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Gas chromatography-mass spectrography method for determining three trace imidazolinone herbicides in bean flour

An imidazolinone and gas chromatography technology, which is applied in the field of analysis and detection of harmful trace substances, can solve the problems of high price, limited types of commercial solid-phase extraction columns and lack, and achieves the effect of saving adsorption time.

Active Publication Date: 2019-01-18
丁立平 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the existing reports, the types of commercial SPE columns that can be used in the SPE method are limited and expensive; the adsorbents of the dispersive SPE method are aimed at the adsorption targets of pigments, sterols, proteins and other impurities, and there is a lack of specialized columns. Some, adsorbents that selectively adsorb imidazolinone herbicide targets

Method used

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  • Gas chromatography-mass spectrography method for determining three trace imidazolinone herbicides in bean flour
  • Gas chromatography-mass spectrography method for determining three trace imidazolinone herbicides in bean flour
  • Gas chromatography-mass spectrography method for determining three trace imidazolinone herbicides in bean flour

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Experimental program
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Embodiment 1

[0078] The present embodiment 1 adopts soybean powder as the sample matrix to carry out the standard addition recovery experiment to verify the feasibility of the method of the present invention, and proceeds according to the following steps:

[0079] 1. Extraction and adsorption of compounds:

[0080] Weigh 4.00g of blank soybean powder samples in 50mL plastic centrifuge tubes with stoppers, add 30mL of 10% methanol aqueous solution with 0.01mol / L sodium hydroxide solution to adjust pH=9.0 to it, and extract by homogenizing at a high speed of 15000rpm for 1min , centrifuge, take the supernatant to another 100.0mL centrifuge tube with a plastic plug, re-extract once and combine the extracts; add 5.00mL of n-hexane to the extract, vortex, remove the upper n-hexane layer after centrifugation, and then Add 0.50 g of 7-amino-2-naphthalenesulfonate-magnesium aluminum hydrotalcite adsorbent to the centrifuge tube, and shake for 15 minutes to make the adsorbent adsorb the target comp...

Embodiment 2

[0092] The present embodiment 2 adopts mung bean flour as the sample matrix to carry out the standard addition recovery experiment to verify the feasibility of the method of the present invention, and proceeds according to the following steps:

[0093] 1. Extraction and adsorption of compounds:

[0094]Weigh 4.00g of blank mung bean flour samples in 50mL plastic centrifuge tubes with stoppers, add 30mL of 10% methanol aqueous solution to adjust pH=9.0 with 0.01mol / L sodium hydroxide solution, and extract by high-speed homogenization at 15000rpm for 1min , centrifuge, take the supernatant to another 100.0mL centrifuge tube with a plastic plug, re-extract once and combine the extracts; add 5.00mL of n-hexane to the extract, vortex, remove the upper n-hexane layer after centrifugation, and then Add 0.50 g of 7-amino-2-naphthalenesulfonate-magnesium aluminum hydrotalcite adsorbent to the centrifuge tube, and shake for 15 minutes to make the adsorbent adsorb the target compound in ...

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Abstract

The invention relates to a trace harmful substance analysis and detection method, and particularly relates to a gas chromatography-mass spectrography method for determining three trace imidazolinone herbicides including imazapyr, imazethapyr and imazamox in bean flour. The method comprises the following steps of taking a 10% methanol aqueous solution for regulating the pH value as an extracting solution; performing high-speed homogenate extraction; enriching a target compound in the extracting solution by a novel 7-amino-2-naphthalenesulfonate-magnesium aluminum hydrotalcite adsorbent; dissolving the adsorbent by an acid to completely elute a target object; performing efficient extraction on the compound by using a small-dose organic solvent; and performing rapid analysis and determinationby the gas chromatography-mass spectrography method after derivation of a boron trifluoride-methanol solution. The novel adsorbent adopted by the method realizes rapid and efficient adsorption of thetarget object in a dispersive solid-phase extraction mode; the complete desorption of the target object can be realized by using the acid to dissolve the adsorbent; and only a small amount of organicsolvent is used for extraction, so that the method has remarkable advantages of safety, environmental protection and economy.

Description

technical field [0001] The invention relates to a method for the analysis and detection of harmful trace substances, in particular to a gas chromatography-mass spectrometry method for the determination of three imidazolinone herbicides such as imazethapyr, imazethapyr and imazethapyr in soybean powder . Background technique [0002] Imidazolinone herbicides are a class of ultra-efficient herbicides discovered by the American cyanamide company in the 1980s. The dosage of its active ingredients is 2.3-16.7 grams per mu. It is mainly used for soybeans, peanuts, vegetables and other upland crops to prevent and control numerous annual and perennial grass weeds, broad-leaved weeds, and sedge weeds. This type of herbicide is an inhibitor of acetolactate synthase (ALS) or acetohydroxyacid synthase (AHAs), which is absorbed through roots, stems, and leaves, and conducts in xylem and phloem, accumulates in plant meristems, and inhibits Plant acetolactate synthase prevents the biosyn...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/08
CPCG01N30/02G01N30/08G01N2030/062
Inventor 丁立平蔡春平张睿郑铃黄菁菁郑麟毅郑香平姜晖陈志涛
Owner 丁立平
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