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A Gas Chromatographic Method for Determination of Eight Kinds of Phenoxycarboxylic Acid Herbicides in Corn

A phenoxycarboxylic acid and gas chromatography technique is applied in the field of gas chromatography for determining the residues of eight phenoxycarboxylic acid herbicides in corn, and can solve the problems of few types of commercial products, lack of selective adsorption fillers, solid Problems such as limited types of phase extraction columns

Active Publication Date: 2021-05-07
丁立平 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the defect that the liquid-liquid extraction method that exists in the detection pretreatment of trace amounts of phenoxycarboxylic acid herbicides in existing plant-derived foods needs to use a large amount of organic solvents; and the solid-phase extraction method has limited types of solid-phase extraction columns, Due to the lack of commercialized product types and lack of exclusive selective adsorption fillers, the technical problem to be solved by the present invention is to provide a rapid solid-phase extraction based on a novel p-toluenesulfonate-magnesium aluminum type hydrotalcite roasting product adsorbent Adsorbed, gas-chromatographic method suitable for the detection of eight trace phenoxycarboxylic acid herbicide residues in maize

Method used

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  • A Gas Chromatographic Method for Determination of Eight Kinds of Phenoxycarboxylic Acid Herbicides in Corn
  • A Gas Chromatographic Method for Determination of Eight Kinds of Phenoxycarboxylic Acid Herbicides in Corn
  • A Gas Chromatographic Method for Determination of Eight Kinds of Phenoxycarboxylic Acid Herbicides in Corn

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Experimental program
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Embodiment 1

[0075] In Example 1, blank corn kernels were used as the sample matrix to carry out the standard addition recovery experiment to verify the feasibility of the method of the present invention, and processed according to the following steps:

[0076] 1. Extraction and adsorption of compounds:

[0077] Weigh 5.00g of blank sample in a 50mL stoppered plastic centrifuge tube, add an appropriate amount of standard solution respectively to prepare three-level and six-parallel spiked samples, add 25mL of alkaline 10% acetone aqueous solution with pH=9.0 to the centrifuge tube, and 15000rpm high-speed homogenate extraction for 1min, centrifuge, transfer the supernatant to another 100mL stoppered plastic centrifuge tube, extract again, combine the extracts, add 0.50g p-toluenesulfonate-magnesium aluminum type to the extract Hydrotalcite roasting product adsorbent, shake for 15 minutes to make the adsorbent adsorb eight target compounds in the extract;

[0078] 2. Desorption of compound...

Embodiment 2

[0090] In Example 2, blank fresh corn kernels were used as the sample matrix to carry out a standard addition recovery experiment to verify the feasibility of the method of the present invention, and the process was carried out according to the following steps:

[0091] 1. Extraction and adsorption of compounds:

[0092] Weigh 5.00g of blank sample in a 50mL stoppered plastic centrifuge tube, add an appropriate amount of standard solution respectively to prepare three-level and six-parallel spiked samples, add 25mL of alkaline 10% acetone aqueous solution with pH=9.0 to the centrifuge tube, and 15000rpm high-speed homogenate extraction for 1min, centrifuge, transfer the supernatant to another 100mL stoppered plastic centrifuge tube, extract again, combine the extracts, add 0.50g p-toluenesulfonate-magnesium aluminum type to the extract Hydrotalcite roasting product adsorbent, shake for 15 minutes to make the adsorbent adsorb eight target compounds in the extract;

[0093] 2. ...

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Abstract

The invention relates to a method for analyzing and detecting trace harmful substances, in particular to a method for determining trace amounts of 2,4-dichlorophenoxyacetic acid, 2,4-dichlorophenoxypropionic acid and 2,4-dichlorophenoxy Gas chromatography for residues of eight phenoxycarboxylic acid herbicides including butyric acid. The method steps include extracting with alkaline 10% acetone aqueous solution, enriching the target compound in the extract with a novel p-toluenesulfonate-magnesium-aluminum hydrotalcite adsorbent, and using an acid-dissolved adsorbent to achieve complete elution of the target compound, The compound is extracted efficiently with a small amount of organic solvent, and quickly analyzed and determined by gas chromatography after derivatization. The new adsorbent used in this method adopts the method of dispersive solid phase extraction to realize the rapid and efficient adsorption of the target substance, and the enrichment is efficient; the application of acid-dissolved adsorbent can realize the complete desorption of the target substance; only a small amount of organic solvent extraction is suitable, and the relative Compared with the liquid-liquid extraction method, which needs to use a large amount of organic solvent, it has significant safety, environmental advantages and economic advantages.

Description

technical field [0001] The invention relates to a method for analyzing and detecting harmful trace substances, in particular to a method for simultaneously determining trace amounts of 2,4-dichlorophenoxyacetic acid, 2,4-dichlorophenoxypropionic acid, and 2,4-dichlorophenoxypropionic acid in corn. Phenoxybutyric acid, 2,4,5-trichlorophenoxyacetic acid, 2,4,5-trichlorophenoxypropionic acid, 2-methyl-4-chlorophenoxypropionic acid, 2-methyl-4- Chlorophenoxyacetic acid, 2-methyl-4-chlorophenoxybutyric acid, eight kinds of phenoxycarboxylic acid herbicide residues by gas chromatography. Background technique [0002] Phenoxycarboxylic acid herbicides are the second largest sales and usage herbicides in the world, and they are also the first selective herbicides put into commercial production. Since they can be absorbed through the stems, leaves and roots of plants, this type of herbicides It is used as stem and leaf treatment agent in agricultural production, widely applied to ce...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 丁立平蔡春平林荆姜晖张睿黄菁菁郑铃郑香平郑麟毅陈志涛
Owner 丁立平