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Method for purifying pesticide residues and special purifier thereof

A technology for pesticide residues and purifiers, applied in chemical/physical processes, preparation of test samples, ion exchange regeneration, etc., can solve problems such as time-consuming, solvent-consuming, accidental errors, complicated methods, etc., and achieve convenient operation and purification effect Good, accurate test results

Active Publication Date: 2015-03-11
CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional sample preparation methods have many time-consuming and laborious manual steps, such as crushing, suction filtration, solvent transfer and evaporation, etc., using separatory funnels and column chromatography, etc., not only the method is complicated, time-consuming and solvent-consuming, but also may cause system failure. error and accidental error

Method used

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  • Method for purifying pesticide residues and special purifier thereof
  • Method for purifying pesticide residues and special purifier thereof
  • Method for purifying pesticide residues and special purifier thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1, purifier

[0029] like figure 1 As shown, the purifier provided by the present invention includes a syringe 1 and a purification column 2; the purification column 2 is a cylindrical shape, and an upper sieve plate 3 distributed along its axial direction is provided near the end of the purification column 2 and the lower sieve plate 4, the upper sieve plate 3 and the lower sieve plate 4 are filled with adsorption filler 5, and both the upper sieve plate 3 and the lower sieve plate 4 have a mesh structure with a pore size of 20 μm, stable physical and chemical properties, and can It acts as a filter and barrier; one end of the purification column 2 away from the adsorption filler 5 is sealed with the syringe 1, and one end of the purification column 2 with the adsorption filler 5 is connected to the needle 6 for extracting the extract.

[0030] In the above-mentioned purifier, the pore size of the upper sieve plate and the lower sieve plate can be adjusted ...

Embodiment 2

[0031] Example 2. Analysis of pesticide residues in tomato (vegetable)

[0032] Utilize the clarifier that embodiment 1 provides to analyze.

[0033] Types of pesticide residues: organophosphorus pesticides (parathion, methyl parathion, monocrotophos, malathion, isocarbophos, profenofos, methyl isofenphos, fenthion, diazines Phosphorus and Phosphorus);

[0034] Purification column packing preparation: 200 mg of adsorption packing, including 50 mg of N-propylethylenediamine, 150 mg of anhydrous magnesium sulfate, and a particle size of 40-100 μm;

[0035] Specific steps are as follows:

[0036] (1) Prepare the sample solution, use 10mL acetonitrile (containing 1% formic acid by volume) to extract the analyte in the tomato to obtain the extract solution, wherein the concentration of pesticide in the extract solution is 0.1mg / L;

[0037] (2) Pipette 1mL of the extract solution into the centrifuge tube 7, draw the extract solution into the purification column 2 with the syringe...

Embodiment 3

[0044] Example 3. Analysis of pesticide residues in grapes (fruits)

[0045] Utilize the clarifier that embodiment 1 provides to analyze.

[0046] Types of pesticide residues: organochlorine pesticides (pentachloronitrobenzene, α-666, β-666, γ-666, DDT and procymidone);

[0047] Purification column packing preparation: 160 mg of adsorption packing, including 10 mg of multi-walled carbon nanotubes (with a diameter of 10-20 nm), 150 mg of anhydrous magnesium sulfate, and a particle size of 5-100 μm;

[0048] Specific steps are as follows:

[0049] (1) Prepare the sample solution, use 10mL of acetonitrile to extract the analytes in the grapes to obtain the extract, and the residual concentration of pesticides in the extract is 0.1mg / L;

[0050] (2) Pipette 1mL of the extract into the centrifuge tube 7, draw the extract into the purification column 2 with the syringe 1, and then push out the solution into the centrifuge tube 7;

[0051] (3) The purified extract enters the sampl...

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Abstract

The invention discloses a method for purifying pesticide residues and a special purifier thereof. The purifier comprises a purifying column, wherein an upper sieve plate and a lower sieve plate distributed in the axial direction are arranged in the position close to the end part in the purifying column; an adsorption filler is filled between the upper sieve plate and the lower sieve plate; the end part of the purifying column far away from the filler is connected with a cylinder body; a piston is arranged in the cylinder body; the piston can move in the axial direction of the cylinder body; and the end part, far away from the filler, of the purifying column is connected with a needle head. The method comprises the steps as follows: (1) extracting the pesticide residues in a sample to be tested by using a solvent to obtain an extracting solution; and (2) placing the extracting solution into a centrifugal pipe, sucking the extracting solution into the purifying column by utilizing the purifier, and pushing the extracting solution into the centrifugal pipe to obtain the purified pesticide residues. According to the method for purifying pesticide residues and the special purifier thereof, the time of finishing the whole operation process is less than 1 min, extracting solutions of various pesticides and agricultural products can be purified by adopting different filler configurations and extracting solvents, the purifying effect is good, and the instrument analysis requirements can be met.

Description

technical field [0001] The invention relates to a pesticide residue purification method and a special purifier thereof, and the field of pesticide residue analysis. Background technique [0002] In the process of pesticide residue analysis, the sample preparation is to transfer the trace amount of pesticides to be tested from the sample matrix to the extract as much as possible in the operation steps, and then purify to remove the existing interfering co-extracted substances. The pretreated extract can be directly processed sample determination. Traditional sample preparation methods have many time-consuming and laborious manual steps, such as crushing, suction filtration, solvent transfer and evaporation, etc., using separatory funnels and column chromatography, etc., not only the method is complicated, time-consuming and solvent-consuming, but also may cause system failure. error and accidental error. Contents of the invention [0003] The purpose of the present invent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/08G01N1/34
Inventor 潘灿平赵鹏跃
Owner CHINA AGRI UNIV
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