Method for quantitatively detecting residual sulfonylurea herbicide trace amount in soil
A sulfonylurea, quantitative detection technology, applied in measurement devices, instruments, scientific instruments, etc., can solve the problem of few reports on the detection of sulfonylurea herbicide residues, and achieve the effect of high detection sensitivity
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Embodiment 1
[0036] Example 1 standard curve drawing
[0037] Pipette 25, 50, 100, 200, 300, 400 and 500 μL of 100mg / L mixed standard stock solution into seven 5mL volumetric flasks, dilute to volume with methanol-water (60:40; v / v) mixed solvent, Obtain mixed standard solutions with concentrations of metsulfuron-methyl, chlorsulfuron-methyl and chlorimuron-methyl at 0.5, 1.0, 2.0, 4.0, 6.0, 8.0 and 10 mg / L, respectively, and use the above detection conditions for capillary electrophoresis detection. Using the peak area and the concentration of metsulfuron-methyl, chlorsulfuron-methyl and chlorimuron-methyl to draw the working standard curve, the working standard curve is used for the quantitative calculation of the residues of metsulfuron-methyl, chlorsulfuron-methyl and chlorimuron-methyl, the results are shown in figure 1 .
Embodiment 2
[0038] Example 2 Determination of the soil sample to be tested
[0039] Weigh 100g of dried soil samples into a 500mL Erlenmeyer flask, add 200mL 0.1mol / L sodium bicarbonate (pH7.8) aqueous solution, cover with a rubber stopper and shake for 1h, then centrifuge at 12000r / min for 5min. The supernatant was obtained, the extraction residue was extracted twice with the same sodium bicarbonate solution, and the obtained supernatants were combined. The combined supernatant was adjusted to pH 2.5 with 0.1M hydrochloric acid solution, and loaded into a C18 column (the C18 column was first activated with 10mL of methanol and passivated with 10mL of double-distilled water, and the eluent was discarded), and then washed with 10mL of dichloro Rinse the C18 column with methane, collect the eluate, concentrate to dryness with a rotary evaporator, dissolve the concentrate in 1 mL of methanol-water (60:40; v / v) mixed solvent, transfer it to a 5 mL volumetric flask, and place in a volumetric f...
Embodiment 3
[0044] Determination of trace metsulfuron-methyl, chlorsulfuron-methyl and chlorimuron-methyl in the paddy field soil sample of embodiment 3
[0045] (1) Soil: The soil samples used for testing were collected from paddy fields in the suburbs of Hangzhou, Zhejiang Province. The soil sample has not been applied with sulfonylurea herbicides. The soil texture is sandy loam, with a clay content of 18.0%, a silt content of 55.2%, a sand content of 26.8%, a pH of 4.74, and an organic matter content of 1.82%.
[0046] (2) 1mg / L mixed standard stock solution
[0047] Accurately weigh 1 mg each of metsulfuron-methyl, chlorsulfuron-methyl, and chlorimuron-methyl, and dissolve them in 1 L of double-distilled water to obtain a mixed standard reserve containing metsulfuron-methyl, chlorsulfuron-methyl, and chlorimuron-methyl at a concentration of 1 mg / L respectively. liquid.
[0048] (3) Detection sensitivity
[0049] The experiment is divided into 3 groups, group a, group b and group c,...
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