A kind of rapid indirect detection method of glyphosate
A detection method, glyphosate technology, applied in the field of rapid and indirect detection of glyphosate, can solve the problems of insufficient sensitivity of rapid detection methods, high technical requirements for personnel, harsh derivatization conditions, etc., and achieve high practical application and promotion value, Improved sensitivity and easy control of reaction conditions
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Embodiment 1
[0049] Embodiment one, the preparation of reagent and instrument condition:
[0050] Step 1, preparation of ninhydrin working solution:
[0051] Ninhydrin working solution consists of 5% ninhydrin, water, acetic acid-sodium acetate buffer (0.4mol L -1 , pH value is 5.5), the volume ratio of ninhydrin, water and acetate buffer is 1:1:1-3:1:1.
[0052] Step 2: Preparation and heat treatment of blank sample, ninhydrin working solution and sodium molybdate mixed solution:
[0053] The volume ratio of blank sample, ninhydrin working solution and sodium molybdate is 1:1:1-3:1:1. Under the condition of 80-100°C, heating for 20-40min, the color of the solution does not change after the solution is cooled.
[0054] Step 3: Preparation of Ag NPs:
[0055] 36mg AgNO 3 Disperse in 200mL of ultra-pure water, heat to boil, add appropriate amount of sodium citrate (1%, 4mL), keep the temperature at 85°C after the color starts to change, and obtain gray-green colloid after 40min, cool to...
Embodiment 2
[0058] Embodiment two, the mensuration of glyphosate standard substance and establishment of standard curve:
[0059] Step 1: Preparation and derivatization of the mixed solution of glyphosate standard substance, ninhydrin working solution and sodium molybdate:
[0060] Prepare different concentrations of glyphosate solutions (1.0 × 10 -9 -1.0×10 -4 mol L -1 ), were mixed with ninhydrin working solution and sodium molybdate respectively, and heated for 20-40min under the condition of 80-100°C to derivate into substances similar to Roman violet in different shades.
[0061] Step 2: Spectral measurement:
[0062] Ag NPs were added to the derivative solutions of different concentrations of glyphosate, and the absorption peak at 560-580nm was measured by the lambda1050+ UV-visible absorption spectrometer of Perkinelmer Company, as shown in figure 1 shown. .
[0063] Step 3: Establishment of standard curve:
[0064] A linear standard curve was established based on the common...
Embodiment 3
[0065] Embodiment 3. Detection of glyphosate residues in soil samples:
[0066] Step 1, the preparation of the extract solution of glyphosate residue in the soil sample:
[0067] Accurately weigh two fresh soil samples, one for dry matter content determination, and the other (dry matter content greater than 10 g) for glyphosate content. After fresh soil samples were centrifuged to remove water, 50.0 mL of sodium phosphate and sodium citrate were added to mix, ultrasonically extracted for 30 min, centrifuged at 8000-12000 r / min for 5 min, and the supernatant was filtered with filter paper.
[0068] Step 2, purification of the extract:
[0069] Add a small amount of concentrated hydrochloric acid, let it stand for 10 minutes, and filter it with filter paper to obtain the supernatant; add 50mL of n-hexane, shake it and let it stand, discard the organic phase, extract the water phase with 50mL of n-hexane again, and filter the water phase with a 0.45μM filter membrane , to obtai...
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