650nm (the average side length of the silver nano triangular plate is 55nm), adding thiram dimethylformamide solution, and using ultrapure water to make the volume reach 1.5mL, and respectively preparing thiram standard solutions with final concentrations of 0, 0.075, 0.15, 0.25, 0.5, 0.75, 0.85, 1.0, 1.1 and 1.25 MuM.
2. Adding 500 mu L of 0.1mM KI aqueous solution into the standard solution prepared in the step 1, mixing, standing for 10 minutes, observing and recording the color change of the solution, measuring the absorption spectrum of the solution after reaction, and making a standard colorimetric card of the concentration and the color of the thiram in the standard solution, wherein the result is shown in figure 5. As can be seen from fig. 5, when the concentration of thiram is low, the silver nano triangular plate is etched, so that the solution appears orange; with the gradual increase of the concentration of thiram, the effect of the thiram on promoting the silver nano triangular plate to resist the etching of iodide ions is gradually enhanced, so that the etching degree is reduced, and the color of the solution is gradually deepened into brownish red, purple and blue; as the concentration of thiram continues to increase, silver nanoplatelets aggregate and the solution appears bluish-grey to off-white. Fig. 6 is a graph of the corresponding absorption spectrum of the sample of fig. 5, which verifies the change of the silver nanoprisms from etched to etch-resistant to aggregation as the concentration of thiram increases.
3. And (2) adding 200 mu L of thiram sample solution to be detected into silver nano triangular plate solution with the peak of 1mLLSPR positioned at 550nm, adding ultrapure water to a constant volume of 1.5mL, then adding 500 mu L0.1mM KI aqueous solution, mixing, standing for 10 minutes, observing the color of the solution, and comparing the color of the solution with the standard colorimetric card of the thiram concentration and the color in the standard solution prepared in the step 2 to determine the concentration of the thiram in the sample solution to be detected.
In this example, thiram was detected in the range of 0.075. mu.M to 0.75. mu.M.
Example 4
1. Taking 1mL of silver nano triangular plate solution with an LSPR peak at 700nm (the average side length of the silver nano triangular plate is 70nm), adding thiram acetone solution into the silver nano triangular plate solution, and using ultrapure water to fix the volume to 1.5mL to prepare thiram standard solutions with final concentrations of 0, 0.075, 0.15, 0.25, 0.5, 0.75, 0.85, 1.0, 1.1 and 1.25 mu M respectively.
2. Adding 500 mu L of 0.1mM KI aqueous solution into the standard solution prepared in the step 1, mixing, standing for 10 minutes, observing and recording the color change of the solution, measuring the absorption spectrum of the solution after reaction, and making a standard colorimetric card of the concentration and the color of the thiram in the standard solution, wherein the result is shown in figure 7. As can be seen from fig. 7, when the thiram concentration is low, the silver nanoprisms are etched, so that the solution appears orange; with the gradual increase of the concentration of thiram, the effect of the thiram on promoting the silver nano triangular plate to resist the etching of iodide ions is gradually enhanced, so that the etching degree is reduced, and the color of the solution is gradually deepened into brownish red, purple and blue; as the concentration of thiram continues to increase, silver nanoplatelets aggregate and the solution appears bluish-grey to off-white. Fig. 8 is a corresponding absorption spectrum of the sample of fig. 7, which verifies that the silver nano-triangular plate changes from being etched to resisting etching to being aggregated with the increase of thiram concentration.
3. And (3) adding 200 mu L of thiram sample solution to be detected into 1mL of silver nano triangular plate solution with the LSPR peak at 550nm, adding ultrapure water to a constant volume of 1.5mL, adding 500 mu L0.1mM of KI aqueous solution, mixing, standing for 10 minutes, observing the color of the solution, and comparing the color of the solution with the standard colorimetric card of the thiram concentration and the color in the standard solution prepared in the step (2) to determine the concentration of the thiram in the sample solution to be detected.
In this example, thiram was detected in the range of 0.075. mu.M to 0.5. mu.M.
Example 5
1. A soil sample (1 g) is weighed, the soil is filtered, and centrifugal cleaning is carried out by using water so that the soil does not contain Fumei series bactericides. Adding thiram into 1g of soil sample without thiram series bactericides, and naturally drying to ensure that the final contents of thiram in the soil sample are respectively 0, 0.8, 1, 2, 4, 6, 8, 10 and 12 mu g/g; then adding 1mL of acetone, stirring for 10 minutes, obtaining a supernatant through centrifugal separation, adding 10 mu L of 10mM sodium polyacrylate aqueous solution into the supernatant, uniformly mixing, and mixing 100 mu L of silver nano triangular plate solution (the average side length of the silver nano triangular plate is 46nm) with 900 mu L of LSPR peak positioned at 600nm to prepare thiram standard solutions with different concentrations.
2. Adding 500 mu L of 0.1mM KI aqueous solution into the standard solution prepared in the step 1, mixing, standing for 10 minutes, observing and recording the color change of the solution, measuring the absorption spectrum of the solution after reaction, and making a standard colorimetric card of the concentration and the color of thiram in the standard solution, wherein the result is shown in figure 9. As can be seen from fig. 9, when the thiram concentration is low, the silver nanoprisms are etched, so that the solution appears orange; with the gradual increase of the concentration of thiram, the effect of the thiram on promoting the silver nano triangular plate to resist the etching of iodide ions is gradually enhanced, so that the etching degree is reduced, and the color of the solution is gradually deepened into red, purple and blue; as the concentration of thiram continues to increase, silver nano triangular plates are aggregated, and the solution is grayish white. Fig. 10 is a graph of the corresponding absorption spectrum of the sample of fig. 9, which demonstrates the change of the silver nanoprisms from etched to etch resistant to aggregation as the concentration of thiram increases.
3. Adding 1g of soil sample to be detected into 1mL of acetone, stirring for 10 minutes, performing centrifugal separation, adding 10 mu L of 10mM sodium polyacrylate aqueous solution into the supernatant, uniformly mixing, mixing 100 mu L of the mixture with 900 mu L of silver nano triangular plate solution (the average side length of the silver nano triangular plate is 46nm) with the LSPR peak positioned at 600nm, then adding 500 mu L of 0.1mM KI aqueous solution, mixing, standing for 10 minutes, observing the color of the solution, comparing the concentration of thiram in the standard solution prepared in the step 2 with the standard colorimetric card of the color, and determining the content of thiram in the soil sample to be detected.
The detection range of thiram in the soil sample of the embodiment is 0.8 mug/g to 12 mug/g.
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| CN112763440A (en) * | 2020-12-29 | 2021-05-07 | 西安邮电大学 | Method for detecting thiram based on silver nano triangular plate |
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Application publication date: 20200421 |
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| WD01 | Invention patent application deemed withdrawn after publication |