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

Inactive Publication Date: 2012-07-04
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few reports on the application of capillary electrophoresis to the detection of sulfonylurea herbicide residues

Method used

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  • Method for quantitatively detecting residual sulfonylurea herbicide trace amount in soil
  • Method for quantitatively detecting residual sulfonylurea herbicide trace amount in soil
  • Method for quantitatively detecting residual sulfonylurea herbicide trace amount in soil

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention discloses a method for quantitatively detecting residual sulfonylurea herbicide trace amount in soil, which comprises the steps of adding soil to be detected into 0.1mol/L sodium bicarbonate water solution with pH7.8, oscillating for 1h, centrifuging for 5min at a speed of 12000r/min, obtaining sediments and primary liquid supernatant, taking the primary liquid supernatant to be adjusted to be in pH2.5 by 0.1M hydrochloric acid water solution, preparing a sample to be detected, and detecting the sample to be detected by a capillary electrophoresis apparatus; and obtaining contents of metsulfuron-methyl, chlorsulfuron and chlorimuron-ethyl in the sample to be detected according to standard curves of the metsulfuron-methyl, the chlorsulfuron and the chlorimuron-ethyl. The method is high in detecting sensitivity, and reaches detection limit with 10-3 microgram/kg grade, wherein the value of the limit of detection with 10-3g/kg grade is higher than that of the detection limit of other methods of an efficient liquid chromatogram and the like (not more than microgram/kg).

Description

(1) Technical field [0001] The invention relates to a method for detecting trace residues of sulfonylurea herbicides in soil, in particular to a method for quantitatively detecting trace residues of sulfonylurea herbicides in soil. (2) Background technology [0002] With the modernization of agricultural technology and the liberation of productivity, chemical herbicides have become the main means of controlling the harm of weeds in farmland. Since DuPont launched the first ultra-efficient sulfonylurea herbicide (chlorsulfuron) in the 1980s, sulfonylurea herbicides have become important herbicides for weed control in farmland in the world today, and are widely used in my country. For example, in Wuxi, Jiangsu Province, 31% of the paddy fields use the mixture of tribenuron-methyl and metsulfuron-methyl to control weeds. The dosage of this kind of herbicide is very low, only 2-75g of active ingredient is needed per hectare; and the selectivity is strong, the sensitivity to diff...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 廖敏谢晓梅
Owner ZHEJIANG UNIV
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