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A Gas Chromatographic Method for the Simultaneous Determination of Four Benzoic Acid Herbicides in Grain

A gas chromatography and benzoic acid technology, which is applied in the field of analysis and detection of harmful trace substances, can solve the problems of large organic solvents, limited types of solid phase extraction columns, time-consuming and inefficient gel permeation chromatography, etc., and can save adsorption time. Effect

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

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Problems solved by technology

[0007] In order to overcome the time-consuming and inefficient use of gel permeation chromatography in the pretreatment of the detection of benzoic acid herbicide residues in the existing standard methods, the need to consume a large amount of organic solvents, not suitable for large-throughput sample screening, and the use of solid phase in literature methods The extraction column is time-consuming and inefficient, and the types of solid-phase extraction columns are limited. The technical problem to be solved by the present invention is to provide a new adsorbent-based dispersive solid-phase extraction for fast adsorption, suitable for trace amounts of dicamba, grass Gas Chromatography for Simultaneous Determination of Residues of Trimethoprim, Metrazil and Chlorophthalic Acid

Method used

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  • A Gas Chromatographic Method for the Simultaneous Determination of Four Benzoic Acid Herbicides in Grain
  • A Gas Chromatographic Method for the Simultaneous Determination of Four Benzoic Acid Herbicides in Grain
  • A Gas Chromatographic Method for the Simultaneous Determination of Four Benzoic Acid Herbicides in Grain

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Embodiment 1

[0076] The present embodiment 1 adopts the blank sample matrix of rice to carry out the addition recovery experiment to verify the feasibility of the method of the present invention, according to the following steps:

[0077] 1. Extraction and adsorption of compounds:

[0078] Weigh 5.00g of blank sample in a 50mL stoppered centrifuge tube, and add 5.00mL of four compound standard solutions with concentrations of 10.0μg / L, 20.0μg / L and 200.0μg / L to each of them to prepare three levels of six For parallel spiked samples, add 20mL of alkaline 10% acetone aqueous solution with pH=9 to the centrifuge tube, seal and vortex, then ultrasonically extract for 15min, centrifuge, transfer the supernatant to another stoppered plastic centrifuge tube, and re- Extract once and combine the extracts; add 0.50 g of benzenesulfonate-magnesium aluminum type hydrotalcite roasted product adsorbent to the centrifuge tube, seal and vortex and shake for 15 minutes to make the adsorbent absorb the tar...

Embodiment 2

[0089] The present embodiment 2 adopts the blank sample matrix of wheat to carry out the standard recovery experiment to verify the feasibility of the method of the present invention, according to the following steps:

[0090] 1. Extraction and adsorption of compounds:

[0091] Weigh 5.00g of blank sample in a 50mL stoppered centrifuge tube, and add 5.00mL of four compound standard solutions with concentrations of 10.0μg / L, 20.0μg / L and 200.0μg / L to each of them to prepare three levels of six For parallel spiked samples, add 20mL of alkaline 10% acetone aqueous solution with pH=9 to the centrifuge tube, seal it and vortex it, then extract it by ultrasonic for 15min, centrifuge, transfer the supernatant to another plastic centrifuge tube with stopper, and re- Extract once and combine the extracts; add 0.5g benzenesulfonate-magnesium aluminum type hydrotalcite roasted product adsorbent to the centrifuge tube, seal and vortex, shake for 15min, and then let the adsorbent absorb the ...

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Abstract

The invention relates to a method for analyzing and detecting trace harmful substances, in particular to a gas chromatographic method for simultaneously measuring trace amounts of dicamba, bacamba, mebazone and chlorophthalic acid residues in grains. The method steps include ultrasonically extracting the target substance in the sample with a 10% acetone aqueous solution with pH=9, enriching the target compound in the extract with a novel adsorbent benzenesulfonate-magnesium aluminum type hydrotalcite roasting product, and dissolving the adsorbent with hydrochloric acid solution to achieve the target The compound is completely eluted, the compound is extracted efficiently with a small amount of organic solvent, and the compound is quickly analyzed and determined by gas chromatography after derivatization. The new adsorbent used in this method adopts the method of dispersed solid phase extraction to achieve fast and efficient adsorption of the target substance, which can save a lot of adsorption time compared with gel permeation chromatography and solid phase extraction; the application of acid-soluble adsorbent can achieve the target Complete desorption of substances; only a small amount of organic solvent extraction has significant safety, environmental protection and economic advantages.

Description

technical field [0001] The invention relates to a method for analyzing and detecting harmful trace substances, in particular to a gas chromatographic method for simultaneously measuring trace amounts of dicamba, bacamba, mebazone and chlorphthalic acid residues in grains. Background technique [0002] Herbicides are important substances in agricultural production and play a major role in killing harmful weeds and increasing the yield of agricultural products. However, with the widespread use of various herbicides, the problems of herbicide abuse and residues have become increasingly prominent. Among them, benzoic acid herbicides are one of the most important ones. Currently, the types sold and used in the market include dicamba, fenfoam, mebafen, and chlorphthalic acid. They all belong to the low-to-medium toxicity herbicides. Skin contact can cause poisoning, clinical symptoms vary. [0003] Benzoic acid herbicides are phytohormone herbicides, which have systemic conductio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 丁立平张睿黄菁菁姜晖郑铃郑香平郑麟毅陈志涛蔡春平
Owner 丁立平