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Measuring method of cloransulam-methyl residues in soybeans and soil

A technology for the determination of cloxazone and its method, which is applied in the field of determination of cloxazone residues in soybeans and soils, can solve problems such as no public reports, and achieve simple and quick operation, avoiding matrix interference, and high accuracy degree of effect

Inactive Publication Date: 2010-09-22
CENT LAB TIANJIN ACADEMY OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Clossulam is a commonly used herbicide in my country. There are no public reports on the detection and analysis of the residues of Clossulam in soil and soybeans.

Method used

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  • Measuring method of cloransulam-methyl residues in soybeans and soil
  • Measuring method of cloransulam-methyl residues in soybeans and soil
  • Measuring method of cloransulam-methyl residues in soybeans and soil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Extraction: Weigh 20 g of soybeans, place them in a stoppered Erlenmeyer flask, add 20 mL of pure water, let stand for 10 minutes, add 50 mL of acetonitrile, shake and extract for 30 minutes;

[0041] (2) Separation: filter and transfer to a separatory funnel, add 20mL 0.01mol / L hydrochloric acid and a saturated aqueous solution of sodium chloride, shake for 3 minutes, and let stand to separate layers;

[0042] (3) Extraction: extract again with 50mL acetonitrile, combine, and concentrate methanol to 10mL under reduced pressure;

[0043] (4) Purification: The solid-phase extraction C18 column is pre-leached with acetonitrile, the above-mentioned extraction phase is purified through the column, the leachate is collected, concentrated and nearly dry, and the V / V methanol:water 1:1 is used to constant volume and filter through the filter membrane to be tested;

[0044] (5) Determination: detection by liquid chromatography, in which chromatographic column: Acquity BEH ...

Embodiment 2

[0047] (1) Extraction: Weigh 20 g of soybeans, place them in a stoppered Erlenmeyer flask, add 60 mL of pure water, let stand for 30 minutes, add 70 mL of acetonitrile, shake and extract for 60 minutes;

[0048] (2) Separation: filter and transfer to a separatory funnel, add 30mL 0.01mol / L hydrochloric acid and saturated aqueous solution of sodium chloride, shake for 10 minutes, and let stand to separate layers;

[0049] (3) Extraction: extract again with 100mL acetonitrile, combine the acetonitrile and concentrate under reduced pressure to 30mL;

[0050] (4) Purification: the solid-phase extraction C18 column is pre-leached with acetonitrile, the above-mentioned extraction phase is purified through the column, the leachate is collected, concentrated and nearly dry, and the V / V methanol:water 1:1 is used to constant volume and filter through the filter membrane to be tested;

[0051] (5) Determination: detection by liquid chromatography, in which chromatographic column: Acqui...

Embodiment 3

[0054] (1) Extraction: weigh 15g of soil, put it in a stoppered Erlenmeyer flask, add 40mL of pure water, let it stand for 20 minutes, add 60mL of acetonitrile, shake and extract for 40 minutes;

[0055] (2) Separation: filter and transfer to a separatory funnel, add 25mL 0.01mol / L hydrochloric acid and saturated aqueous solution of sodium chloride, shake for 10 minutes, and let stand to separate layers;

[0056] (3) Extraction: extract again with 80mL acetonitrile, combine the acetonitrile and concentrate under reduced pressure to 25mL;

[0057] (4) Purification: the solid-phase extraction C18 column is pre-leached with acetonitrile, the above-mentioned extraction phase is purified through the column, the leachate is collected, concentrated and nearly dry, and the V / V methanol:water 1:1 is used to constant volume and filter through the filter membrane to be tested;

[0058] (5) Determination: detection by liquid chromatography, in which chromatographic column: Acquity BEH C8...

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Abstract

The invention relates to a measuring method of cloransulam-methyl residues in soybeans and soil, comprising the following concrete steps of: weighing 10-20g of samples and then putting in a conical flask with a plug; adding 20-60mL of pure water and standing for 10-30 min; then adding 50-70mL of acetonitrile; extracting for 30-60 min under vibration; filtering and transferring to a separating funnel; adding 20-30mL of 0.01mol / L hydrochloric acid and a saturated sodium chloride aqueous solution; vibrating for 3-10 min and standing for demixing; extracting again by using 50-100mL of acetonitrile, merging and concentrating to 10-30mL; purifying: sprinkling a solid phase extraction C18 column with the acetonitrile in advance, and purifying the extraction phase by adopting a column chromatography; collecting leaching liquid; concentrating for dryness; making at constant volume by using methanol and water the volume ratio of which is 1:1 and filtering through a filter membrane; and carrying out detection by adopting a liquid chromatogram method. The measuring method has the characteristics of simple and quick operation, high recovery rate, high sensitivity and small impurity interference and provides the reliable guarantee for rapidly and accurately measuring the cloransulam-methyl residues in the soybeans and the soil and establishing a simple and convenient and effective analysis method.

Description

technical field [0001] The invention belongs to the technical field of determination of pesticide residues, and in particular relates to a method for determining the residues of cloxazone in soybeans and soil. Background technique: [0002] The World Health Organization and the Food and Agriculture Organization of the United Nations (WHO / FAO) define pesticide residue limits as the maximum concentration of pesticide residues formed in food and feed after direct or indirect use of pesticides in accordance with good agricultural production (GAP) practices . First of all, according to the toxicity evaluation of pesticides and their residues, in accordance with the good agricultural practices and safe and rational use of pesticides promulgated by the country, to meet the needs of the prevention and control of various pests and diseases in the country, under strict technical supervision, under the premise of effective control of pests and diseases, in the Take the representative ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 郭永泽邵辉程奕李辉李娜刘磊张玉婷宋淑荣
Owner CENT LAB TIANJIN ACADEMY OF AGRI SCI
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