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Application method of dispersive solid phase extraction purification tube for detection of six phenoxycarboxylic acid herbicides in grain

A technology of phenoxycarboxylic acids and dispersed solid phase, which is applied in the fields of analytical chemistry and food safety detection, can solve the problems of low adsorption rate, large amount of organic solvent, and single type of adsorbent, and achieve the effect of simple operation

Inactive Publication Date: 2019-10-29
丁立平 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In order to overcome the disadvantages of using the pretreatment liquid-liquid extraction method to detect phenoxycarboxylic acid herbicides in grains, there are large amounts of organic solvents used and complicated operations; Due to the disadvantages of low adsorption rate and long time-consuming pretreatment, the purpose of the present invention is to provide a method for using a dispersed solid-phase extraction purification tube that can be used for the detection of six phenoxycarboxylic acid herbicides in grains.

Method used

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  • Application method of dispersive solid phase extraction purification tube for detection of six phenoxycarboxylic acid herbicides in grain
  • Application method of dispersive solid phase extraction purification tube for detection of six phenoxycarboxylic acid herbicides in grain
  • Application method of dispersive solid phase extraction purification tube for detection of six phenoxycarboxylic acid herbicides in grain

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Effect test

Embodiment 1

[0053] In this embodiment 1, the matrix is ​​a blank rice sample, and the concentration of the standard is 0.2 mg / kg:

[0054] (1) Extraction: Weigh 10g of ground rice flour into a 50mL centrifuge tube, add 30mL of deionized water to the centrifuge tube, homogenize at a high speed of 12000r / min for 1min, and centrifuge at a speed of 4500r / min for 3min ;

[0055] (2) Activation: take a dispersive solid-phase extraction purification tube, add 15 mL of deionized water to it, vortex for 3 min, centrifuge at 4500 r / min for 3 min, and discard the supernatant.

[0056] (3) Adsorption: Pour all the supernatant in the extraction step into the washed dispersive SPE purification tube, vortex for 3 minutes, shake for 15 minutes, centrifuge at 4500r / min for 3 minutes, and discard the supernatant;

[0057] (4) Desorption: Add 2.00mL of 1.00mol / L sodium sulfate solution to the centrifuge tube, vortex for 3min, shake for 15min, centrifuge at 4500r / min for 3min, and the supernatant obtained c...

Embodiment 2

[0061] In Example 2, the matrix is ​​a blank wheat sample, and the spiked concentration is 0.2 mg / kg:

[0062] (1) Extraction: Weigh 10 g of wheat flour ground into powder in a 50 mL centrifuge tube, add 30 mL of deionized water to the centrifuge tube, homogenize at a high speed of 12000 r / min for 1 min, and centrifuge at a speed of 4500 r / min for 3 min;

[0063] (2) Activation: take a dispersive solid-phase extraction purification tube, add 15 mL of deionized water to it, vortex for 3 min, centrifuge at 4500 r / min for 3 min, and discard the supernatant.

[0064] (3) Adsorption: Pour all the supernatant in the extraction step into the washed dispersive SPE purification tube, vortex for 3 minutes, shake for 15 minutes, centrifuge at 4500r / min for 3 minutes, and discard the supernatant;

[0065] (4) Desorption: Add 2.00mL of 1.00mol / L sodium sulfate solution to the centrifuge tube, vortex for 3min, shake for 15min, centrifuge at 4500r / min for 3min, and the supernatant obtained c...

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Abstract

Belonging to the field of analytical chemistry and food safety detection, the invention relates to a dispersive solid-phase extraction purification tube for detection of six phenoxy carboxylic acid herbicides in cereals and a use method thereof. Specifically, the dispersive solid-phase extraction purification tube consists of a tube cap (1), a tube body (2) and filler (3), wherein the filler (3) is 0.10g of a magnesium-aluminum type toluene-4-sodium sulfonate pillared hydrotalcite adsorbent. The use method of the dispersive solid-phase extraction purification tube includes the following three steps: activating the purification tube, adsorbing a target object and eluting the target object. The adsorbent adopted by the invention is an adsorbent with high efficiency adsorption effect on the six phenoxy carboxylic acid herbicides, and only a 0.10g dosage is needed. The employed dispersive solid-phase extraction purification tube pretreatment method has the characteristics of no use of organic solvent, safety and environmental protection, and also has the advantages of simple operation, rapidity and high efficiency.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and food safety detection, and in particular relates to a method for using a dispersed solid-phase extraction purification tube that can be used for six kinds of phenoxycarboxylic acid herbicides in grains. Background technique [0002] Phenoxycarboxylic acid herbicides are the second most selective herbicides in agricultural production, and are widely used in paddy fields, non-cultivated lands and pastures. Important factors affecting the food safety of cereals. For this reason, major countries and regions such as China, the European Union, the United States, and Japan have all stipulated maximum limit values ​​(MRL) requirements for phenoxycarboxylic acid herbicides in grains such as rice, wheat, and corn. [0003] At present, the detection methods of phenoxycarboxylic acid herbicides in grains are mainly chromatography and chromatography-mass spectrometry; the pretreatment method has gone t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/08
CPCG01N30/02G01N30/08G01N2030/062
Inventor 丁立平蔡春平陈学灿刘正才
Owner 丁立平
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