Method using surface enhanced raman spectroscopy to detect paraquat
A surface-enhanced Raman and spectral detection technology, applied in Raman scattering, preparation of test samples, measurement devices, etc., can solve the problems of detection substrate interference, complex components, affecting the sensitivity of detection results, etc., and achieve low-cost detection, The effect of high sensitivity and low detection limit
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Embodiment 1
[0038] Example 1 Preparation of gold nanoparticle sol
[0039]100mL concentration is that the chloroauric acid solution of 0.01wt% is poured in the flask, is placed on the constant temperature magnetic stirrer, 1100rpm vigorously stirs and is heated to solution boiling, then adds 0.7mL concentration and is the trisodium citrate solution of 1wt%, simultaneously Stir vigorously at 1100rpm and keep boiling for 15min. The reaction is quickly terminated in an ice bath. After the reaction solution is cooled, 15mL is taken for centrifugation and the supernatant (about 14mL) is discarded. The gold nanoparticle hydrosol in the lower layer is used for subsequent detection.
[0040] The prepared gold nanoparticles were detected, and the results were as follows: figure 2 , the average particle size of the prepared gold nanoparticles is 64±6nm, the size is uniform, and the dispersion is good.
Embodiment 2
[0041] Example 2 Detection of Paraquat Standard Solution
[0042] Firstly prepare paraquat standard aqueous solutions with gradient concentrations (10μg / L, 5μg / L, 2μg / L, 1μg / L, 0.5μg / L, 0.2μg / L, 0μg / L), and filter the standard aqueous solution with a 0.22μm filter membrane Finally, take 50 μL and place it in a 1.5 mL centrifuge tube, add an equal volume of gold nanoparticle sol (prepared in Example 1) to mix, vortex and shake for 10 seconds, take 5 μL of the mixed solution and add it dropwise to a clean silicon chip, and dry it. Surface-enhanced Raman spectroscopy was performed using a micro-Raman spectrometer. The power of the micro-Raman spectrometer is 80mW, the laser wavelength is 780nm, and the collected spectrum ranges from 550 to 2000cm -1 .
[0043] The test results of paraquat standard solution with gradient concentration are as follows: image 3 As shown, the Raman spectrum of paraquat standard is shown as figure 1 shown. according to image 3 It can be seen fr...
Embodiment 3
[0044] Example 3 Direct Determination of Paraquat in Apple Juice
[0045] Add paraquat mother liquor to apple juice, prepare apple juice samples of paraquat with a gradient concentration of 0-20 μg / mL and filter through a 0.22 μm filter membrane, take 50 μL and place it in a 1.5 mL centrifuge tube, add an equal volume of gold nanoparticle sol (implemented Example 1 (preparation and mixing), after shaking for 10s, take 5 μL and drop it on a clean silicon wafer, dry it, and use a micro-Raman spectrometer to measure it. The power of the micro-Raman spectrometer is 80mW, the laser wavelength is 780nm, and the scanning range is 550-2000cm -1 .
[0046] The obtained SERS spectrum is as follows Figure 6 As shown, it can be seen that the direct mixing method was used to determine the content of paraquat in apple juice, and the minimum detection concentration was 5 μg / mL.
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